National Library of Energy BETA

Sample records for neutron powder diffraction

  1. Neutron powder diffraction analysis of (Tm{sub 0.50}Ca{sub 0...

    Office of Scientific and Technical Information (OSTI)

    Neutron powder diffraction analysis of (Tmsub 0.50Casub 0.50)MnOsub 3 and (Lusub 0.50Casub 0.50)MnOsub 3 Citation Details In-Document Search Title: Neutron powder ...

  2. Structural studies of magnesium nitride fluorides by powder neutron diffraction

    SciTech Connect (OSTI)

    Brogan, Michael A.; Hughes, Robert W.; Smith, Ronald I.; Gregory, Duncan H.

    2012-01-15

    Samples of ternary nitride fluorides, Mg{sub 3}NF{sub 3} and Mg{sub 2}NF have been prepared by solid state reaction of Mg{sub 3}N{sub 2} and MgF{sub 2} at 1323-1423 K and investigated by powder X-ray and powder neutron diffraction techniques. Mg{sub 3}NF{sub 3} is cubic (space group: Pm3m) and has a structure related to rock-salt MgO, but with one cation site vacant. Mg{sub 2}NF is tetragonal (space group: I4{sub 1}/amd) and has an anti-LiFeO{sub 2} related structure. Both compounds are essentially ionic and form structures in which nitride and fluoride anions are crystallographically ordered. The nitride fluorides show temperature independent paramagnetic behaviour between 5 and 300 K. - Graphical abstract: Definitive structures of the ternary magnesium nitride fluorides Mg{sub 3}NF{sub 3} and the lower temperature polymorph of Mg{sub 2}NF have been determined from powder neutron diffraction data. The nitride halides are essentially ionic and exhibit weak temperature independent paramagnetic behaviour. Highlights: Black-Right-Pointing-Pointer Definitive structures of Mg{sub 3}NF{sub 3} and Mg{sub 2}NF were determined by neutron diffraction. Black-Right-Pointing-Pointer Nitride and fluoride anions are crystallographically ordered in both structures. Black-Right-Pointing-Pointer Both compounds exhibit weak, temperature independent paramagnetic behaviour. Black-Right-Pointing-Pointer The compounds are essentially ionic with ionicity increasing with F{sup -} content.

  3. Strain and particle size of palladium powders by time-of-flight neutron diffraction

    SciTech Connect (OSTI)

    Lawson, A.C.; Conant, J.W.; Talcott, C.L.; David, M.A.; Vaninetti, J.; Goldstone, J.A.; Williams, A.; Von Dreele, R.B.; Roof, R.B.; Hitterman, R.L.; Richardson, J.W. Jr.; Faber, J. Jr.

    1989-01-01

    We have determined the strain and particle size for several samples of palladium powder by time-of-flight neutron powder diffraction on two different diffractometers and by x-ray powder diffraction. The results are compared and found to be in fair agreement. The time-of-flight method gives good enough precision to reveal deficiencies in the simple models used for strain and particle size line broadening. 6 refs., 4 figs., 2 tabs.

  4. MnO spin-wave dispersion curves from neutron powder diffraction

    SciTech Connect (OSTI)

    Goodwin, Andrew L.; Dove, Martin T.; Tucker, Matthew G.; Keen, David A.

    2007-02-15

    We describe a model-independent approach for the extraction of spin-wave dispersion curves from powder neutron total scattering data. Our approach is based on a statistical analysis of real-space spin configurations to calculate spin-dynamical quantities. The RMCPROFILE implementation of the reverse Monte Carlo refinement process is used to generate a large ensemble of supercell spin configurations from MnO powder diffraction data collected at 100 K. Our analysis of these configurations gives spin-wave dispersion curves for MnO that agree well with those determined independently using neutron triple-axis spectroscopic techniques.

  5. Neutron and X-ray powder diffraction study of skutterudite thermoelectrics

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Wang, H.; Kirkham, M. J.; Watkins, T. R.; Payzant, E. A.; Salvador, J. R.; Thompson, A. J.; Sharp, J.; Brown, D.; Miller, D.

    2016-02-17

    N- and p-type filled-skutterudite materials prepared for thermoelectric power generation modules were analyzed by neutron diffraction at the POWGEN beam line of the Spallation Neutron Source (SNS) and X-ray diffraction (XRD). The skutterudite powders were processed by melt spinning, followed by ball milling and annealing. The n-type material consists of Ba–Yb–Co–Sb and the p-type material consists of Di–Fe–Ni–Sb or Di–Fe–Co–Sb (Di = didymium, an alloy of Pr and Nd). Powders for prototype module fabrication from General Motors and Marlow Industries were analyzed in this study. XRD and neutron diffraction studies confirm that both the n- and p-type materials have cubicmore » symmetry. Structural Rietveld refinements determined the lattice parameters and atomic parameters of the framework and filler atoms. The cage filling fraction was found to depend linearly on the lattice parameter, which in turn depends on the average framework atom size. Ultimately, this knowledge may allow the filling fraction of these skutterudite materials to be purposefully adjusted, thereby tuning the thermoelectric properties.« less

  6. Neutron powder diffraction study of tetragonal crystal structures of cerium-neodymium dicarbides

    SciTech Connect (OSTI)

    Jones, D.W.; McColm, I.J.; Steadman, R.; Yerkess, J.

    1986-04-01

    The three ternary cerium-neodymium dicarbides Ce/sub x/Nd/sub 1-x/C/sub 2/ (x = 0.25, 0.50, 0.75) and the two binary dicarbides CeC/sub 2/ and NdC/sub 2/ were prepared and their room temperature crystal structures examined by neutron powder diffraction by the Rietveld profile analysis method. The five compounds are isostructural, with tetragonal unit cell dimensions changing monotonically over the range a = 3.881(2), c = 6.487(3) A to a = 3.827(2), c = 6.407(2) A and they contain discrete acetylenic C-C groups with carbon-carbon bond lengths close to 1.29(1) A. 10 references, 1 figure, 1 table.

  7. Applications of pulsed neutron powder diffraction to actinide elements. [Pu-Al

    SciTech Connect (OSTI)

    Lawson, A.C.; Richardson, J.W.; Mueller, M.H.; Lander, G.H.; Goldstone, J.A.; Williams, A.; Kwei, G.H.; Von Dreele, R.B.; Faber, J. Jr.; Hitterman, R.L.

    1987-11-01

    We have been using the technique of pulsed neutron powder diffraction to study several problems in the physics and chemistry of the actinide elements. In these elements one often encounters very complex structures resulting from polymorphic transformations presumably induced by the presence of 5f-electrons. For example, at least five distinct structures of plutonium metal are found between room temperature and its melting point of 640/sup 0/C, and two of the structures are monoclinc. The determination of the crystal structure of beta-uranium (tetragonal, 30 atoms per unit cell) which has finnaly been shown to be centrosymmetric, after decades of uncertainty is discussed. Some preliminary results on the structure of alpha-plutonium (which confirm Zachariasen's original determination of the monoclinic structure) are presented. Pu-Al alloys were also studied. 12 refs., 18 figs.

  8. Anomalous volume expansion in CaRu{sub 0.85}Fe{sub 0.15}O{sub 3}: Neutron powder diffraction and magnetic Compton scattering

    SciTech Connect (OSTI)

    Taniguchi, T.; Mizusaki, S.; Okada, N.; Nagata, Y.; Mori, K.; Wuernisha, T.; Kamiyama, T.; Hiraoka, N.; Itou, M.; Sakurai, Y.; Ozawa, T. C.; Noro, Y.; Samata, H.

    2007-01-01

    Neutron powder diffraction and magnetic Compton scattering measurements were conducted for ferromagnetic CaRu{sub 0.85}Fe{sub 0.15}O{sub 3} at temperatures between 10 and 300 K. Anomalous volume expansion was observed in the neutron diffraction measurement below the Curie temperature (85 K), and Invar-like behavior was observed below 40 K. However, no structural phase transition was observed down to 10 K. The strong correlation between the volume expansion, {delta}V, and the square magnetization, M{sup 2}, suggests that the anomalous volume expansion is due to the magnetovolume effect that is caused by the occurrence of ferromagnetism. The magnetic Compton scattering experiments revealed the existence of a magnetic moment on Ru and the antiferromagnetic configuration of Fe and Ru moments. The formation of a ferrimagnetic order through the induction of the magnetic moment on the Ru ion is a possible reason for the anomalous volume expansion observed for CaRu{sub 0.85}Fe{sub 0.15}O{sub 3}.

  9. A study of nitrogenation of a NdFe{sub 12-x}Mo{sub x} compound by in situ neutron powder diffraction.

    SciTech Connect (OSTI)

    Ding, Y.; Lin, J.; Loong, C.-K.; Short, S. M.

    1997-11-18

    The effects on the crystal lattice of a NdFe{sub 12{minus}x}Mo{sub x}(x {approx_equal} 1.7) compound which contained {approximately}12 vol% of bcc-Fe were studied by neutron powder diffraction during controlled nitrogenation over the 25-600 C temperature range. The sample inside the furnace was connected to a closed volume of ultra-pure nitrogen gas while neutron data were collected over regular time intervals during sequential heating. Substantial nitrogen absorption occurred between 500 to 600 C. During the nitrogenation process the NdFe{sub 12{minus}x}Mo{sub x}N{sub y} lattice expanded while the bcc-Fe lattice contracted. An increasing decomposition of the compound into bcc-Fe at 600 C was observed. The average size of the NdFe{sub 12{minus}x}Mo{sub x}N{sub y} crystalline grains decreased starting at {approximately}300 C, reaching a minimum at {approximately}500 C and then increased markedly at higher temperatures. The development of lattice strains, on the other hand, showed an opposite trend, i.e., a maximum at 500 C. A correlation of structural modification of the crystalline phases and the nitrogenation process is discussed.

  10. Crystal structure of α- and β-Na{sub 2}U{sub 2}O{sub 7}: From Rietveld refinement using powder neutron diffraction data

    SciTech Connect (OSTI)

    IJdo, D.J.W. Akerboom, S.; Bontenbal, A.

    2015-01-15

    The crystal structures of α- and β-Na{sub 2}U{sub 2}O{sub 7} have been determined from neutron powder diffraction. At 293 K, the compound α-Na{sub 2}U{sub 2}O{sub 7} has a monoclinic unit cell, space group P2{sub 1}/a, with a=12.7617(14) Å, b=7.8384(10) Å, c=6.8962(9) Å, β=111.285(9)°, and Z=4. At 773 K, β-Na{sub 2}U{sub 2}O{sub 7} is also monoclinic, space group C2/m, with a=12.933(1) Å, b=7.887(1) Å, c=6.9086(8) Å, β=110.816(10)°, and Z=4. The structures can be described by layers U{sub 2}O{sub 7}{sup 2−} built from corner linked deformed UO{sub 6} octahedra with pentagonal UO{sub 7} bipyramids in between linked with common edges to each other and to the octahedra. The Na atoms occupy the interlayer space. The Na{sub 2}U{sub 2}O{sub 7} layers are similar as in K{sub 2}U{sub 2}O{sub 7}, but with a different stacking sequence of the layers. The layers in β-Na{sub 2}U{sub 2}O{sub 7} are more symmetric. The relationship with the compounds A{sub 2}U{sub 2}O{sub 7} (A=K, Rb, and Cs) is discussed. - Graphical abstract: The U{sub 2}O{sub 7} layer of α-Na{sub 2}U{sub 2}O{sub 7} (left) at 293 K and of β-Na{sub 2}U{sub 2}O{sub 7} (right) at 773 K determined by neutron diffraction. Some Na atoms between the layers are visible. - Highlights: • Na{sub 2}U{sub 2}O{sub 7} has been prepared by means of a solid state reaction. • The structure has been determined using neutron diffraction. • At 293 K, the compound adopts a monoclinic structure with space group P2{sub 1}/a. • The structure at 773 K is closely related, and is described in the space group C2/m.

  11. Neutron detectors comprising boron powder

    DOE Patents [OSTI]

    Wang, Zhehui; Morris, Christopher; Bacon, Jeffrey Darnell; Makela, Mark F; Spaulding, Randy Jay

    2013-05-21

    High-efficiency neutron detector substrate assemblies comprising a first conductive substrate, wherein a first side of the substrate is in direct contact with a first layer of a powder material comprising .sup.10boron, .sup.10boron carbide or combinations thereof, and wherein a conductive material is in proximity to the first layer of powder material; and processes of making said neutron detector substrate assemblies.

  12. Neutron powder diffraction study of the layer organic-inorganic hybrid iron(II) methylphosphonate-hydrate, Fe[(CD{sub 3}PO{sub 3})(D{sub 2}O)

    SciTech Connect (OSTI)

    Leone, Philippe Bellitto, Carlo; Bauer, Elvira M.; Righini, Guido; Andre, Gilles; Bouree, Francoise

    2008-11-15

    The crystal and magnetic structures of the hybrid organic-inorganic layer compound Fe[(CD{sub 3}PO{sub 3})(D{sub 2}O)] have been studied by neutron powder diffraction as a function of temperature down to 1.5 K. The neutron diffraction pattern recorded at 200 K shows that the fully deuterated compound crystallizes in one of the two known forms of the undeuterated Fe[(CH{sub 3}PO{sub 3})(H{sub 2}O)]. The crystal structure is orthorhombic, space group Pmn2{sub 1}, with the following unit-cell parameters: a=5.7095(1) A, b=8.8053(3) A and c=4.7987(1) A; Z=2. The crystal structure remains unchanged on cooling from 200 to 1.5 K. Moreover, at low temperature, Fe[(CD{sub 3}PO{sub 3})(D{sub 2}O)] shows a commensurate magnetic structure (k=(0,0,0)). As revealed by bulk susceptibility measurements on Fe[(CH{sub 3}PO{sub 3})(H{sub 2}O)], the magnetic structure corresponds to a canted antiferromagnet with a critical temperature T{sub N}=25 K. Neutron powder diffraction reveals that below T{sub N}=23.5 K the iron magnetic moments in Fe[(CD{sub 3}PO{sub 3})(D{sub 2}O)] are antiferromagnetically coupled and oriented along the b-axis, perpendicular to the inorganic layers. No ferromagnetic component is observable in the neutron powder diffraction experiment, due to its too small value (<0.1{mu}{sub B}). - Graphical abstract: Crystal structure and magnetic structure of Fe[(CD{sub 3}PO{sub 3})(D{sub 2}O)].

  13. High-Pressure and High-Temperature Powder Diffraction (Journal...

    Office of Scientific and Technical Information (OSTI)

    High-Pressure and High-Temperature Powder Diffraction Citation Details In-Document Search Title: High-Pressure and High-Temperature Powder Diffraction Authors: Fei, Yingwei ; Wang, ...

  14. Palladium deuteride formation in the cathode of an electrochemical cell: An in situ neutron diffraction study

    SciTech Connect (OSTI)

    Rotella, F.J.; Richardson, J.W. Jr.; Redey, L.; Felcher, G.P.; Hitterman, R.L.; Kleb, R.

    1991-01-01

    In this report, neutron diffraction of palladium cathodes is utilized to reveal palladium deuteride formation within the crystal structure of the metal. The experiment described in this report demonstrates the efficacy of neutron powder diffraction as a tool for structural studies of metal deuterides/hydrides and the feasibility of in situ diffraction measurements from a working electrochemical cell. (JL)

  15. Palladium deuteride formation in the cathode of an electrochemical cell: An in situ neutron diffraction study

    SciTech Connect (OSTI)

    Rotella, F.J.; Richardson, J.W. Jr.; Redey, L.; Felcher, G.P.; Hitterman, R.L.; Kleb, R.

    1991-12-31

    In this report, neutron diffraction of palladium cathodes is utilized to reveal palladium deuteride formation within the crystal structure of the metal. The experiment described in this report demonstrates the efficacy of neutron powder diffraction as a tool for structural studies of metal deuterides/hydrides and the feasibility of in situ diffraction measurements from a working electrochemical cell. (JL)

  16. Clifford G. Shull, Neutron Diffraction, Hydrogen Atoms, and Neutron...

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    ... Laue Photography of Neutron Diffraction; Physical Review, Vol 73, Issue 5, 527-528, March 1, 1948 The Crystal Structure of Thorium and Zirconium Dihydrides by X-ray and Neutron ...

  17. Hydrogen in polar intermetallics: Syntheses and structures of the ternary Ca5Bi3D0.93, Yb5Bi3Hx, and Sm5Bi3H~1 by powder neutron or single crystal X-ray diffraction

    SciTech Connect (OSTI)

    Leon-Escamilla, E. Alejandro; Dervenagas, Panagiotis; Stasis, Constantine; Corbett, John D.

    2010-01-01

    The syntheses of the title compounds are described in detail. Structural characterizations from refinements of single crystal X-ray diffraction data for Yb{sub 5}Bi{sub 3}H{sub x} and Sm{sub 5}Bi{sub 3}H{sub 1} and of powder neutron diffraction data for Ca{sub 5}Bi{sub 3}D{sub 0.93(3)} are reported. These confirm that all three crystallize with the heavy atom structure type of {beta}-Yb{sub 5}Sb{sub 3}, and the third gives the first proof that the deuterium lies in the center of nominal calcium tetrahedra, isostructural with the Ca{sub 5}Sb{sub 3}F-type structure. These Ca and Yb phases are particularly stable with respect to dissociation to Mn{sub 5}Si{sub 3}-type product plus H{sub 2}. Some contradictions in the literature regarding Yb{sub 5}Sb{sub 3} and Yb{sub 5}Sb{sub 3}H{sub x} phases are considered in terms of adventitious hydrogen impurities that are generated during reactions in fused silica containers at elevated temperatures.

  18. Quality experimental and calculated powder x-ray diffraction

    SciTech Connect (OSTI)

    Sullenger, D.B.; Cantrell, J.S.; Beiter, T.A.; Tomlin, D.W.

    1996-08-01

    For several years, we have submitted quality powder XRD patterns to the International Centre for Diffraction Data for inclusion as reference standards in their Powder Diffraction File. The procedure followed is described; examples used are {beta}-UH{sub 3}, {alpha}- BaT{sub 2}, alpha-lithium disilicate ({alpha}-Li{sub 2}Si{sub 2}O{sub 5}), and 2,2`,4,4`,6,6`hexanitroazobenzene-III (HNAB-III).

  19. Structural characterization of Bi{sub 2}Te{sub 3} and Sb{sub 2}Te{sub 3} as a function of temperature using neutron powder diffraction and extended X-ray absorption fine structure techniques

    SciTech Connect (OSTI)

    Mansour, A. N.; Wong-Ng, W.; Huang, Q.; Tang, W.; Thompson, A.; Sharp, J.

    2014-08-28

    The structure of Bi{sub 2}Te{sub 3} (Seebeck coefficient Standard Reference Material (SRM™ 3451)) and the related phase Sb{sub 2}Te{sub 3} have been characterized as a function of temperature using the neutron powder diffraction (NPD) and the extended X-ray absorption fine structure (EXAFS) techniques. The neutron structural studies were carried out from 20 K to 300 K for Bi{sub 2}Te{sub 3} and from 10 K to 298 K for Sb{sub 2}Te{sub 3}. The EXAFS technique for studying the local structure of the two compounds was conducted from 19 K to 298 K. Bi{sub 2}Te{sub 3} and Sb{sub 2}Te{sub 3} are isostructural, with a space group of R3{sup ¯}m. The structure consists of repeated quintuple layers of atoms, Te2-M-Te1-M-Te2 (where M = Bi or Sb) stacking along the c-axis of the unit cell. EXAFS was used to examine the bond distances and static and thermal disorders for the first three shells of Bi{sub 2}Te{sub 3} and Sb{sub 2}Te{sub 3} as a function of temperature. The temperature dependencies of thermal disorders were analyzed using the Debye and Einstein models for lattice vibrations. The Debye and Einstein temperatures for the first two shells of Bi{sub 2}Te{sub 3} are similar to those of Sb{sub 2}Te{sub 3} within the uncertainty in the data. However, the Debye and Einstein temperatures for the third shell of Bi-Bi are significantly lower than those of the third shell of Sb-Sb. The Einstein temperature for the third shell is consistent with a soft phonon mode in both Bi{sub 2}Te{sub 3} and Sb{sub 2}Te{sub 3}. The lower Einstein temperature of Bi-Bi relative to Sb-Sb is consistent with the lower value of thermal conductivity of Bi{sub 2}Te{sub 3} relative to Sb{sub 2}Te{sub 3}.

  20. The Advanced Automation for Powder Diffraction toward Industrial Application

    SciTech Connect (OSTI)

    Osaka, Keiichi; Matsumoto, Takuya; Miura, Keiko; Sato, Masugu; Hirosawa, Ichiro; Watanabe, Yoshio

    2010-06-23

    A highly automated system for powder diffraction with synchrotron radiation was installed on the large Debye-Scherrer camera at the BL19B2 Engineering Science Research I beamline of SPring-8. Combined with a sample transfer and an automated centering system, we have succeeded in increasing the ratio of exposure time in the user beam time to 85%. The proposed system can be applied to a wide range of industrial uses.

  1. Structural properties of Sr{sub 0.61}Ba{sub 0.39}Nb{sub 2}O{sub 6} in the temperature range 10-500 K investigated by high-resolution neutron powder diffraction and specific heat measurements

    SciTech Connect (OSTI)

    Schefer, J.; Pomjakushin, V.; Stuhr, U.; Schaniel, D.; Woike, Th.; Petricek, V.; Woehlecke, M.; Imlau, M.

    2006-10-01

    We report high-resolution neutron powder diffraction on Sr{sub 0.61}Ba{sub 0.39}Nb{sub 2}O{sub 6} in the temperature range 15-500 K. The results indicate that the low-temperature anomalies (T{<=}100 K) observed in the dielectric dispersion are due to small changes in the incommensurate modulation of the NbO{sub 6} octahedra, as no structural phase transition of the average structure was observed. This interpretation is supported by specific heat measurements, which show no latent heat, but a glass-like behavior at low temperatures. Furthermore, we find that the structural changes connected with the ferroelectric phase transition at T{sub c}{approx_equal}350 K start already at 200 K, explaining the anisotropic thermal expansion in the temperature range 200-300 K observed in a recent x-ray diffraction study.

  2. Neutron detectors comprising ultra-thin layers of boron powder

    DOE Patents [OSTI]

    Wang, Zhehul; Morris, Christopher

    2013-07-23

    High-efficiency neutron detector substrate assemblies comprising a first conductive substrate, wherein a first side of the substrate is in direct contact with a first layer of a powder material having a thickness of from about 50 nm to about 250 nm and comprising .sup.10boron, .sup.10boron carbide or combinations thereof, and wherein a conductive material is in proximity to the first layer of powder material; and processes of making said neutron detector substrate assemblies.

  3. LANSCE | Lujan Center | Highlights | In situ neutron diffraction study of

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    CO clathrate hydrate In situ neutron diffraction study of CO clathrate hydrate The structure of a CO clathrate hydrate has been studied for the first time using high-P low-T neutron diffraction. Clathrate Rietveld analysis shows that lattice parameter a (SII cubic clathrate structure) increases with increasing temperature. CO molecules are positionally disordered and off-centered in both large and small cages. Each large cage is occupied by two CO molecules while each small cage is occupied

  4. High throughput screening of ligand binding to macromolecules using high resolution powder diffraction

    DOE Patents [OSTI]

    Von Dreele, Robert B.; D'Amico, Kevin

    2006-10-31

    A process is provided for the high throughput screening of binding of ligands to macromolecules using high resolution powder diffraction data including producing a first sample slurry of a selected polycrystalline macromolecule material and a solvent, producing a second sample slurry of a selected polycrystalline macromolecule material, one or more ligands and the solvent, obtaining a high resolution powder diffraction pattern on each of said first sample slurry and the second sample slurry, and, comparing the high resolution powder diffraction pattern of the first sample slurry and the high resolution powder diffraction pattern of the second sample slurry whereby a difference in the high resolution powder diffraction patterns of the first sample slurry and the second sample slurry provides a positive indication for the formation of a complex between the selected polycrystalline macromolecule material and at least one of the one or more ligands.

  5. Electrostatic levitation facility optimized for neutron diffraction...

    Office of Scientific and Technical Information (OSTI)

    studies of high temperature liquids at a spallation neutron source Authors: Mauro, N. A. 1 ; Vogt, A. J. 2 Search DOE PAGES for author "Vogt, A. J." Search DOE PAGES for ...

  6. Determination of the response of pentaerythritol tetranitrate to static high pressure up to 4.2 GPa by neutron diffraction

    SciTech Connect (OSTI)

    Dick, J.J.; Dreele, R.B. von

    1997-11-01

    Neutron powder diffraction experiments were performed on pentaerythritol tetranitrate explosive up to 4.28 GPa. For deuterated samples the changes in lattice parameters, intramolecular torsional angles and molecular rotation were measured. The lattice parameter changes were different from those observed in protonated samples. However, there is no evidence of a phase transition or change in molecular symmetry.

  7. Total-scattering pair-distribution function of organic material from powder electron diffraction data

    SciTech Connect (OSTI)

    Gorelik, Tatiana E.; Billinge, Simon J. L.; Schmidt, Martin U.; Kolb, Ute

    2015-04-01

    This paper shows for the first time that pair-distribution function analyses can be carried out on organic and organo-metallic compounds from powder electron diffraction data. Different experimental setups are demonstrated, including selected area electron diffraction (SAED) and nanodiffraction in transmission electron microscopy (TEM) or nanodiffraction in scanning transmission electron microscopy (STEM) modes. The methods were demonstrated on organo-metallic complexes (chlorinated and unchlorinated copper-phthalocyanine) and on purely organic compounds (quinacridone). The PDF curves from powder electron diffraction data, called ePDF, are in good agreement with PDF curves determined from X-ray powder data demonstrating that the problems of obtaining kinematical scattering data and avoiding beam-damage of the sample are possible to resolve.

  8. Total-scattering pair-distribution function of organic material from powder electron diffraction data

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Gorelik, Tatiana E.; Billinge, Simon J. L.; Schmidt, Martin U.; Kolb, Ute

    2015-04-01

    This paper shows for the first time that pair-distribution function analyses can be carried out on organic and organo-metallic compounds from powder electron diffraction data. Different experimental setups are demonstrated, including selected area electron diffraction (SAED) and nanodiffraction in transmission electron microscopy (TEM) or nanodiffraction in scanning transmission electron microscopy (STEM) modes. The methods were demonstrated on organo-metallic complexes (chlorinated and unchlorinated copper-phthalocyanine) and on purely organic compounds (quinacridone). The PDF curves from powder electron diffraction data, called ePDF, are in good agreement with PDF curves determined from X-ray powder data demonstrating that the problems of obtaining kinematical scattering datamore » and avoiding beam-damage of the sample are possible to resolve.« less

  9. Long-range magnetic ordering in Ba{sub 2}CoS{sub 3}: A neutron diffraction study

    SciTech Connect (OSTI)

    Headspith, D.A. [Department of Chemistry, University of Hull, Cottingham Road, Hull HU6 7RX (United Kingdom); Battle, P.D. [Inorganic Chemistry Laboratory, Oxford University, South Parks Road, Oxford OX1 3QR (United Kingdom); Francesconi, M.G. [Department of Chemistry, University of Hull, Cottingham Road, Hull HU6 7RX (United Kingdom)], E-mail: m.g.francesconi@hull.ac.uk

    2007-10-15

    Neutron powder diffraction has been used to determine the magnetic structure of the quasi-one-dimensional compound Ba{sub 2}CoS{sub 3}, which contains linear [001] chains of vertex-sharing CoS{sub 4} tetrahedra, spaced apart by Ba{sup 2+} cations. At 1.5 K the Co{sup 2+} cations in the chains are antiferromagnetically ordered with an ordered magnetic moment of 1.97(4) {mu}{sub B} per cation aligned along [100]. Each Co{sup 2+} cation is ferromagnetically aligned with four cation in neighbouring chains and antiferromagnetically aligned with two others. - Graphical abstract: Neutron powder diffraction has been used to prove that Ba{sub 2}CoS{sub 3} shows long-range antiferromagnetic order at low temperatures, despite the quasi-one-dimensional arrangement of the CoS{sub 4} tetrahedra in the crystal structure.

  10. Double helix boron-10 powder thermal neutron detector

    DOE Patents [OSTI]

    Wang, Zhehui; Morris, Christopher L.; Bacon, Jeffrey D.

    2015-06-02

    A double-helix Boron-10 powder detector having intrinsic thermal neutron detection efficiency comparable to 36'' long, 2-in diameter, 2-bar Helium-3 detectors, and which can be used to replace such detectors for use in portal monitoring, is described. An embodiment of the detector includes a metallic plate coated with Boron-10 powder for generating alpha and Lithium-7 particles responsive to neutrons impinging thereon supported by insulators affixed to at least two opposing edges; a grounded first wire wound in a helical manner around two opposing insulators; and a second wire having a smaller diameter than that of the first wire, wound in a helical manner around the same insulators and spaced apart from the first wire, the second wire being positively biased. A gas, disposed within a gas-tight container enclosing the plate, insulators and wires, and capable of stopping alpha and Lithium-7 particles and generating electrons produces a signal on the second wire which is detected and subsequently related to the number of neutrons impinging on the plate.

  11. A New Camera for Powder Diffraction of Macromolecular Crystallography at SPring-8

    SciTech Connect (OSTI)

    Miura, Keiko; Inoue, Katsuaki; Goto, Shunji; Ishikawa, Tetsuya; Yamamoto, Masaki; Ueki, Tatzuo

    2004-05-12

    A powder diffractometer of Guinier geometry was developed and tested on a beamline, BL40B2, at SPring-8. The long specimen-to-detector distance, 1,000 mm, is advantageous in recording diffraction from Bragg spacing of 20 nm or larger. The angular resolution, 0.012 degrees, was realized together with the focusing optics, the long specimen-to-detector distance and the small pixel size of Blue-type Imaging Plate detector. Such a high resolution makes the peak separation possible in the powder diffraction from microcrystals with large unit cell and low symmetry of biological macromolecules.

  12. Neutron diffraction measurements and micromechanical modelling of temperature-dependent variations in TATB lattice parameters

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Yeager, John D.; Luscher, Darby J.; Vogel, Sven C.; Clausen, Bjorn; Brown, Donald W.

    2016-06-01

    Triaminotrinitrobenzene (TATB) is a highly anisotropic molecular crystal used in several plastic-bonded explosive (PBX) formulations. TATB-based explosives exhibit irreversible volume expansion (“ratchet growth”) when thermally cycled. A theoretical understanding of the relationship between anisotropy of the crystal, crystal orientation distribution (texture) of polycrystalline aggregates, and the intergranular interactions leading to this irreversible growth is necessary to accurately develop physics-based predictive models for TATB-based PBXs under various thermal environments. In this work, TATB lattice parameters were measured using neutron diffraction during thermal cycling of loose powder and a pressed pellet. The measured lattice parameters help clarify conflicting reports in the literaturemore » as these new results are more consistent with one set of previous results than another. The lattice parameters of pressed TATB were also measured as a function of temperature, showing some differences from the powder. This data is used along with anisotropic single-crystal stiffness moduli reported in the literature to model the nominal stresses associated with intergranular constraints during thermal expansion. The texture of both specimens were characterized and the pressed pellet exhibits preferential orientation of (001) poles along the pressing direction, whereas no preferred orientation was found for the loose powder. Lastly, thermal strains for single-crystal TATB computed from lattice parameter data for the powder is input to a self-consistent micromechanical model, which predicts the lattice parameters of the constrained TATB crystals within the pellet. The agreement of these model results with the diffraction data obtained from the pellet is discussed along with future directions of research.« less

  13. High-resolution neutron diffraction study of CuNCN: New evidence of structure anomalies at low temperature

    SciTech Connect (OSTI)

    Jacobs, Philipp; Houben, Andreas; Dronskowski, Richard; Tchougreff, Andrei L.; Lomonosov Moscow State University, Department of Chemistry and Poncelet Laboratory of Mathematics in Interaction with Physics and Informatics, Independent University of Moscow, Moscow Center for Continuous Mathematical Education, Bolshoi Vlasevsky Per. 11, 119002 Moscow

    2013-12-14

    Copper carbodiimide (CuNCN) is the nitrogen-containing analogue of cupric oxide. Based on high-resolution neutron-diffraction data, CuNCN's lattice parameters are derived as a function of the temperature. In accordance with a recent synchrotron study, a clear trend in the cell parameter a is observed accompanying the changing magnetic behavior. With decreasing temperature, a slowly decreases to a minimum at ?100 K after which it rises again. The same trendalbeit more pronouncedis observed for the c lattice parameter at ?35 K. The herein presented neutron powder-diffraction data also support the conjectured sequence of transitions from the high-temperature one-dimensional resonating valence-bond (RVB) state to a transient two-dimensional RVB state and eventually, at lowest temperatures, into another two-dimensional RVB state, presumably the ground state.

  14. Six-axis multi-anvil press for high-pressure, high-temperature neutron diffraction experiments

    SciTech Connect (OSTI)

    Sano-Furukawa, A. Hattori, T.; Arima, H.; Yamada, A.; Tabata, S.; Kondo, M.; Nakamura, A.; Kagi, H.; Yagi, T.

    2014-11-15

    We developed a six-axis multi-anvil press, ATSUHIME, for high-pressure and high-temperature in situ time-of-flight neutron powder diffraction experiments. The press has six orthogonally oriented hydraulic rams that operate individually to compress a cubic sample assembly. Experiments indicate that the press can generate pressures up to 9.3 GPa and temperatures up to 2000 K using a 6-6-type cell assembly, with available sample volume of about 50 mm{sup 3}. Using a 6-8-type cell assembly, the available conditions expand to 16 GPa and 1273 K. Because the six-axis press has no guide blocks, there is sufficient space around the sample to use the aperture for diffraction and place an incident slit, radial collimators, and a neutron imaging camera close to the sample. Combination of the six-axis press and the collimation devices realized high-quality diffraction pattern with no contamination from the heater or the sample container surrounding the sample. This press constitutes a new tool for using neutron diffraction to study the structures of crystals and liquids under high pressures and temperatures.

  15. Density functional and neutron diffraction studies of lithium polymer electrolytes.

    SciTech Connect (OSTI)

    Baboul, A. G.

    1998-06-26

    The structure of PEO doped with lithium perchlorate has been determined using neutron diffraction on protonated and deuterated samples. The experiments were done in the liquid state. Preliminary analysis indicates the Li-O distance is about 2.0 {angstrom}. The geometries of a series of gas phase lithium salts [LiCF{sub 3}SO{sub 3}, Li(CF{sub 3}SO{sub 2}){sub 2}N, Li(CF{sub 3}SO{sub 2}){sub 2}CH, LiClO{sub 4}, LiPF{sub 6}, LiAsF{sub 6}] used in polymer electrolytes have been optimized at B3LYP/6-31G(d) density functional level of theory. All local minima have been identified. For the triflate, imide, methanide, and perchlorate anions, the lithium cation is coordinated to two oxygens and have binding energies of ca 141 kcal/mol at the B3LYP/6-311+G(3df,2p)/B3LYP/6-31G* level of theory. For the hexafluoroarsenate and hexafluorophosphate the lithium cation is coordinated to three oxygens and have binding energies of ca. 136 kcal/mol.

  16. The early development of neutron diffraction: Science in the wings of the Manhattan Project

    SciTech Connect (OSTI)

    Mason, Thom; Gawne, Timothy J; Nagler, Stephen E; Nestor, Margaret Boone {Bonnie}; Carpenter, John M

    2012-01-01

    Although neutron diffraction was first observed using radioactive decay sources shortly after the discovery of the neutron, it was only with the availability of higher intensity neutron beams from the first nuclear reactors, constructed as part of the Manhattan project, that systematic investigation of Bragg scattering became possible. Remarkably, at a time when the war effort was singularly focused on the development of the atomic bomb, groups working at Oak Ridge and Chicago carried out key measurements and recognized the future utility of neutron diffraction quite independent of its contributions to the measurements of nuclear cross sections. Ernest O. Wollan, Lyle B. Borst, and Walter H. Zinn were all able to observe neutron diffraction in 1944 using the X-10 graphite reactor and the CP-3 heavy water reactor.

  17. The early development of neutron diffraction: science in the wings of the Manhattan Project

    SciTech Connect (OSTI)

    Mason, T. E. Gawne, T. J.; Nagler, S. E.; Nestor, M. B.; Carpenter, J. M.

    2013-01-01

    Early neutron diffraction experiments performed in 1944 using the first nuclear reactors are described. Although neutron diffraction was first observed using radioactive decay sources shortly after the discovery of the neutron, it was only with the availability of higher intensity neutron beams from the first nuclear reactors, constructed as part of the Manhattan Project, that systematic investigation of Bragg scattering became possible. Remarkably, at a time when the war effort was singularly focused on the development of the atomic bomb, groups working at Oak Ridge and Chicago carried out key measurements and recognized the future utility of neutron diffraction quite independent of its contributions to the measurement of nuclear cross sections. Ernest O. Wollan, Lyle B. Borst and Walter H. Zinn were all able to observe neutron diffraction in 1944 using the X-10 graphite reactor and the CP-3 heavy water reactor. Subsequent work by Wollan and Clifford G. Shull, who joined Wollan’s group at Oak Ridge in 1946, laid the foundations for widespread application of neutron diffraction as an important research tool.

  18. Kinetics of Methane Hydrate Decomposition Studied via in Situ Low Temperature X-ray Powder Diffraction

    SciTech Connect (OSTI)

    Everett, Susan M; Rawn, Claudia J; Keffer, David J.; Mull, Derek L; Payzant, E Andrew; Phelps, Tommy Joe

    2013-01-01

    Gas hydrates are known to have a slowed decomposition rate at ambient pressure and temperatures below the melting point of ice termed self-preservation or anomalous preservation. As hydrate exothermically decomposes, gas is released and water of the clathrate cages transforms into ice. Two regions of slowed decomposition for methane hydrate, 180 200 K and 230 260 K, were observed, and the kinetics were studied by in situ low temperature x-ray powder diffraction. The kinetic constants for ice formation from methane hydrate were determined by the Avrami model within each region and activation energies, Ea, were determined by the Arrhenius plot. Ea determined from the data for 180 200 K was 42 kJ/mol and for 230 260 K was 22 kJ/mol. The higher Ea in the colder temperature range was attributed to a difference in the microstructure of ice between the two regions.

  19. Single phase synthesis and room temperature neutron diffraction studies on multiferroic PbFe{sub 0.5}Nb{sub 0.5}O{sub 3}

    SciTech Connect (OSTI)

    Matteppanavar, Shidaling; Angadi, Basavaraj; Rayaprol, Sudhindra

    2013-02-05

    The lead-iron-niobate, (PbFe{sub 0.5}Nb{sub 0.5}O{sub 3} or PFN) was synthesized by low temperature sintering Single Step / Solid State Reaction Method. The 700 Degree-Sign C/2 hrs. calcined powder was sintered at 1050 Degree-Sign C/1 hr. The sintered pellets were characterized through X-Ray Diffraction and Neutron Diffraction at room temperature. It is found from the XRD pattern that the materials is in single phase with no traces of pyrochlore phase. It was also confirmed from the neutron diffraction pattern, the structure of PFN to be monoclinic, space group Cm. Structural studies has been carried out by refining the obtained neutron diffraction data by Rietveld refinement method using Fullprof program. The neutron diffraction pattern at 300 K (room temperature) was selected to refine the structure. The lattice parameters obtained are; a = 5.6709 A, b = 5.6732 A, c = 4.0136 A, and {alpha}= 90, {beta}= 89.881, {gamma}= 90. The P-E measurements showed hysteretic behavior with high remnant polarization.

  20. Neutron diffraction and X-ray absorption study of Ag{sub 5}Pb{sub 2}O{sub 6}

    SciTech Connect (OSTI)

    Yoshii, K. Mizumaki, M.; Kato, K.; Uruga, T.; Abe, H.; Nakamura, A.; Shimojo, Y.; Ishii, Y.; Morii, Y.

    2007-01-15

    Neutron diffraction and X-ray absorption measurements were carried out for a silver-lead oxide Ag{sub 5}Pb{sub 2}O{sub 6}. The powder neutron diffraction patterns could be fitted to the trigonal P3-bar 1m structure, as was found by X-ray diffraction. From the bond-valence-sum (BVS) analysis, the valences of the Ag and Pb ions were estimated to be about 1+ and 3.7+, respectively. The X-ray absorption measurements indicated that the ionic state of Ag is close to 1+, while that of Pb stands between 3+ and 4+. The deviation of the valence of the Pb ion from 4+ suggests a contribution of Pb orbitals to the metallic conduction as well as the possible superconductivity of this material, consistently with a recent band-structure calculation.

  1. Neutron diffraction measurements of residual stresses in friction stir welding: a review

    SciTech Connect (OSTI)

    Woo, Wan Chuck [ORNL; Feng, Zhili [ORNL; Wang, Xun-Li [ORNL; David, Stan A [ORNL

    2011-01-01

    Significant amounts of residual stresses are often generated during welding and result in critical degradation of the structural integrity and performance of components. Neutron diffraction has become a well established technique for the determination of residual stresses in welds because of the unique deep penetration, three-dimensional mapping capability, and volume averaged bulk measurements characteristic of the scattering neutron beam. Friction stir welding has gained prominence in recent years. The authors reviewed a number of neutron diffraction measurements of residual stresses in friction stir welds and highlighted examples addressing how the microstructures and residual stresses are correlated with each other. An example of in situ neutron diffraction measurement result shows the evolution of the residual stresses during welding.

  2. In-Situ Neutron Diffraction Studies of Complex Hydrogen Storage Materials

    SciTech Connect (OSTI)

    Yelon, William B.

    2013-05-13

    should make it a very valuable resource for the study of oxides being considered for application to solid oxide fuel cells (SOFCs), in that materials can be studied at potential operating temperatures in both reducing and oxidizing environments to determine their stoichiometry, and lattice parameters. Our research, which was predicated, in part, on the use of hydrogenous samples (as opposed to deuteration), demonstrated that such studies are feasible and can yield high quality, refinable data. The precision of the refined hydrogen positions appears to be more than adequate for theory calculations (molecular modeling-thermodynamics) and the uncertainty is certainly less than that achieved by attempting to extrapolate the hydrogen positions from refined deuterium positions. In fact the 2008 annual report from the Institute Laue Langevin (ILL), the world's premier neutron scattering laboratory, highlights: Another trend is the increasing interest in hydrogen. This defies the widespread assumption that neutron diffraction experiments need to be done at deuterated samples. In situ experiments on phase transitions involving hydrogen and in particular on the real time behaviour of hydrogen-storage systems increase in number and scope. Our work in this area predates the ILL efforts be several years. Unfortunately, the productivity of our program was significantly curtailed by the unavailability of the MURR powder diffractometer for almost all of the second years of the project. The diffractometer was disassembled to allow partial extraction of the beam tube and replacement of the graphite element that is penetrated by the beam tube. Re-commissioning of the instrument was substantially delayed by errors of the MURR engineering staff, which failed to properly reinstall the sapphire filter that conditions the beam prior to the neutron monochromator, and reduces the radiological background to acceptable levels.

  3. Pressure/temperature fluid cell apparatus for the neutron powder diffractometer instrument: Probing atomic structure in situ

    SciTech Connect (OSTI)

    Wang, Hsiu-Wen; Fanelli, Victor R.; Reiche, Helmut M.; Larson, Eric; Taylor, Mark A.; Siewenie, Joan; Xu, Hongwu; Zhu, Jinlong; Page, Katharine

    2014-12-15

    This contribution describes a new local structure compatible gas/liquid cell apparatus for probing disordered materials at high pressures and variable temperatures in the Neutron Powder Diffraction instrument at the Lujan Neutron Scattering Center, Los Alamos National Laboratory. The new sample environment offers choices for sample canister thickness and canister material type. Finite element modeling is utilized to establish maximum allowable working pressures of 414 MPa at 15 K and 121 MPa at 600 K. High quality atomic pair distribution function data extraction and modeling have been demonstrated for a calibration standard (Si powder) and for supercritical and subcritical CO{sub 2} measurements. The new sample environment was designed to specifically target experimental studies of the local atomic structures involved in geologic CO{sub 2} sequestration, but will be equally applicable to a wide variety of energy applications, including sorption of fluids on nano/meso-porous solids, clathrate hydrate formation, catalysis, carbon capture, and H{sub 2} and natural gas uptake/storage.

  4. Pressure/temperature fluid cell apparatus for the neutron powder diffractometer instrument: Probing atomic structure in situ

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Wang, Hsiu -Wen; Fanelli, Victor R.; Reiche, Helmut M.; Larson, Eric; Taylor, Mark A.; Xu, Hongwu; Zhu, Jinlong; Siewenie, Joan; Page, Katharine

    2014-12-24

    This contribution describes a new local structure compatible gas/liquid cell apparatus for probing disordered materials at high pressures and variable temperatures in the Neutron Powder Diffraction instrument at the Lujan Neutron Scattering Center, Los Alamos National Laboratory. The new sample environment offers choices for sample canister thickness and canister material type. Finite element modeling is utilized to establish maximum allowable working pressures of 414 MPa at 15 K and 121 MPa at 600 K. High quality atomic pair distribution function data extraction and modeling have been demonstrated for a calibration standard (Si powder) and for supercritical and subcritical CO2measurements. Asmore » a result, the new sample environment was designed to specifically target experimental studies of the local atomic structures involved in geologic CO2 sequestration, but will be equally applicable to a wide variety of energy applications, including sorption of fluids on nano/meso-porous solids, clathrate hydrate formation, catalysis, carbon capture, and H2 and natural gas uptake/storage.« less

  5. in-situ chemistry mapping of hydrogen storage materials by neutron diffraction

    SciTech Connect (OSTI)

    Payzant, E Andrew; Bowman Jr, Robert C; Johnson, Terry A; Jorgensen, Scott W

    2013-01-01

    Neutron diffraction was used to nondestructively study the microstructures for two hydrogen storage media systems. In the first case, sodium alanate based hydrogen storage is a vehicle-scale candidate system developed by Sandia/GM. Neutron scattering was used to determine the distribution of phases in the storage media at different hydrogen loading levels, to help understand the absorption/desorption of hydrogen in large-scale systems. This study also included a 3D neutron tomographic study of the microstructure. In the second case, tin-doped lanthanum nickel alloys have been studied at JPL for space-based applications, for which the gradual degradation of the material due to segregation and disproportionation of phases is a known problem. A regenerative process developed to restore the storage properties of these alloys was studied, using in-situ neutron diffraction to relate the microstructure to the thermodynamic simulations.

  6. Calculations of single crystal elastic constants for yttria partially stabilised zirconia from powder diffraction data

    SciTech Connect (OSTI)

    Lunt, A. J. G. Xie, M. Y.; Baimpas, N.; Korsunsky, A. M.; Zhang, S. Y.; Kabra, S.; Kelleher, J.; Neo, T. K.

    2014-08-07

    Yttria Stabilised Zirconia (YSZ) is a tough, phase-transforming ceramic that finds use in a wide range of commercial applications from dental prostheses to thermal barrier coatings. Micromechanical modelling of phase transformation can deliver reliable predictions in terms of the influence of temperature and stress. However, models must rely on the accurate knowledge of single crystal elastic stiffness constants. Some techniques for elastic stiffness determination are well-established. The most popular of these involve exploiting frequency shifts and phase velocities of acoustic waves. However, the application of these techniques to YSZ can be problematic due to the micro-twinning observed in larger crystals. Here, we propose an alternative approach based on selective elastic strain sampling (e.g., by diffraction) of grain ensembles sharing certain orientation, and the prediction of the same quantities by polycrystalline modelling, for example, the Reuss or Voigt average. The inverse problem arises consisting of adjusting the single crystal stiffness matrix to match the polycrystal predictions to observations. In the present model-matching study, we sought to determine the single crystal stiffness matrix of tetragonal YSZ using the results of time-of-flight neutron diffraction obtained from an in situ compression experiment and Finite Element modelling of the deformation of polycrystalline tetragonal YSZ. The best match between the model predictions and observations was obtained for the optimized stiffness values of C11 = 451, C33 = 302, C44 = 39, C66 = 82, C12 = 240, and C13 = 50 (units: GPa). Considering the significant amount of scatter in the published literature data, our result appears reasonably consistent.

  7. X-Ray Powder Diffraction Study of Synthetic Palmierite, K{sub 2}Pb(SO{sub 4}){sub 2}

    SciTech Connect (OSTI)

    TISSOT JR.,RALPH G.; RODRIGUEZ,MARK A.; SIPOLA,DIANA L.; VOIGT,JAMES A.

    2000-12-19

    Palmierite (K{sub 2}Pb(SO{sub 4}){sub 2}) has been prepared via a chemical synthesis method. Intensity differences were observed when X-ray powder data from the newly synthesized compound were compared to the published powder diffraction card (PDF) 29-1015 for Palmierite. Investigation of these differences indicated the possibility of preferred orientation and/or chemical inhomogeneity affecting intensities, particularly those of the basal (00{ell}) reflections. Annealing of the Palmierite was found to reduce the effects of preferred orientation. Electron microprobe analysis confirmed K:Pb:S as 2:1:2 for the annealed Palmierite powder. Subsequent least-squares refinement and Rietveld analysis of the annealed powder showed peak intensities very close to that of a calculated Palmierite pattern (based on single crystal data), yet substantially higher than many of the PDF 29-1015 published intensities. Further investigation of peak intensity variation via calculated patterns suggested that the intensity discrepancies between the annealed sample and those found in PDF 29-1015 were potentially due to chemical variation in the K{sub 2}Pb(SO{sub 4}){sub 2} composition. X-ray powder diffraction and crystal data for Palmierite are reported for the annealed sample. Palmierite is Trigonal/Hexagonal with unit cell parameters a = 5.497(1){angstrom}, c = 20.864(2) {angstrom}, space group R-3m (166), and Z = 3.

  8. Oxygen transport pathways in Ruddlesden–Popper structured oxides revealed via in situ neutron diffraction

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Tomkiewicz, Alex C.; Tamimi, Mazin; Huq, Ashfia; McIntosh, Steven

    2015-09-21

    Ruddlesden-Popper structured oxides, general form An+1BnO3n+1, consist of n-layers of the perovskite structure stacked in between rock-salt layers, and have potential application in solid oxide electrochemical cells and ion transport membrane reactors. Three materials with constant Co/Fe ratio, LaSrCo0.5Fe0.5O4-δ (n = 1), La0.3Sr2.7CoFeO7-δ (n = 2), and LaSr3Co1.5Fe1.5O10-δ (n = 3) were synthesized and studied via in situ neutron powder diffraction between 765 K and 1070 K at a pO2 of 10-1 atm. Then, the structures were fit to a tetragonal I4/mmm space group, and were found to have increased total oxygen vacancy concentration in the order La0.3Sr2.7CoFeO7-δ > LaSr3Co1.5Fe1.5O10-δmore » > LaSrCo0.5Fe0.5O4-δ, following the trend predicted for charge compensation upon increasing Sr2+/La3+ ratio. The oxygen vacancies within the material were almost exclusively located within the perovskite layers for all of the crystal structures with only minimal vacancy formation in the rock-salt layer. Finally, analysis of the concentration of these vacancies at each distinct crystallographic site and the anisotropic atomic displacement parameters for the oxygen sites reveals potential preferred oxygen transport pathways through the perovskite layers.« less

  9. A method for the monitoring of metal recrystallization based on the in-situ measurement of the elastic energy release using neutron diffraction

    SciTech Connect (OSTI)

    Christien, F. Le Gall, R.; Telling, M. T. F.; Knight, K. S.

    2015-05-15

    A method is proposed for the monitoring of metal recrystallization using neutron diffraction that is based on the measurement of stored energy. Experiments were performed using deformed metal specimens heated in-situ while mounted at the sample position of the High Resolution Powder Diffractometer, HRPD (ISIS Facility), UK. Monitoring the breadth of the resulting Bragg lines during heating not only allows the time-dependence (or temperature-dependence) of the stored energy to be determined but also the recrystallized fraction. The analysis method presented here was developed using pure nickel (Ni270) specimens with different deformation levels from 0.29 to 0.94. In situ temperature ramping as well as isothermal annealing was undertaken. The method developed in this work allows accurate and quantitative monitoring of the recrystallization process. The results from neutron diffraction are satisfactorily compared to data obtained from calorimetry and hardness measurements.

  10. Neutron diffraction measurements of intergranular strains in MONEL-400

    SciTech Connect (OSTI)

    Holden, T.M.; Holt, R.A.; Clarke, A.P.

    1997-12-01

    Measurements have been made of the strain response parallel and perpendicular to an applied stress in uniaxial tensile specimens of MONEL-400. The diffraction elastic constants are in close agreement with the Kroener model. Beyond the yield point, different crystallographic orientations respond quite differently to the applied stress and, upon unloading, residual intergranular strains are generated which are tensile for some orientations and compressive for others. A simple theory based on the Taylor-Bishop-Hill (TBH) model gives a good qualitative description of the effects.

  11. Neutron diffraction measurements of dislocation density in copper crystals deformed at high strain rate

    SciTech Connect (OSTI)

    Rao, Mala N.; Chaplot, S. L.; Rawat, S.

    2013-02-05

    Neutron diffraction measurements of the rocking curves were carried out for single crystals of copper subjected to dynamic compression at 10{sup 3}/s strain rate. The line broadening is expected to be produced by dislocations, and an analysis of this broadening gives the dislocation density. Dislocation density is found to increase with increase of pressure.

  12. Processing of Neutron Diffraction Data for Strain Measurement in Geological Materials

    SciTech Connect (OSTI)

    Polsky, Yarom; An, Ke; Anovitz, Lawrence {Larry} M; Bingham, Philip R; Carmichael, Justin R; Dessieux Jr, Luc Lucius

    2014-01-01

    : Conventional rock mechanics testing techniques typically involve the loading of samples and measurement of displacements or strains on the outer boundary of the specimen surface. Neutron diffraction based strain measurement techniques represent a unique and powerful tool for measuring the strain within geological materials under load. The structural variability and non-uniform crystallinity of geological materials, however, create many complexities in the intensity patterns that must be analyzed to quantify strains within the material. The attenuating and scattering properties of the pressure cell housing the sample further add difficulties to the data analysis. This paper describes the methods and processes used to process neutron scattering data for strain measurement in geological materials. It is intended to provide a primer for those in the rock mechanics community that are interested in utilizing this technique along with additional discussion of neutron diffraction experimental factors that may affect data quality.

  13. Irradiation creep of nano-powder sintered silicon carbide at low neutron fluences

    SciTech Connect (OSTI)

    Koyanagi, Takaaki; Shimoda, Kazuya; Kondo, Sosuke; Hinoki, Tatsuya; Ozawa, Kazumi; Katoh, Yutai

    2014-12-01

    The irradiation creep behavior of nano-powder sintered silicon carbide was investigated using the bend stress relaxation method under neutron irradiation up to 1.9 dpa. The creep deformation was observed at all temperatures ranging from 380 to 1180 C mainly from the irradiation creep but with the increasing contributions from the thermal creep at higher temperatures. Microstructural observation and data analysis were performed.

  14. Electrostatic levitation facility optimized for neutron diffraction studies of high temperature liquids at a spallation neutron source

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Mauro, N. A.; Vogt, A. J.; Derendorf, K. S.; Johnson, M. L.; Rustan, G. E.; Quirinale, D. G.; Kreyssig, A.; Lokshin, K. A.; Neuefeind, J. C.; An, Ke; et al

    2016-01-01

    Neutron diffraction studies of metallic liquids provide valuable information about inherent topological and chemical ordering on multiple length scales as well as insight into dynamical processes at the level of a few atoms. But, there exist very few facilities in the world that allow such studies to be made of reactive metallic liquids in a containerless environment, and these are designed for use at reactor-based neutron sources. We present an electrostatic levitation facility, NESL (for Neutron ElectroStatic Levitator), which takes advantage of the enhanced capabilities and increased neutron flux available at spallation neutron sources (SNSs). NESL enables high quality elasticmore » and inelastic neutron scattering experiments to be made of reactive metallic and other liquids in the equilibrium and supercooled temperature regime. The apparatus is comprised of a high vacuum chamber, external and internal neutron collimation optics, and a sample exchange mechanism that allows up to 30 samples to be processed between chamber openings. Two heating lasers allow excellent sample temperature homogeneity, even for samples approaching 500 mg, and an automated temperature control system allows isothermal measurements to be conducted for times approaching 2 h in the liquid state, with variations in the average sample temperature of less than 0.5%. Furthermore, to demonstrate the capabilities of the facility for elastic scattering studies of liquids, a high quality total structure factor for Zr64Ni36 measured slightly above the liquidus temperature is presented from experiments conducted on the nanoscale-ordered materials diffractometer (NOMAD) beam line at the SNS after only 30 min of acquisition time for a small sample ( 100 mg).« less

  15. X-ray and neutron diffraction of Er-hydride films.

    SciTech Connect (OSTI)

    Rodriguez, Mark Andrew

    2004-10-01

    The outline of this report is: (1) structures of hexagonal Er meal, ErH{sub 2} fluorite, and molybdenum; (2) texture issues and processing effects; (3) idea of pole figure integration; and (4) promising neutron diffraction work. Summary of this report are: (1) ErD{sub 2} and ErT{sub 2} film microstructures are strongly effected by processing conditions; (2) both x-ray and neutron diffraction are being pursued to help diagnose structure/property issues regarding ErT{sub 2} films and these correlations to He retention/release; (3) texture issues are great challenges for determination of site occupancy; and (4) work on pole-figure-integration looks to have promise addressing texture issues in ErD{sub 2} and ErT{sub 2} films.

  16. Sample cell for powder x-ray diffraction at up to 500 bars and 200 deg. C

    SciTech Connect (OSTI)

    Jupe, Andrew C.; Wilkinson, Angus P.

    2006-11-15

    A low cost sample cell for powder diffraction at high pressure and temperature that employs either sapphire or steel pressure tubes is described. The cell can be assembled rapidly, facilitating the study of chemically reacting systems, and it provides good control of both pressure and temperature in a regimen where diamond anvil cells and multianvil apparatus cannot be used. The design provides a relatively large sample volume making it suitable for the study of quite large grain size materials, such as hydrating cement slurries. However, relatively high energy x rays are needed to penetrate the pressure tube.

  17. Sample cell for powder x-ray diffraction at up to 500 bars and 200 °C

    SciTech Connect (OSTI)

    Jupe, Andrew C.; Wilkinson, Angus P.

    2008-10-03

    A low cost sample cell for powder diffraction at high pressure and temperature that employs either sapphire or steel pressure tubes is described. The cell can be assembled rapidly, facilitating the study of chemically reacting systems, and it provides good control of both pressure and temperature in a regimen where diamond anvil cells and multianvil apparatus cannot be used. The design provides a relatively large sample volume making it suitable for the study of quite large grain size materials, such as hydrating cement slurries. However, relatively high energy x rays are needed to penetrate the pressure tube.

  18. Synchrotron X-ray powder diffraction and convergent beam electron diffraction studies on the cubic phase of MgV{sub 2}O{sub 4} spinel

    SciTech Connect (OSTI)

    Niitaka, Seiji; Lee, Soyeon; Oshima, Yoshifumi; Kato, Kenichi; Hashizume, Daisuke; Takata, Masaki; Takagi, Hidenori

    2014-07-01

    The A V{sub 2}O{sub 4} (A=Mg{sup 2+}, Zn{sup 2+}, Cd{sup 2+}) spinels are three-dimensional spin-1 frustrated systems with orbital degree of freedom, which have been known to possess intriguing orbital states causing releases of spin frustration at low temperatures. We have performed synchrotron X-ray and convergent beam electron diffraction measurements for one of these vanadates, MgV{sub 2}O{sub 4} in order to clarify its crystal structure in the high temperature cubic phase, which is regarded as an important starting point for understanding the details of the low temperature phase. We have successfully observed that the [001] zone axis convergent beam electron diffraction pattern exhibits 4mm symmetry, suggesting the space group of Fd3{sup ¯}m in the cubic MgV{sub 2}O{sub 4}. It has also been demonstrated that the crystal structure of the cubic MgV{sub 2}O{sub 4} contains VO{sub 6} octahedra elongated along the threefold rotation axis. Based on our results, we discuss the orbital states of MgV{sub 2}O{sub 4} as well as the other spinel vanadates. - Graphical abstract: Precise geometry of the VO{sub 6} octahedra in the cubic phase of MgV{sub 2}O{sub 4} spinel determined with the synchrotron powder XRD data. - Highlights: • We examined the crystal structure of the cubic phase of MgV{sub 2}O{sub 4} spinel. • We prepared the single crystal and powdered sample of MgV{sub 2}O{sub 4} with high quality. • The result of the CBED measurement agrees with the space group of Fd3{sup ¯}m in the phase. • The cubic phase has VO{sub 6} octahedra elongated along the threefold rotation axis.

  19. Azine bridged silver coordination polymers: Powder X-ray diffraction route to crystal structure determination of silver benzotriazole

    SciTech Connect (OSTI)

    Rajeswaran, Manju . E-mail: manju.rajeswaran@kodak.com; Blanton, Thomas N.; Giesen, David J.; Whitcomb, David R.; Zumbulyadis, Nicholas; Antalek, Brian J.; Neumann, Marcus M.; Misture, Scott T.

    2006-04-15

    In continuation of our interest in solid-state structures of silver complexes of photographic importance, the structure for silver benzotriazole (AgBZT), has now been obtained. The preferred method for solving crystal structures is via single-crystal X-ray diffraction (XRD). However, for some materials, growing single crystals of appropriate size and quality is often difficult or even impossible. AgBZT is an example of such a silver complex with poor solubility. The usual routes to preparing single crystals using recrystallization from a cooperating solvent resulted in polycrystalline powder samples. We propose a crystal structure for AgBZT, solved from synchrotron X-ray powder diffraction data, using a direct-space Monte Carlo simulated annealing approach. AgBZT crystals are monoclinic (P2{sub 1} /c), with unit cell dimensions, a=14.8052(3) A, b=3.7498(4) A, c=12.3495(12) A, and {beta}=114.200(6){sup o}. The AgBZT complex is constructed from all three of the Benzotriazole (BZT) nitrogens bonding to a separate silver atom. As a consequence of this bonding mode, the structure is a highly cross-linked, coordination polymer.

  20. The Crystal Structure of Thorium and Zirconium Dihydrides by X-ray and Neutron Diffraction

    DOE R&D Accomplishments [OSTI]

    Rundle, R.E.; Shull, C.G.; Wollan, E.O.

    1951-04-20

    Thorium forms a tetragonal lower hydride of composition ThH{sub 2}. The hydrides ThH{sub 2}, ThD{sub 2}, and ZrD{sub 2} have been studied by neutron diffraction in order that hydrogen positions could be determined. The hydrides are isomorphous, and have a deformed fluorite structure. Metal-hydrogen distances in thorium hydride are unusually large, as in UH{sub 3}. Thorium and zirconium scattering amplitudes and a revised scattering amplitude for deuterium are reported.

  1. Quantitative determination of mineral composition by powder X-ray diffraction

    DOE Patents [OSTI]

    Pawloski, Gayle A.

    1986-01-01

    An external standard intensity ratio method is used for quantitatively determining mineralogic compositions of samples by x-ray diffraction. The method uses ratios of x-ray intensity peaks from a single run. Constants are previously determined for each mineral which is to be quantitatively measured. Ratios of the highest intensity peak of each mineral to be quantified in the sample and the highest intensity peak of a reference mineral contained in the sample are used to calculate sample composition.

  2. Quantitative determination of mineral composition by powder x-ray diffraction

    DOE Patents [OSTI]

    Pawloski, G.A.

    1984-08-10

    An external standard intensity ratio method is used for quantitatively determining mineralogic compositions of samples by x-ray diffraction. The method uses ratios of x-ray intensity peaks from a single run. Constants are previously determined for each mineral which is to be quantitatively measured. Ratios of the highest intensity peak of each mineral to be quantified in the sample and the highest intensity peak of a reference mineral contained in the sample are used to calculate sample composition.

  3. Pressure dependence of the magnetic order in CrAs: a neutron diffraction investigation

    SciTech Connect (OSTI)

    Keller, L.; White, J. S.; Babkevich, P.; Susner, Michael A.; Sims, Zachary C; Safa-Sefat, Athena; Ronnow, H. M.; Ruegg, Ch.

    2015-01-29

    The suppression of magnetic order with pressure concomitant with the appearance of pressure-induced superconductivity was recently discovered in CrAs. Here we present a neutron diffraction study of the pressure evolution of the helimagnetic ground-state towards and in the vicinity of the superconducting phase. Neutron diffraction on polycrystalline CrAs was employed from zero pressure to 0.65 GPa and at various temperatures. The helimagnetic long-range order is sustained under pressure and the magnetic propagation vector does not show any considerable change. The average ordered magnetic moment is reduced from 1.73(2) μB at ambient pressure to 0.4(1) μB close to the critical pressure Pc ≈ 0.7 GPa, at which magnetic order is completely suppressed. The width of the magnetic Bragg peaks strongly depends on temperature and pressure, showing a maximum in the region of the onset of superconductivity. In conclusion, we interpret this as associated with competing ground-states in the vicinity of the superconducting phase.

  4. Neutron diffraction studies of a four-coordinated hydride in near square-planar geometry

    SciTech Connect (OSTI)

    Liao, Jian -Hong; Dhayal, Rajendra Singh; Wang, Xiaoping; Kahlal, Samia; Saillard, Jean -Yves; Liu, C. W.

    2014-10-07

    The structure of a nanospheric polyhydrido copper cluster, [Cu20(H)11{S2P(OiPr)2}9], was determined by single-crystal neutron diffraction. Cu20 cluster consists of an elongated triangular orthobicupola constructed from 18 Cu atoms that encapsulate a [Cu2H5}3- ion in the center with an exceptionally short Cu-Cu distance. The eleven hydrides in the cluster display three different coordination modes to the Cu atoms: Six μ3-hydrides in pyramidal geometry, two μ4-hydrides in tetrahedral cavity, and three μ4-hydrides in an unprecedented near square-planar geometry. The neutron data set was collected on a small crystal of the size 0.20 mm x 0.50 mm x 0.65 mm for seven days using the Spallation Neutron Source TOPAZ single-crystal time-of-flight Laue diffractometer at the Oak Ridge National Laboratory. Furthermore, the final R-factor is 8.64% for 16014 reflections.

  5. Neutron diffraction studies of a four-coordinated hydride in near square-planar geometry

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Liao, Jian -Hong; Dhayal, Rajendra Singh; Wang, Xiaoping; Kahlal, Samia; Saillard, Jean -Yves; Liu, C. W.

    2014-10-07

    The structure of a nanospheric polyhydrido copper cluster, [Cu20(H)11{S2P(OiPr)2}9], was determined by single-crystal neutron diffraction. Cu20 cluster consists of an elongated triangular orthobicupola constructed from 18 Cu atoms that encapsulate a [Cu2H5}3- ion in the center with an exceptionally short Cu-Cu distance. The eleven hydrides in the cluster display three different coordination modes to the Cu atoms: Six μ3-hydrides in pyramidal geometry, two μ4-hydrides in tetrahedral cavity, and three μ4-hydrides in an unprecedented near square-planar geometry. The neutron data set was collected on a small crystal of the size 0.20 mm x 0.50 mm x 0.65 mm for seven daysmore » using the Spallation Neutron Source TOPAZ single-crystal time-of-flight Laue diffractometer at the Oak Ridge National Laboratory. Furthermore, the final R-factor is 8.64% for 16014 reflections.« less

  6. Pressure/temperature fluid cell apparatus for the neutron powder diffractometer instrument: Probing atomic structure in situ

    SciTech Connect (OSTI)

    Wang, Hsiu -Wen; Fanelli, Victor R.; Reiche, Helmut M.; Larson, Eric; Taylor, Mark A.; Xu, Hongwu; Zhu, Jinlong; Siewenie, Joan; Page, Katharine

    2014-12-24

    This contribution describes a new local structure compatible gas/liquid cell apparatus for probing disordered materials at high pressures and variable temperatures in the Neutron Powder Diffraction instrument at the Lujan Neutron Scattering Center, Los Alamos National Laboratory. The new sample environment offers choices for sample canister thickness and canister material type. Finite element modeling is utilized to establish maximum allowable working pressures of 414 MPa at 15 K and 121 MPa at 600 K. High quality atomic pair distribution function data extraction and modeling have been demonstrated for a calibration standard (Si powder) and for supercritical and subcritical CO2measurements. As a result, the new sample environment was designed to specifically target experimental studies of the local atomic structures involved in geologic CO2 sequestration, but will be equally applicable to a wide variety of energy applications, including sorption of fluids on nano/meso-porous solids, clathrate hydrate formation, catalysis, carbon capture, and H2 and natural gas uptake/storage.

  7. In-situ time-of-flight neutron diffraction of ErD2 (beta phase) formation during D2 loading.

    SciTech Connect (OSTI)

    Browning, James Frederick; Llobet, Anna; Snow, Clark Sheldon; Rodriguez, Mark Andrew; Wixom, Ryan R.

    2008-06-01

    In an effort to better understand the structural changes occurring during hydrogen loading of erbium target materials, we have performed D{sub 2} loading of erbium metal (powder) with simultaneous neutron diffraction analysis. This experiment tracked the conversion of Er metal to the {alpha} erbium deuteride (solid-solution) phase and then on to the {beta} (fluorite) phase. Complete conversion to ErD{sub 2.0} was accomplished at 10 Torr D{sub 2} pressure with deuterium fully occupying the tetrahedral sites in the fluorite lattice. Increased D{sub 2} pressure (up to 500 Torr at 450 C) revealed {approx}10 % deuterium occupation of the octahedral sites. Subsequent vacuum pumping of the sample at 450 C removed octahedral site occupancy while maintaining tetrahedral deuterium occupancy, thereby yielding stoichiometric ErD{sub 2.0} {beta} phase.

  8. Study of tempering behavior of lath martensite using in situ neutron diffraction

    SciTech Connect (OSTI)

    Shi, Z.M.; Gong, W.; Tomota, Y.; Harjo, S.; Li, J.; Chi, B.; Pu, J.

    2015-09-15

    To elucidate changes in the density and substructure of dislocations during tempering of lath martensite steel, a convolutional multiple whole-profile fitting method was applied to in situ neutron diffraction profiles. With increasing tempering temperature, the dislocation density scarcely changed in the beginning and then decreased at temperatures above 473 K, whereas the dislocation arrangement drastically changed at temperatures above 673 K. The strength of the steel is speculated to depend on the density and arrangement of dislocations. - Highlights: • A convolutional multiple whole-profile fitting method was applied. • Dislocation density and dislocation arrangement changing with tempering were discussed. • Dislocation density scarcely changed in the beginning. • And then dislocation density decreased at temperatures above 473 K. • The dislocation arrangement drastically changed at temperatures above 673 K.

  9. A comparison of dilatometry and in-situ neutron diffraction in tracking bulk phase transformations in a martensitic stainless steel

    SciTech Connect (OSTI)

    Christien, F.; Telling, M.T.F.; Knight, K.S.

    2013-08-15

    Phase transformations in the 17-4PH martensitic stainless steel have been studied using different in-situ techniques, including dilatometry and high resolution neutron diffraction. Neutron diffraction patterns were quantitatively processed using the Rietveld refinement method, allowing the determination of the temperature-dependence of martensite (α′, bcc) and austenite (γ, fcc) phase fractions and lattice parameters on heating to 1000 °C and then cooling to room temperature. It is demonstrated in this work that dilatometry doesn't permit an accurate determination of the end temperature (Ac3) of the α′ → γ transformation which occurs upon heating to high temperature. The analysis of neutron diffraction data has shown that the respective volumes of the two phases become very close to each other at high temperature, thus making the dilatometric technique almost insensitive in that temperature range. However, there is a very good agreement between neutron diffraction and dilatometry at lower temperature. The martensitic transformation occurring upon cooling has been analysed using the Koistinen–Marburger equation. The thermal expansion coefficients of the two phases have been determined in addition. A comparison of the results obtained in this work with data from literature is presented. - Highlights: • Martensite is still present at very high temperature (> 930 °C) upon heating. • The end of austenitisation cannot be accurately monitored by dilatometry. • The martensite and austenite volumes become similar at high temperature (> ∼ 850 °C)

  10. SSRL Powder Diffraction Workshop

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    Date: Wed., 21st Oct. 1998 Speakers: Apurva Mehta (SSRl) Dave Cox (NSLSBNL) Richard Harlow (E. I. DuPont de Nemours & Co.) Poul Norby (University of Aarhus) Larry Finger ...

  11. Structural phase transition and magnetism in hexagonal SrMnO{sub 3} by magnetization measurements and by electron, x-ray, and neutron diffraction studies

    SciTech Connect (OSTI)

    Daoud-Aladine, A.; Chapon, L. C.; Knight, K. S.; Martin, C.; Hervieu, M.; Brunelli, M.; Radaelli, P. G.

    2007-03-01

    The structural and magnetic properties of the hexagonal four-layer form of SrMnO{sub 3} have been investigated by combining magnetization measurements, electron diffraction, and high-resolution synchrotron x-ray and neutron powder diffraction. Below 350 K, there is subtle structural phase transition from hexagonal symmetry (space group P6{sub 3}/mmc) to orthorhombic symmetry (space group C222{sub 1}) where the hexagonal metric is preserved. The second-order phase transition involves a slight tilting of the corner-sharing Mn{sub 2}O{sub 9} units composed of two face-sharing MnO{sub 6} octahedra and the associated displacement of Sr{sup 2+} cations. The phase transition is described in terms of symmetry-adapted displacement modes of the high symmetry phase. Upon further cooling, long range magnetic order with propagation vector k=(0,0,0) sets in below 300 K. The antiferromagnetic structure, analyzed using representation theory, shows a considerably reduced magnetic moment indicating the crucial role played by direct exchange between Mn centers of the Mn{sub 2}O{sub 9} units.

  12. Operando Lithium Dynamics in the Li-Rich Layered Oxide Cathode Material via Neutron Diffraction

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Liu, Haodong; An, Ke; Venkatachalam, Subramanian; Qian, Danna; Zhang, Minghao; Meng, Ying Shirley

    2016-04-06

    Neutron diffraction under operando battery cycling is used to study the lithium and oxygen dynamics of high Li-rich Li(Lix/3Ni(3/8-3x/8)Co(1/4-x/4)Mn(3/8+7x/24)O2 (x = 0.6, HLR) and low Li-rich Li(Lix/3Ni(1/3-x/3)Co(1/3-x/3)Mn(1/3+x/3)O2 (x = 0.24, LLR) compounds that exhibit different degrees of oxygen activation at high voltage. The measured lattice parameter changes and oxygen position show largely contrasting changes for the two cathodes where the LLR exhibits larger movement of oxygen and lattice contractions in comparison to the HLR that maintains relatively constant lattice parameters and oxygen position during the high voltage plateau until the end of charge. Density functional theory calculations show the presencemore » of oxygen vacancy during the high voltage plateau; changes in the lattice parameters and oxygen position are consistent with experimental observations. Lithium migration kinetics for the Li-rich material is observed under operando conditions for the first time to reveal the rate of lithium extraction from the lithium layer, and transition metal layer is related to the different charge and discharge characteristics. At the beginning of charging, the lithium extraction predominately occurs within the lithium layer. The lithium extraction from the lithium layer slows down and extraction from the transition metal layer evolves at a faster rate once the high voltage plateau is reached.« less

  13. Partial Spin Ordering and Complex Magnetic Structure in BaYFeO4: A Neutron Diffraction and High Temperature Susceptibility Study

    SciTech Connect (OSTI)

    Thompson, Corey; Greedan, John; Garlea, Vasile O; Flacau, Roxana; Tan, Malinda; Derakhshan, Shahab

    2014-01-01

    The novel iron-based compound, BaYFeO4, crystallizes in the Pnma space group with two distinct Fe3+ sites, that are alternately corner-shared [FeO5]7 square pyramids and [FeO6]9 octahedra, forming into [Fe4O18]24 rings, which propagate as columns along the b-axis. A recent report shows two discernible antiferromagnetic (AFM) transitions at 36 and 48 K in the susceptibility, yet heat capacity measurements reveal no magnetic phase transitions at these temperatures. An upturn in the magnetic susceptibility measurements up to 400 K suggests the presence of shortrange magnetic behavior at higher temperatures. In this Article, variable-temperature neutron powder diffraction and hightemperature magnetic susceptibility measurements were performed to clarify the magnetic behavior. Neutron powder diffraction confirmed that the two magnetic transitions observed at 36 and 48 K are due to long-range magnetic order. Below 48 K, the magnetic structure was determined as a spin-density wave (SDW) with a propagation vector, k = (0, 0, 1/3), and the moments along the b-axis, whereas the structure becomes an incommensurate cycloid [k = (0, 0, 0.35)] below 36 K with the moments within the bc-plane. However, for both cases the ordered moments on Fe3+ are only of the order 3.0 B, smaller than the expected values near 4.5 B, indicating that significant components of the Fe moments remain paramagnetic to the lowest temperature studied, 6 K. Moreover, new high-temperature magnetic susceptibility measurements revealed a peak maximum at 550 K indicative of short-range spin correlations. It is postulated that most of the magnetic entropy is thus removed at high temperatures which could explain the absence of heat capacity anomalies at the long-range ordering temperatures. Published spin dimer calculations, which appear to suggest a k = (0, 0, 0) magnetic structure, and allow for neither low dimensionality nor geometric frustration, are inadequate to explain the observed complex magnetic

  14. The Manuel Lujan, Jr. Neutron Scattering Center LANSCE experiment reports 1989 run cycle

    SciTech Connect (OSTI)

    Hyer, D.K.; DiStravolo, M.A.

    1990-10-01

    This report contains a listing and description of experiments carried on at the LANSCE neutron scattering facility in the following areas: High Density Powder Diffraction; Neutron Powder Diffractometer, (NPD); Single Crystal Diffractometer, (SCD); Low-Q Diffractometer, (LQD); Surface Profile Analysis Reflectometer, (SPEAR); Filter Difference Spectrometer, (FDS); and Constant-Q Spectrometer.

  15. Investigation of phase evolution of CaCu{sub 3}Ti{sub 4}O{sub 12} (CCTO) by in situ synchrotron high-temperature powder diffraction

    SciTech Connect (OSTI)

    Ouyang, Xin; Huang, Saifang; Zhang, Weijun; Cao, Peng; Huang, Zhaohui; Gao, Wei

    2014-03-15

    In situ synchrotron X-ray powder diffraction was used to study the high-temperature phase evolution of CaCu{sub 3}Ti{sub 4}O{sub 12} (CCTO) precursors prepared via solid-state and sol–gel methods. After the precursors are heated to 1225 °C, the CCTO phase is the main phase observed in the calcined powder, with the presence of some minor impurities. Comparing the two precursors, we found that the onset temperature for the CCTO phase formation is 800 °C in the sol–gel precursor, lower than that in the solid-state precursor (875 °C). Intermediate phases were only observed in the sol–gel precursor. Both precursors are able to be calcined to sub-micrometric sized powders. Based on the synchrotron data along with differential scanning calorimetry (DSC) and thermal gravimetric analysis (TGA), the phase formation sequence and mechanism during calcination are proposed in this study. -- Graphical abstract: The in situ synchrotron HT-XRD patterns of CCTO sol–gel and solid-state precursor. Highlights: • Phase formation sequence/mechanism in two CCTO precursors has been established. • Formation temperature of CCTO via sol–gel method is lower than solid-state method. • Intermediate phases are only observed in the sol–gel precursor. • Both precursors are able to be calcined into sub-micrometric sized powders.

  16. Neutron diffraction studies on chemical and magnetic structure of multiferroic PbFe{sub 0.67}W{sub 0.33}O{sub 3}

    SciTech Connect (OSTI)

    Matteppanavar, Shidaling Angadi, Basavaraj; Rayaprol, Sudhindra

    2014-04-24

    We report on the single phase synthesis and room temperature structural characterization of PbFe{sub 0.67}W{sub 0.33}O{sub 3} (PFW) multiferroic. The PFW was synthesized by low temperature sintering, Columbite method. Analysis of powder XRD pattern exhibits single phase formation of PFW with no traces of pyrochlore phase. Detailed analysis of room temperature neutron diffraction (ND) reveals cubic phase at room temperature, space group Pm-3m. The ND pattern clearly reveals magnetic Bragg peak at 2? = 18.51 (Q = 1.36{sup ?1}). The refinement of magnetic structure reveals G-type antiferromagnetic structure in PFW at room temperature. The dielectric constant and loss tangent decreases with increasing frequency. The room temperature P-E measurements shows a non-linear slim hysteresis, typical nature of relaxor multiferroics, with saturation and remnant polarizations of P{sub s} = 1.50 ?C/cm{sup 2} and P{sub r} = 0.40 ?C/cm{sup 2}, respectively.

  17. Anisotropic lattice thermal expansion of PbFeBO4: A study by X-ray and neutron diffraction, Raman spectroscopy and DFT calculations

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Murshed, M. Mangir; Mendive, Cecilia B.; Curti, Mariano; Nénert, Gwilherm; Kalita, Patricia E.; Lipinska, Kris; Cornelius, Andrew L.; Huq, Ashfia; Gesing, Thorsten M.

    2014-11-01

    We present the lattice thermal expansion of mullite-type PbFeBO4 in this study. The thermal expansion coefficients of the metric parameters were obtained from composite data collected from temperature-dependent neutron and X-ray powder diffraction between 10 K and 700 K. The volume thermal expansion was modeled using extended Grüneisen first-order approximation to the zero-pressure equation of state. The additive frame of the model includes harmonic, quasi-harmonic and intrinsic anharmonic potentials to describe the change of the internal energy as a function of temperature. Moreover, the unit-cell volume at zero-pressure and 0 K was optimized during the DFT simulations. Harmonic frequencies ofmore » the optical Raman modes at the Γ-point of the Brillouin zone at 0 K were also calculated by DFT, which help to assign and crosscheck the experimental frequencies. The low-temperature Raman spectra showed significant anomaly in the antiferromagnetic regions, leading to softening or hardening of some phonons. Selected modes were analyzed using a modified Klemens model. The shift of the frequencies and the broadening of the line-widths helped to understand the anharmonic vibrational behaviors of the PbO4, FeO6 and BO3 polyhedra as a function of temperature.« less

  18. Anisotropic lattice thermal expansion of PbFeBO4: A study by X-ray and neutron diffraction, Raman spectroscopy and DFT calculations

    SciTech Connect (OSTI)

    Murshed, M. Mangir; Mendive, Cecilia B.; Curti, Mariano; Nénert, Gwilherm; Kalita, Patricia E.; Lipinska, Kris; Cornelius, Andrew L.; Huq, Ashfia; Gesing, Thorsten M.

    2014-11-01

    We present the lattice thermal expansion of mullite-type PbFeBO4 in this study. The thermal expansion coefficients of the metric parameters were obtained from composite data collected from temperature-dependent neutron and X-ray powder diffraction between 10 K and 700 K. The volume thermal expansion was modeled using extended Grüneisen first-order approximation to the zero-pressure equation of state. The additive frame of the model includes harmonic, quasi-harmonic and intrinsic anharmonic potentials to describe the change of the internal energy as a function of temperature. Moreover, the unit-cell volume at zero-pressure and 0 K was optimized during the DFT simulations. Harmonic frequencies of the optical Raman modes at the Γ-point of the Brillouin zone at 0 K were also calculated by DFT, which help to assign and crosscheck the experimental frequencies. The low-temperature Raman spectra showed significant anomaly in the antiferromagnetic regions, leading to softening or hardening of some phonons. Selected modes were analyzed using a modified Klemens model. The shift of the frequencies and the broadening of the line-widths helped to understand the anharmonic vibrational behaviors of the PbO4, FeO6 and BO3 polyhedra as a function of temperature.

  19. Extracting grain-orientation-dependent data from in situ time-of-flight neutron diffraction. I. Inverse pole figures

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Stoica, Grigoreta M.; Stoica, Alexandru Dan; An, Ke; Ma, Dong; Vogel, S. C.; Carpenter, J. S.; Wang, Xun-Li

    2014-11-28

    The problem of calculating the inverse pole figure (IPF) is analyzed from the perspective of the application of time-of flight neutron diffraction toin situmonitoring of the thermomechanical behavior of engineering materials. On the basis of a quasi-Monte Carlo (QMC) method, a consistent set of grain orientations is generated and used to compute the weighting factors for IPF normalization. The weighting factors are instrument dependent and were calculated for the engineering materials diffractometer VULCAN (Spallation Neutron Source, Oak Ridge National Laboratory). The QMC method is applied to face-centered cubic structures and can be easily extended to other crystallographic symmetries. Examples includemore » 316LN stainless steelin situloaded in tension at room temperature and an Al–2%Mg alloy, substantially deformed by cold rolling and in situannealed up to 653 K.« less

  20. Neutron diffraction and scattering study on M/sub x/WO/sub 3/ (M=Rb and K)

    SciTech Connect (OSTI)

    Sato, M.; Fujishita, H.; Moodenbaugh, A.R.; Hoshino, S.; Grier, B.H.

    1982-01-01

    To study the relationship between the lattice instability and the superconductivity of nonstoichiometric hexagonal tungsten bronze, M/sub x/WO/sub 3/, neutron diffraction and scattering studies were made. Two types of the structural phase transitions were observed. One is associated with the distortion of the corner linked WO/sub 6/ octahedra. The other is associated with the ordering of the M atoms which partially fill the sites in the WO/sub 3/ cage. A long period modulation of the structure appears for some values of x at low temperature. The discussion on the x dependence of the superconducting transition temperature is presented.

  1. Expanding Lorentz and spectrum corrections to large volumes of reciprocal space, for single crystal TOF neutron diffraction

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Michels-Clark, Tara M; Savici, Andrei T; Lynch, Vickie E; Hoffmann, Christina; Wang, Xiaoping

    2016-01-01

    Evidence is mounting that potentially exploitable properties of technologically and chemically interesting crystalline materials are often attributed to local structure effects, which can be observed as modulated diffuse scattering (mDS) next to Bragg diffraction (BD). BD forms a regular, sparse grid of discrete points in diffraction space; traditionally, the information in each Bragg peak is extracted first by integration, followed by the application of the required corrections. In contrast, mDS covers expansive volumes of reciprocal space close to, or between, Bragg reflections. For a full measurement of the diffuse scattering, multiple instrument configurations might be required, and the same pointmore » might be measured multiple times. The common integration method is not sufficient and a new, inclusive correction-plus-intensity-extraction method is in demand. In this contribution we introduce a comprehensive data analysis approach to correct and scale the full volume of scattering data in one step. Hence, we explore data treatment and data correction that includes the complete, collected reciprocal space simultaneously, using neutron time of flight (TOF) or wavelength-resolved data, collected at the Spallation Neutron Source (SNS) at Oak Ridge National Laboratory.« less

  2. Visualizing the Structural Evolution of LSM/xYSZ Composite Cathodes for SOFC by in-situ Neutron Diffraction

    SciTech Connect (OSTI)

    Chen, Yan; Yang, Ling; Ren, Fei; An, Ke

    2014-01-01

    Composite cathodes for solid oxide fuel cells, the mixtures of (La0.8Sr0.2)0.95MnO3- (LSM) and (Y2O3)x(ZrO2)1-x (xYSZ, x = 3, 6, 8 and 10), have the thermal stability unraveled at elevated temperatures by using in-situ neutron diffraction. The Rietveld refinement analysis of neutron diffraction visualizes the phase evolutions and the ion activities in the material systems. The phase transition of tetragonal YSZ at T > 900 C leads to a heterogeneous redistribution of Mn ions. The reaction of LSM and YSZ occurring at T > 1100 C was revealed as a three-stage process, yielding La2Zr2O7, SrZrO3 and MnO. The activities of Y, Mn and La ions at elevated temperatures are derived by the structural analysis, and the three-stage reaction of YSZ and LSM was found strongly correlated to ions behaviors.

  3. Structure of 2 molar NaOH in aqueous solution from neutron diffraction and empirical potential structure refinement

    SciTech Connect (OSTI)

    McLain, Sylvia E.; Imberti, Silvia; Soper, Alan K.; Botti, Alberto; Bruni, Fabio; Ricci, Maria Antonietta

    2006-09-01

    Neutron diffraction with isotopic substitution has been used to investigate aqueous solutions of 2M NaOH in the liquid state. The data were modeled using empirical potential structure refinement which allows for the extraction of the ion-water and water-water correlations. The data show that the ion-water radial distribution functions are in accordance with those found by previous studies on NaOH solutions and follow a trend which is dependent on the concentration of the solute. In particular, the shape of the hydroxide hydration shell is found to be concentration independent, but the number of water molecules occupying this shell increases with dilution. Additionally, the water-water correlations show that there is still a measurable effect on water structure with the addition of ions at this concentration, as the second shell in the water oxygen radial distribution function is compressed relative to the first shell. The data are also used to discuss the recent claims that the published radial distribution functions of water are unreliable, showing that data taken at different neutron sources, with different diffraction geometry and systematic errors lead to the same structural information when analyzed via a realistic modeling regime.

  4. Neutron diffraction and electrical transport studies on magnetic ordering in terbium at high pressures and low temperatures

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Thomas, Sarah A.; Montgomery, Jeffrey M.; Tsoi, Georgiy M.; Vohra, Yogesh K.; Chesnut, Gary N.; Weir, Samuel T.; Tulk, Christopher A.; dos Santos, Antonio M.

    2013-06-11

    Neutron diffraction and electrical transport measurements have been carried out on the heavy rare earth metal terbium at high pressures and low temperatures in order to elucidate the onset of ferromagnetic order as a function of pressure. The electrical resistance measurements show a change in slope as the temperature is lowered through the ferromagnetic Curie temperature. The temperature of this ferromagnetic transition decreases from approximately 240 K at ambient pressure at a rate of –16.7 K/GPa up to a pressure of 3.6 GPa, at which point the onset of ferromagnetic order is suppressed. Neutron diffraction measurements as a function ofmore » pressure at temperatures ranging from 90 K to 290 K confirm that the change of slope in the resistance is associated with the ferromagnetic ordering, since this occurs at pressures similar to those determined from the resistance results at these temperatures. Furthermore, a change in ferromagnetic ordering as the pressure is increased above 3.6 GPa is correlated with the phase transition from the ambient hexagonal close packed (hcp) structure to an α-Sm type structure at high pressures.« less

  5. Neutron diffraction and electrical transport studies on magnetic ordering in terbium at high pressures and low temperatures

    SciTech Connect (OSTI)

    Thomas, Sarah A.; Montgomery, Jeffrey M.; Tsoi, Georgiy M.; Vohra, Yogesh K.; Chesnut, Gary N.; Weir, Samuel T.; Tulk, Christopher A.; dos Santos, Antonio M.

    2013-06-11

    Neutron diffraction and electrical transport measurements have been carried out on the heavy rare earth metal terbium at high pressures and low temperatures in order to elucidate the onset of ferromagnetic order as a function of pressure. The electrical resistance measurements show a change in slope as the temperature is lowered through the ferromagnetic Curie temperature. The temperature of this ferromagnetic transition decreases from approximately 240 K at ambient pressure at a rate of –16.7 K/GPa up to a pressure of 3.6 GPa, at which point the onset of ferromagnetic order is suppressed. Neutron diffraction measurements as a function of pressure at temperatures ranging from 90 K to 290 K confirm that the change of slope in the resistance is associated with the ferromagnetic ordering, since this occurs at pressures similar to those determined from the resistance results at these temperatures. Furthermore, a change in ferromagnetic ordering as the pressure is increased above 3.6 GPa is correlated with the phase transition from the ambient hexagonal close packed (hcp) structure to an α-Sm type structure at high pressures.

  6. α-Phase transformation kinetics of U – 8 wt% Mo established by in situ neutron diffraction

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Garlea, Elena; Steiner, M. A.; Calhoun, C. A.; Klein, R. W.; An, K.; Agnew, S. R.

    2016-05-08

    The α-phase transformation kinetics of as-cast U - 8 wt% Mo below the eutectoid temperature have been established by in situ neutron diffraction. α-phase weight fraction data acquired through Rietveld refinement at five different isothermal hold temperatures can be modeled accurately utilizing a simple Johnson-Mehl-Avrami-Kolmogorov impingement-based theory, and the results are validated by a corresponding evolution in the γ-phase lattice parameter during transformation that follows Vegard’s law. Neutron diffraction data is used to produce a detailed Time-Temperature-Transformation diagram that improves upon inconsistencies in the current literature, exhibiting a minimum transformation start time of 40 min at temperatures between 500 °Cmore » and 510 °C. Lastly, the transformation kinetics of U – 8 wt% Mo can vary significantly from as-cast conditions after extensive heat treatments, due to homogenization of the typical dendritic microstructure which possesses non-negligible solute segregation.« less

  7. Deuterium sites in the defect pyrochlore DTaWO/sub 6/: location from neutron power-diffraction data

    SciTech Connect (OSTI)

    Rotella, F.J.; Jorgensen, J.D.; Morosin, B.; Biefeld, R.M.

    1981-01-01

    Time-of-flight Rietveld refinement and Fourier synthesis of high-resolution powder diffraction data from DTaWO/sub 6/ led to the location of deuterium in partially occupied 48f sites of Fd3m (origin at 3m) as distances of 1.024(9) A at 300/sup 0/K and 1.021(10) A at 12/sup 0/K from each oxygen position. The deuterium sites form spirals in the interconnecting open channels parallel to (110) directions with distances between nearest neighbors of 2.653(2) A at 300/sup 0/K and 2.652(2) A at 12/sup 0/K. These results are consistent with both classical hopping and tunneling models of deuteron transport in this system.

  8. Vacancy-induced nanoscale phase separation in KxFe2–ySe₂ single crystals evidenced by Raman scattering and powder x-ray diffraction

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Lazarević, N.; Abeykoon, M.; Stephens, P. W.; Lei, Hechang; Bozin, E. S.; Petrovic, C.; Popović, Z. V.

    2012-08-06

    Polarized Raman scattering spectra of KxFe2–ySe₂ were analyzed in terms of peculiarities of both I4/m and I4/mmm space group symmetries. The presence of the Raman active modes from both space group symmetries (16 Raman-active modes of the I4/m phase and two Raman-active modes of the I4/mmm phase) confirmed the existence of two crystallographic domains with different space group symmetry in a KxFe2–ySe₂ sample. High-resolution synchrotron powder x-ray diffraction structural refinement of the same sample confirmed the two-phase description, and determined the atomic positions and occupancies for both domains.

  9. High-pressure cell for neutron diffraction with in situ pressure control at cryogenic temperatures

    SciTech Connect (OSTI)

    Jacobsen, Matthew K.; Ridley, Christopher J.; Bocian, Artur; Kamenev, Konstantin V.; Kirichek, Oleg; Manuel, Pascal; Khalyavin, Dmitry; Azuma, Masaki; Attfield, J. Paul

    2014-04-15

    Pressure generation at cryogenic temperatures presents a problem for a wide array of experimental techniques, particularly neutron studies due to the volume of sample required. We present a novel, compact pressure cell with a large sample volume in which load is generated by a bellow. Using a supply of helium gas up to a pressure of 350 bar, a load of up to 78 kN is generated with leak-free operation. In addition, special fiber ports added to the cryogenic center stick allow for in situ pressure determination using the ruby pressure standard. Mechanical stability was assessed using finite element analysis and the dimensions of the cell have been optimized for use with standard cryogenic equipment. Load testing and on-line experiments using NaCl and BiNiO{sub 3} have been done at the WISH instrument of the ISIS pulsed neutron source to verify performance.

  10. Neutron diffraction and thermoelectric properties of indium filled In x Co 4 Sb 12 ( x=0.05, 0.2) and indium cerium filled Ce 0.05 In 0.1 Co 4 Sb 12 skutterudites: Neutron diffraction and thermoelectric properties of In/Ce skutterudites

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Sesselmann, Andreas; Klobes, Benedikt; Dasgupta, Titas; Gourdon, Olivier; Hermann, Raphael; Mueller, Eckhard

    2015-09-25

    The thermoelectric properties on polycrystalline single (In) and double filled (Ce, In) skutterudites are characterized between 300 and 700 K. Powder neutron diffraction measurements of the skutterudite compositions InxCo4Sb12 (x= 0.05, 0.2) and Ce0.05In0.1Co4Sb12 as a function of temperature (12- 300 K) were carried out, which gives more insight into the structural data of single and double-filled skutterudites. Our results show that due to the annealing treatment, a Sb deficiency is detectable and thus verifies defects at the Sb lattice site of the skutterudite. Furthermore, we show by electron microprobe analysis that a considerable amount of indium is lost duringmore » synthesis and post-processing for the single indium filled samples, but not for the double cerium and indium skutterudite sample. The double-filled skutterudite is superior to the single-filled skutterudite composition due to a higher charge carrier density, a comparable lattice thermal resistivity, and a higher density of states effective mass in our experiment. Finally, we obtained a significantly higher Einstein temperature for the double-filled skutterudite composition in comparison to the single-filled species, which reflects the high sensitivity due to filling of the void lattice position within the skutterudite crystal.« less

  11. Solid solubilities of (La Nd,){sub 2}(Zr,Ti){sub 2}O{sub 7} phases deduced by neutron diffraction

    SciTech Connect (OSTI)

    Harvey, Elizabeth J.; Whittle, Karl R.; Lumpkin, Gregory R.; Smith, Ronald I.; Redfern, Simon A.T. . E-mail: satr@cam.ac.uk

    2005-03-15

    Time-of-flight powder neutron diffraction has been performed on oxides with composition (La{sub 1-x}Nd{sub x}){sub 2}Zr{sub 2}O{sub 7} and Nd{sub 2}(Zr{sub 1-x}Ti{sub x}){sub 2}O{sub 7}, where x=0, 0.2, 0.4,...1.0, in order to determine the solid solution behaviour across each series. Between La{sub 2}Zr{sub 2}O{sub 7} and Nd{sub 2}Zr{sub 2}O{sub 7}, a cubic pyrochlore phase is observed (Fd3-bar m, Z=8). A linear decrease in the lattice parameter from 10.8047 to 10.6758A indicates complete miscibility of the two end-members. For the same series, the 48f oxygen x-parameter increases from 0.3313 to 0.3348, suggesting increased distortion of the 6 coordinate B sites and reduced distortion of the 8 coordinate A sites. There is limited solubility of Nd{sub 2}Ti{sub 2}O{sub 7} in Nd{sub 2}Zr{sub 2}O{sub 7}. Exsolution of a monoclinic phase (P2{sub 1}, Z=8) rich in Nd{sub 2}Ti{sub 2}O{sub 7} is observed at approximately x=0.56. The compositional range over which a solid solution exists is more extensive than that which has been previously reported. The solubility of Nd{sub 2}Zr{sub 2}O{sub 7} in Nd{sub 2}Ti{sub 2}O{sub 7} is very low.

  12. Anisotropic lattice thermal expansion of PbFeBO{sub 4}: A study by X-ray and neutron diffraction, Raman spectroscopy and DFT calculations

    SciTech Connect (OSTI)

    Murshed, M. Mangir; Mendive, Cecilia B.; Curti, Mariano; Nénert, Gwilherm; Kalita, Patricia E.; Lipinska, Kris; Cornelius, Andrew L.; Huq, Ashfia; Gesing, Thorsten M.

    2014-11-15

    Highlights: • Mullite-type PbFeBO{sub 4} shows uni-axial negative coefficient of thermal expansion. • Anisotropic thermal expansion of the metric parameters was modeled using modified Grüneisen approximation. • The model includes harmonic, quasi-harmonic and intrinsic anharmonic contributions to the internal energy. • DFT calculation, temperature- and pressure-dependent Raman spectra help understand the phonon decay and associated anharmonicity. - Abstract: The lattice thermal expansion of mullite-type PbFeBO{sub 4} is presented in this study. The thermal expansion coefficients of the metric parameters were obtained from composite data collected from temperature-dependent neutron and X-ray powder diffraction between 10 K and 700 K. The volume thermal expansion was modeled using extended Grüneisen first-order approximation to the zero-pressure equation of state. The additive frame of the model includes harmonic, quasi-harmonic and intrinsic anharmonic potentials to describe the change of the internal energy as a function of temperature. The unit-cell volume at zero-pressure and 0 K was optimized during the DFT simulations. Harmonic frequencies of the optical Raman modes at the Γ-point of the Brillouin zone at 0 K were also calculated by DFT, which help to assign and crosscheck the experimental frequencies. The low-temperature Raman spectra showed significant anomaly in the antiferromagnetic regions, leading to softening or hardening of some phonons. Selected modes were analyzed using a modified Klemens model. The shift of the frequencies and the broadening of the line-widths helped to understand the anharmonic vibrational behaviors of the PbO{sub 4}, FeO{sub 6} and BO{sub 3} polyhedra as a function of temperature.

  13. Neutron diffraction study of the magnetic-field-induced transition in Mn{sub 3}GaC

    SciTech Connect (OSTI)

    akir, .; Acet, M.; Farle, M.; Senyshyn, A.

    2014-01-28

    The antiperovskite Mn{sub 3}GaC undergoes an isostructural cubiccubic first order transition from a low-temperature, large-cell-volume antiferromagnetic state to a high-temperature, small-cell-volume ferromagnetic state at around 160?K. The transition can also be induced by applying a magnetic field. We study here the isothermal magnetic-field-evolution of the transition as ferromagnetism is stabilized at the expense of antiferromagnetism. We make use of the presence of the two distinct cell volumes of the two magnetic states as a probe to observe by neutron diffraction the evolution of the transition, as the external magnetic field carries the system from the antiferromagnetic to the ferromagnetic state. We show that the large-volume antiferromagnetic and the small-volume ferromagnetic states coexist in the temperature range of the transition. The ferromagnetic state is progressively stabilized as the field increases.

  14. In-situ neutron diffraction of LaCoO{sub 3} perovskite under uniaxial compression. II. Elastic properties

    SciTech Connect (OSTI)

    Lugovy, Mykola; Aman, Amjad; Orlovskaya, Nina; Chen, Yan; Kuebler, Jakob; Graule, Thomas; Reece, Michael J.; Ma, Dong; Stoica, Alexandru D.; An, Ke

    2014-07-07

    Calculations of elastic constants and development of elastic anisotropy under uniaxial compression in originally isotropic polycrystalline LaCoO{sub 3} perovskite are reported. The lattice strains in individual (hkl) planes as well as average lattice strain were determined both for planes oriented perpendicular and parallel to the loading direction using in-situ neutron diffraction. Utilizing average lattice strains as well as lattice strains along the a and c crystallographic directions, an attempt was made to determine Poisson's ratio of LaCoO{sub 3}, which was then compared with that measured using an impulse excitation technique. The elastic constants were calculated and Young's moduli of LaCoO{sub 3} single crystal in different crystallographic directions were estimated.

  15. Neutron diffraction study on very high elastic strain of 6% in an Fe{sub 3}Pt under compressive stress

    SciTech Connect (OSTI)

    Yamaguchi, Takashi; Fukuda, Takashi Kakeshita, Tomoyuki; Harjo, Stefanus; Nakamoto, Tatsushi

    2014-06-09

    An Fe{sub 3}Pt alloy with degree of order 0.75 exhibits a second-order-like martensitic transformation from a cubic structure to a tetragonal one at about 90?K; its tetragonality c/a changes nearly continuously from 1 to 0.945 on cooling from 90?K to 14?K. We have investigated the change in lattice parameters in a single crystal of the Fe{sub 3}Pt alloy at 93?K under compressive stresses, ?, applied in the [001] direction by neutron diffraction. The tetragonality c/a has decreased continuously from 1 to 0.907 with an increase in |?| up to |?|?=?280?MPa; the corresponding lattice strain in the [001] direction, due to the continuous structure change, increases from 0% to 6.1%. When the stress of 300?MPa is reached, c/a has changed abruptly from 0.907 to 0.789 due to a first-order martensitic transformation.

  16. Investigation of the structure of C{sub 60} fullerene halides by the neutron and synchrotron diffraction methods

    SciTech Connect (OSTI)

    Troyanov, S. I.

    2006-10-15

    The crystal and molecular structures of bromofullerenes and chlorofullerenes, namely, C{sub 60}Br{sub 6} . 0.5PhCl . 0.5Br{sub 2}, C{sub 60}Br{sub 8} . TiBr{sub 4} . Br{sub 2}, C{sub 60}Br{sub 24} . Br{sub 2}, and C{sub 60}Cl{sub 24} . TiCl{sub 4}, are determined and refined using neutron and synchrotron diffraction. The interatomic distances are determined with an accuracy higher than the accuracy in the determination of the corresponding parameters for the same molecular structures with the use of X-ray laboratory equipment.

  17. Single crystal neutron diffraction study of the magnetic structure of TmNi{sub 2}B{sub 2}C

    SciTech Connect (OSTI)

    Sternlieb, B.; Shapiro, S.; Stassis, C.; Goldman, A.I.; Canfield, P.

    1997-02-01

    Neutron diffraction techniques have been used to study the magnetic structure of single crystals of the magnetic superconductor (T{sub c} {congruent} 11K) TmNi{sub 2}B{sub 2}C. We find that below approximately 1.5K the magnetic moments order in an incommensurate spin wave with propagation vector q{sub m} = q{sub m} (a* +b*) (or q{sub m} = q{sub m} (a* + b*)) with q{sub m} = 0.094 {+-} 0.001. The spin wave is transverse with the moments aligned along the c-axis, and the observation of relatively intense higher order harmonics shows that the modulation is not purely sinusoidal but considerably squared. This incommensurate magnetic structure, which coexists with superconductivity below T{sub N} {congruent} 1.5K, is quite different from those observed in the magnetic superconductors HoNi{sub 2}B{sub 2}C and ErNi{sub 2}B{sub 2}C. The origin of diffraction peaks observed in scans parallel to a* is briefly discussed.

  18. Obtaining aluminas from the thermal decomposition of their different precursors: An {sup 27}Al MAS NMR and X-ray powder diffraction studies

    SciTech Connect (OSTI)

    Chagas, L.H.; De Carvalho, G.S.G.; San Gil, R.A.S.; Chiaro, S.S.X.; Leito, A.A.; Diniz, R.

    2014-01-01

    Graphical abstract: - Highlights: We synthesized three precursors of alumina from different methods. The calcination of the precursors generated several alumina polymorphs. XRD and NMR were used for structural investigation of the polymorphs. The synthesis route determines the structural and textural properties of the solids. - Abstract: A commercial sample of Boehmite was used as precursor of alumina polymorphs. For comparison, three other precursors were synthesized from different methods. Particularly, the use of excess of urea promoted a very crystalline form of basic aluminum carbonate. The characteristics of the four precursors were investigated by thermal, vibrational and X-ray powder diffraction (XRD) analysis. Additionally, the nuclear magnetic resonance, with magic angle spinning ({sup 27}Al MAS NMR), was used to verify the coordination of aluminum cations. Each precursor was calcined at various temperatures generating alumina polymorphs, which were structurally analyzed by XRD and {sup 27}Al MAS NMR. Due to interest in catalysis supports, special attention was given to the ?-Al{sub 2}O{sub 3} phase, which in addition to structural investigation was subjected to textural analysis. The results showed that, from different synthesis procedures and common route of calcination, one can obtain materials with the same composition but with different structural and textural properties, which in turn can significantly influence the performance of a supported catalyst.

  19. A Novel In-situ Electrochemical Cell for Neutron Diffraction Studies of Phase Transitions in Small Volume Electrodes of Li-ion Batteries

    SciTech Connect (OSTI)

    Vadlamani, Bhaskar S; An, Ke; Jagannathan, M.; Ravi Chandran, K.

    2014-01-01

    The design and performance of a novel in-situ electrochemical cell that greatly facilitates the neutron diffraction study of complex phase transitions in small volume electrodes of Li-ion cells, is presented in this work. Diffraction patterns that are Rietveld-refinable could be obtained simultaneously for all the electrodes, which demonstrates that the cell is best suited to explore electrode phase transitions driven by the lithiation and delithiation processes. This has been facilitated by the use of single crystal (100) Si sheets as casing material and the planar cell configuration, giving improved signal-to-noise ratio relative to other casing materials. The in-situ cell has also been designed for easy assembly and to facilitate rapid experiments. The effectiveness of cell is demonstrated by tracking the neutron diffraction patterns during the charging of graphite/LiCoO2 and graphite/LiMn2O4 cells. It is shown that good quality neutron diffraction data can be obtained and that most of the finer details of the phase transitions, and the associated changes in crystallographic parameters in these electrodes, can be captured.

  20. Deformation mechanisms in a precipitation-strengthened ferritic superalloy revealed by in situ neutron diffraction studies at elevated temperatures

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Huang, Shenyan; Gao, Yanfei; An, Ke; Zheng, Lili; Wu, Wei; Teng, Zhenke; Liaw, Peter K

    2014-10-22

    In this study, the ferritic superalloy Fe–10Ni–6.5Al–10Cr–3.4Mo strengthened by ordered (Ni,Fe)Al B2-type precipitates is a candidate material for ultra-supercritical steam turbine applications above 923 K. Despite earlier success in improving its room-temperature ductility, the creep resistance of this material at high temperatures needs to be further improved, which requires a fundamental understanding of the high-temperature deformation mechanisms at the scales of individual phases and grains. In situ neutron diffraction has been utilized to investigate the lattice strain evolution and the microscopic load-sharing mechanisms during tensile deformation of this ferritic superalloy at elevated temperatures. Finite-element simulations based on the crystal plasticitymore » theory are employed and compared with the experimental results, both qualitatively and quantitatively. Based on these interphase and intergranular load-partitioning studies, it is found that the deformation mechanisms change from dislocation slip to those related to dislocation climb, diffusional flow and possibly grain boundary sliding, below and above 873 K, respectively. Insights into microstructural design for enhancing creep resistance are also discussed.« less

  1. Deformation mechanisms in a precipitation-strengthened ferritic superalloy revealed by in situ neutron diffraction studies at elevated temperatures

    SciTech Connect (OSTI)

    Huang, Shenyan; Gao, Yanfei; An, Ke; Zheng, Lili; Wu, Wei; Teng, Zhenke; Liaw, Peter K

    2014-10-22

    In this study, the ferritic superalloy Fe–10Ni–6.5Al–10Cr–3.4Mo strengthened by ordered (Ni,Fe)Al B2-type precipitates is a candidate material for ultra-supercritical steam turbine applications above 923 K. Despite earlier success in improving its room-temperature ductility, the creep resistance of this material at high temperatures needs to be further improved, which requires a fundamental understanding of the high-temperature deformation mechanisms at the scales of individual phases and grains. In situ neutron diffraction has been utilized to investigate the lattice strain evolution and the microscopic load-sharing mechanisms during tensile deformation of this ferritic superalloy at elevated temperatures. Finite-element simulations based on the crystal plasticity theory are employed and compared with the experimental results, both qualitatively and quantitatively. Based on these interphase and intergranular load-partitioning studies, it is found that the deformation mechanisms change from dislocation slip to those related to dislocation climb, diffusional flow and possibly grain boundary sliding, below and above 873 K, respectively. Insights into microstructural design for enhancing creep resistance are also discussed.

  2. Non destructive neutron diffraction measurements of cavities, inhomogeneities, and residual strain in bronzes of Ghiberti's relief from the Gates of Paradise

    SciTech Connect (OSTI)

    Festa, G.; Senesi, R.; Alessandroni, M.; Andreani, C.; Vitali, G.; Porcinai, S.; Giusti, A. M.; Materna, T.; Paradowska, A. M.

    2011-03-15

    Quantitative neutron studies of cultural heritage objects provide access to microscopic, mesoscopic, and macroscopic structures in a nondestructive manner. In this paper we present a neutron diffraction investigation of a Ghiberti Renaissance gilded bronze relief devoted to the measurement of cavities and inhomogeneities in the bulk of the sample, along with the bulk phase composition and residual strain distribution. The quantitative measurements allowed the determination of the re-melting parts extension, as well as improving current knowledge about the manufacturing process. The study provides significant and unique information to conservators and restorators about the history of the relief.

  3. Lithium insertion properties of Li{sub x}TiNb{sub 2}O{sub 7} investigated by neutron diffraction and first-principles modelling

    SciTech Connect (OSTI)

    Catti, Michele; Pinus, Ilya; Knight, Kevin

    2015-09-15

    TiNb{sub 2}O{sub 7}, a good candidate as anode in lithium batteries, was treated with n-butyllithium to synthesize Li{sub x}TiNb{sub 2}O{sub 7} phases similar to those formed during electrochemical reactions. The Li{sub 2.67}TiNb{sub 2}O{sub 7} and Li{sub 3.33}TiNb{sub 2}O{sub 7} compounds, monoclinic C2/m, were studied by time-of-flight powder neutron diffraction. Their crystal structures, containing 3×3 blocks of (Ti,Nb)O{sub 6} octahedra, were Rietveld refined including Li positions. The Li atoms are distributed in similar amounts over sites with (Li–O) Coordination Numbers 5 and 4, although CN=5 should be preferred for having lower energy. Quantum-mechanical calculations were also performed, determining the average charge–discharge voltages to be 1.415 and 1.571 V for Li{sub 3.33}TiNb{sub 2}O{sub 7} and Li{sub 2.67}TiNb{sub 2}O{sub 7}, respectively, in good agreement with experimental results. An analysis of the theoretical charge distribution shows that, on lithiation, the chemical reduction of Ti and Nb atoms concentrates in the more condensed peripheral octahedra of the 3×3 block. This corresponds to electrons moving into a partly spin-polarized small band which gives rise to semi-metallic conductivity. - Graphical abstract: Structure of monoclinic Li{sub 3.33}TiNb{sub 2}O{sub 7}, and corresponding electron density of states. - Highlights: • Lithium was chemically inserted into the battery anode material TiNb{sub 2}O{sub 7}. • Li atoms are distributed over four- and fivefold oxygen coordinated sites. • On lithiation Nb and Ti atoms are reduced according to a peculiar structural pattern. • Theoretically predicted charge–discharge voltages fit experiments very well.

  4. Powder Diffraction Crystallography Instructional Materials

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    to Least-squares Fitting: A mostly descriptive approach A non-rigorous introduction to linear algebra, linear and non-linear least squares and related concepts. Software...

  5. A short note on physical properties to irradiated nuclear fuel by means of X-ray diffraction and neutron scattering techniques

    SciTech Connect (OSTI)

    Abdullah, Yusof Husain, Hishamuddin; Hak, Cik Rohaida Che; Alias, Nor Hayati; Yusof, Mohd Reusmaazran; Kasim, Norasiah Ab; Zali, Nurazila Mat; Mohamed, Abdul Aziz

    2015-04-29

    For nuclear reactor applications, understanding the evolution of the fuel materials microstructure during irradiation are of great importance. This paper reviews the physical properties of irradiated nuclear fuel analysis which are considered to be of most importance in determining the performance behavior of fuel. X-rays diffraction was recognize as important tool to investigate the phase identification while neutron scattering analyses the interaction between uranium and other materials and also investigation of the defect structure.

  6. Hidden Superlattice in Tl2(SC6H4S) and Tl2(SeC6H4Se) Solved from Powder X-ray Diffraction

    SciTech Connect (OSTI)

    K Stone; D Turner; M Singh; T Vaid; P Stephens

    2011-12-31

    The crystal structures of the isostructural title compounds poly[({mu}-benzene-1,4-dithiolato)dithallium], Tl{sub 2}(SC{sub 6}H{sub 4}S), and poly[({mu}-benzene-1,4-diselenolato)dithallium], Tl{sub 2}(SeC{sub 6}H{sub 4}Se), were solved by simulated annealing from high-resolution synchrotron X-ray powder diffraction. Rietveld refinements of an initial structure with one formula unit per triclinic cell gave satisfactory agreement with the data, but led to a structure with impossibly close non-bonded contacts. A disordered model was proposed to alleviate this problem, but an alternative supercell structure leads to slightly improved agreement with the data. The isostructural superlattice structures were confirmed for both compounds through additional data collection, with substantially better counting statistics, which revealed the presence of very weak superlattice peaks not previously seen. Overall, each structure contains Tl-S or Tl-Se two-dimensional networks, connected by phenylene bridges. The sulfur (or selenium) coordination sphere around each thallium is a highly distorted square pyramid or a 'see-saw' shape, depending upon how many Tl-S or Tl-Se interactions are considered to be bonds. In addition, the two compounds contain pairs of Tl{sup I} ions that interact through a closed-shell 'thallophilic' interaction: in the sulfur compound there are two inequivalent pairs of Tl atoms with Tl-Tl distances of 3.49 and 3.58 {angstrom}, while in the selenium compound those Tl-Tl interactions are at 3.54 and 3.63 {angstrom}.

  7. Neutron diffraction study of the martensitic transformation and chemical order in Heusler alloy Ni1.91Mn1.29Ga0.8

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Ari-Gur, Pnina; Garlea, Vasile O.; Cao, Huibo; Ge, Y.; Aaltio, I.; Hannula, S. P.; Koledov, V.

    2015-11-05

    In this study, Heusler alloys of Ni-Mn-Ga compositions demonstrate ferromagnetic shape memory effect in the martensitic state. The transformation temperature and the chemical order depend strongly on the composition. In the current work, the structure and chemical order of the martensitic phase of Ni1.91Mn1.29Ga0.8 were studied using neutron diffraction; the diffraction pattern was refined using the FullProf software. It was determined that the structural transition occurs around 330 K. At room temperature, 300 K, which is below the martensite transformation temperature, all the Bragg reflections can be described by a monoclinic lattice with a symmetry of space group P 1more » 2/m 1 and lattice constants of a = 4.23047(7) [Å], b = 5.58333(6) [Å], c = 21.0179(2) [Å], beta = 90.328(1). The chemical order is of critical importance in these alloys, and it was previously studied at 363 K. Analysis of the neutron diffraction in the monoclinic phase shows that the chemical order is maintained during the martensitic transformation.« less

  8. Neutron diffraction and thermoelectric properties of indium filled In x Co 4 Sb 12 ( x=0.05, 0.2) and indium cerium filled Ce 0.05 In 0.1 Co 4 Sb 12 skutterudites: Neutron diffraction and thermoelectric properties of In/Ce skutterudites

    SciTech Connect (OSTI)

    Sesselmann, Andreas; Klobes, Benedikt; Dasgupta, Titas; Gourdon, Olivier; Hermann, Raphael; Mueller, Eckhard

    2015-09-25

    The thermoelectric properties on polycrystalline single (In) and double filled (Ce, In) skutterudites are characterized between 300 and 700 K. Powder neutron diffraction measurements of the skutterudite compositions InxCo4Sb12 (x= 0.05, 0.2) and Ce0.05In0.1Co4Sb12 as a function of temperature (12- 300 K) were carried out, which gives more insight into the structural data of single and double-filled skutterudites. Our results show that due to the annealing treatment, a Sb deficiency is detectable and thus verifies defects at the Sb lattice site of the skutterudite. Furthermore, we show by electron microprobe analysis that a considerable amount of indium is lost during synthesis and post-processing for the single indium filled samples, but not for the double cerium and indium skutterudite sample. The double-filled skutterudite is superior to the single-filled skutterudite composition due to a higher charge carrier density, a comparable lattice thermal resistivity, and a higher density of states effective mass in our experiment. Finally, we obtained a significantly higher Einstein temperature for the double-filled skutterudite composition in comparison to the single-filled species, which reflects the high sensitivity due to filling of the void lattice position within the skutterudite crystal.

  9. Neutron diffraction study of magnetic field induced behavior in the heavy Fermion Ce3Co4Sn13

    SciTech Connect (OSTI)

    Christianson, Andrew D; Goremychkin, E. A.; Gardner, J. S.; Kang, H. J.; Chung, J.-H.; Manuel, P.; Thompson, J. D.; Sarrao, J. L.; Lawrence, J. M.

    2008-01-01

    The specific heat of Ce3Co4Sn13 exhibits a crossover from heavy Fermion behavior with antiferromagnetic correlations at low field to single impurity Kondo behavior above 2 T. We have performed neutron diffraction measurements in magnetic fields up to 6 Tesla on single crystal samples. The (001) position shows a dramatic increase in intensity in field which appears to arise from static polarization of the 4f level and which at 0.14 K also exhibits an anomaly near 2T reflecting the crossover to single impurity behavior.

  10. Change in the magnetic structure of (Bi,Sm)FeO{sub 3} thin films at the morphotropic phase boundary probed by neutron diffraction

    SciTech Connect (OSTI)

    Maruyama, Shingo; Anbusathaiah, Varatharajan; Takeuchi, Ichiro; Fennell, Amy; Enderle, Mechthild; Ratcliff, William D.

    2014-11-01

    We report on the evolution of the magnetic structure of BiFeO{sub 3} thin films grown on SrTiO{sub 3} substrates as a function of Sm doping. We determined the magnetic structure using neutron diffraction. We found that as Sm increases, the magnetic structure evolves from a cycloid to a G-type antiferromagnet at the morphotropic phase boundary, where there is a large piezoelectric response due to an electric-field induced structural transition. The occurrence of the magnetic structural transition at the morphotropic phase boundary offers another route towards room temperature multiferroic devices.

  11. In-situ neutron diffraction study of martensitic variant redistribution in polycrystalline Ni-Mn-Ga alloy under cyclic thermo-mechanical treatment

    SciTech Connect (OSTI)

    Li, Zongbin; Zou, Naifu; Zhao, Xiang; Zuo, Liang E-mail: yudong.zhang@univ-lorraine.fr; Zhang, Yudong E-mail: yudong.zhang@univ-lorraine.fr; Esling, Claude; Gan, Weimin

    2014-07-14

    The influences of uniaxial compressive stress on martensitic transformation were studied on a polycrystalline Ni-Mn-Ga bulk alloy prepared by directional solidification. Based upon the integrated in-situ neutron diffraction measurements, direct experimental evidence was obtained on the variant redistribution of seven-layered modulated (7M) martensite, triggered by external uniaxial compression during martensitic transformation. Large anisotropic lattice strain, induced by the cyclic thermo-mechanical treatment, has led to the microstructure modification by forming martensitic variants with a strong 〈0 1 0〉{sub 7M} preferential orientation along the loading axis. As a result, the saturation of magnetization became easier to be reached.

  12. Determination of the absolute configuration of (-)-(2R)-succinic-2-d acid by neutron diffraction study: Unambiguous proof of the absolute stereochemistry of the NAD/sup +//NADH interconversion

    SciTech Connect (OSTI)

    Yuan, H.S.H.; Stevens, R.C.; Fujita, S.; Watkins, M.I.; Koetzle, T.F.; Bau, R.

    1988-05-01

    The absolute configuration of the CHD group (D = deuterium) in (-)-(2R)-succinic-2-d acid, as prepared from (-)-(2S,3R)-malic-3-d acid, has been shown unambiguously to be R by the technique of single-crystal neutron diffraction. The optically active cation (+)-phenylethylammonium was used as the chiral reference. The structure of (C/sub 6/H/sub 5/CH/sub 3/CHNH/sub 3/)/sup +/(HOOCCH/sub 2/CHDCOOO)/sup -/ has been studied with x-ray diffraction at room temperature and neutron diffraction at room temperature and neutron diffraction at 100 K. Crystal data from the neutron diffraction analysis of the phenylethylammonium slat of the title compound at 100 K: space group P2/sub 1/; a = 8.407 /angstrom/, b = 8.300 /angstrom/, c = 8.614 /angstrom/, ..beta.. = 91.20/degrees/; unit cell volume = 600.9 /angstrom//sup 3/, Z = 2. The result confirms the stereochemistry of the malate/succinate transformation, as well as the NAD/sup +//NADH interconversion, and demonstrates the usefulness of the single-crystal neutron diffraction method for determining the absolute configuration of molecules having a chiral monodeuteriomethylene group.

  13. In-situ neutron diffraction of LaCoO3 perovskite under uniaxial compression. I. Crystal structure analysis and texture development

    SciTech Connect (OSTI)

    Aman, Amjad; Chen, Yan; Lugovy, Mykola; Orlovskaya, Nina; Reece, Michael John; Ma, Dong; Stoica, Alexandru Dan; An, Ke

    2014-01-01

    The dynamics of texture formation, changes in crystal structure and stress accommodation mechanisms are studied in R3c rhombohedral LaCoO3 perovskite during in-situ uniaxial compression experiment by neutron diffraction. The neutron diffraction revealed the complex crystallographic changes causing the texture formation and significant straining along certain crystallographic directions during in-situ compression, which are responsible for the appearance of hysteresis and non-linear ferroelastic deformation in LaCoO3 perovskite. The irreversible strain after the first loading was connected with the appearance of non-recoverable changes in the intensity ratio of certain crystallographic peaks, causing non-reversible texture formation. However in the second loading/unloading cycle the hysteresis loop was closed and no irreversible strain appears after deformation. The significant texture formation is responsible for increase in the Young s modulus of LaCoO3 at high compressive loads, where the reported values of Young s modulus increase from 76 GPa measured at the very beginning of the loading to 194 GPa at 900 MPa applied compressive stress measured at the beginning of the unloading curve.

  14. In-situ neutron diffraction of LaCoO? perovskite under uniaxial compression. I. Crystal structure analysis and texture development

    SciTech Connect (OSTI)

    Aman, Amjad; Orlovskaya, Nina; Chen, Yan; Lugovy, Mykola; Reece, Michael J.; Ma, Dong; Stoica, Alexandru D.; An, Ke

    2014-07-07

    The dynamics of texture formation, changes in crystal structure, and stress accommodation mechanisms have been studied in perovskite-type R3?c rhombohedral LaCoO? during uniaxial compression using in-situ neutron diffraction. The in-situ neutron diffraction revealed the complex crystallographic changes causing the texture formation and significant straining along certain crystallographic directions during compression, which are responsible for the appearance of hysteresis and non-linear ferroelastic deformation in the LaCoO? perovskite. The irreversible strain after the first loading was connected with the appearance of non-recoverable changes in the intensity ratio of certain crystallographic peaks, causing non-reversible texture formation. However, in the second loading/unloading cycle, the hysteresis loop was closed and no further irrecoverable strain appeared after deformation. The significant texture formation is responsible for an increase in the Young's modulus of LaCoO? at high compressive stresses, ranging from 76 GPa at the very beginning of the loading to 194 GPa at 900 MPa at the beginning of the unloading curve.

  15. Single crystal neutron diffraction study of lattice and magnetic structures of 5M modulated Ni2Mn1.14Ga0.86

    SciTech Connect (OSTI)

    Pramanick, Abhijit; Wang, Xiaoping; An, Ke; Stoica, Alexandru Dan; Hoffmann, Christina; Wang, Xun-Li

    2012-01-01

    A comprehensive description of the crystal and magnetic structures of Ni-Mn-Ga magnetic shape memory alloys is important to understand the physical origins of their magnetoelastic properties. These structural details for an off-stoichiometric Ni2Mn1.14Ga0.86 alloy have been obtained from refinement of high-resolution single crystal neutron diffraction data following a (3+1)-dimensional superspace formalism. In particular, the structure adopts a P2/m( 0 )00 (3+1)-D superspace symmetry with the following fundamental lattice parameters: a=4.255(4) , b=5.613(4) , c=4.216(3) , a commensurate periodicity of 5M and a modulation wave vector of . The magnetic moments are aligned along the b-axis. The modulations for atomic site displacements, site occupancies and magnetic moments are elucidated from a (3+1)-D refinement of the neutron diffraction data. In addition to atomic displacements corresponding to shear waves along <110>, distortions of Ni-centric tetrahedra are also evident. Physical interpretations for the different structural distortions and their relationship with magnetic properties are discussed.

  16. Electronically- and crystal-structure-driven magnetic structures and physical properties of RScSb (R = rare earth) compounds. A neutron diffraction, magnetization and heat capacity study

    SciTech Connect (OSTI)

    Ritter, C; Dhar, S K; Kulkarni, R; Provino, A; Paudyal, Durga; Manfrinetti, Pietro; Gschneidner, Karl A

    2014-08-14

    The synthesis of the new equiatomic RScSb ( R = La-Nd, Sm, Gd-Tm, Lu, Y) compounds has been recently reported. These rare earth compounds crystallize in two different crystal structures, adopting the CeScSi-type ( I 4/ mmm) for the lighter R (La-Nd, Sm) and the CeFeSi-type (P4 /nmm) structure for the heavier R ( R = Gd-Tm, Lu, Y). Here we report the results of neutron diffraction, magnetization and heat capacity measurements on some of these compounds ( R = Ce, Pr, Nd, Gd and Tb). Band structure calculations have also been performed on CeScSb and GdScGe (CeScSi-type), and on GdScSb and TbScSb (CeFeSi-type) to compare and understand the exchange interactions in CeScSi and CeFeSi structure types. The neutron diffraction investigation shows that all five compounds order magnetically, with the highest transition temperature of 66 K in TbScSb and the lowest of about 9 K in CeScSb. The magnetic ground state is simple ferromagnetic (τ = [0 0 0]) in CeScSb, as well in NdScSb for 32 >T > 22 K. Below 22 K a second magnetic transition, with propagation vector τ = [¼ ¼ 0], appears in NdScSb. PrScSb has a magnetic structure within, determined by mostly ferromagnetic interactions and antiferromagnetic alignment of the Pr-sites connected through the I-centering ( τ = [1 0 0]). A cycloidal spiral structure with a temperature dependent propagation vector τ = [δ δ ½] is found in TbScSb. The results of magnetization and heat capacity lend support to the main conclusions derived from neutron diffraction. As inferred from a sharp peak in magnetization, GdScSb orders antiferromagnetically at 56 K. First principles calculations show lateral shift of spin split bands towards lower energy from the Fermi level as the CeScSi-type structure changes to the CeFeSi-type structure. This rigid shift may force the system to transform from exchange split ferromagnetic state to the antiferromagnetic state in RScSb compounds (as seen for example in GdScSb and TbScSb) and is proposed to

  17. [Cu32(H)20{S2P(O i Pr)2 }12 ]: The Largest Number of Hydrides Recorded in a Molecular Nanocluster by Neutron Diffraction

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Dhayal, Rajendra S.; Liao, Jian-Hong; Kahlal, Samia; Wang, Xiaoping; Liu, Yu-Chiao; Chiang, Ming-Hsi; van Zyl, Werner E.; Saillard, Jean-Yves; Liu, C. W.

    2015-04-20

    An air- and moisture-stable nanoscale polyhydrido copper cluster [Cu32(H)20{S2P(O i Pr)2 }12 ] (1H) was synthesized and structurally characterized. The molecular structure of 1H exhibits a hexacapped pseudo-rhombohedral core of 14 Cu atoms sandwiched between two nestlike triangular cupola fragments of (2x9) Cu atoms in an elongated triangular gyrobicupola polyhedron. The discrete Cu32 cluster is stabilized by 12 dithiophosphate ligands and a record number of 20 hydride ligands, which were found by high-resolution neutron diffraction to exhibit tri-, tetra-, and pentacoordinated hydrides in capping and interstitial modes. We conclude that this result was further supported by a density functional theorymore » investigation on the simplified model [Cu32(H)20(S2PH2)12].« less

  18. Expanding Lorentz and spectrum corrections to large volumes of reciprocal space for single-crystal time-of-flight neutron diffraction

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Michels-Clark, Tara M.; Savici, Andrei T.; Lynch, Vickie E.; Wang, Xiaoping; Hoffmann, Christina M.

    2016-03-01

    Evidence is mounting that potentially exploitable properties of technologically and chemically interesting crystalline materials are often attributable to local structure effects, which can be observed as modulated diffuse scattering (mDS) next to Bragg diffraction (BD). BD forms a regular sparse grid of intense discrete points in reciprocal space. Traditionally, the intensity of each Bragg peak is extracted by integration of each individual reflection first, followed by application of the required corrections. In contrast, mDS is weak and covers expansive volumes of reciprocal space close to, or between, Bragg reflections. For a representative measurement of the diffuse scattering, multiple sample orientationsmore » are generally required, where many points in reciprocal space are measured multiple times and the resulting data are combined. The common post-integration data reduction method is not optimal with regard to counting statistics. A general and inclusive data processing method is needed. In this contribution, a comprehensive data analysis approach is introduced to correct and merge the full volume of scattering data in a single step, while correctly accounting for the statistical weight of the individual measurements. Lastly, development of this new approach required the exploration of a data treatment and correction protocol that includes the entire collected reciprocal space volume, using neutron time-of-flight or wavelength-resolved data collected at TOPAZ at the Spallation Neutron Source at Oak Ridge National Laboratory.« less

  19. Performance improvements of wavelength-shifting-fiber neutron detectors using high-resolution positioning algorithms

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Wang, C. L.

    2016-05-17

    On the basis of FluoroBancroft linear-algebraic method [S.B. Andersson, Opt. Exp. 16, 18714 (2008)] three highly-resolved positioning methodswere proposed for wavelength-shifting fiber (WLSF) neutron detectors. Using a Gaussian or exponential-decay light-response function (LRF), the non-linear relation of photon-number profiles vs. x-pixels was linearized and neutron positions were determined. The proposed algorithms give an average 0.03-0.08 pixel position error, much smaller than that (0.29 pixel) from a traditional maximum photon algorithm (MPA). The new algorithms result in better detector uniformity, less position misassignment (ghosting), better spatial resolution, and an equivalent or better instrument resolution in powder diffraction than the MPA. Moreover,more » these characters will facilitate broader applications of WLSF detectors at time-of-flight neutron powder diffraction beamlines, including single-crystal diffraction and texture analysis.« less

  20. Schoenborn wins Bau Neutron Award

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    of LANL's Bioenergy and Biome Sciences group, to receive the 2016 Bau Neutron Diffraction Award. The award recognizes exceptional research achievement in neutron...

  1. Neutron Diffraction Measurement of Residual Stresses, Dislocation Density and Texture in Zr-bonded U-10Mo ''Mini'' Fuel Foils and Plates

    SciTech Connect (OSTI)

    Brown, Donald W.; Okuniewski, M. A.; Sisneros, Thomas A.; Clausen, Bjorn; Moore, G. A.; Balogh, L

    2014-08-07

    Aluminum clad monolithic uranium 10 weight percent molybdenum (U-10Mo) fuel plates are being considered for conversion of several research and test nuclear reactors from high-enriched to low-enriched uranium fuel due to the inherently high density of fissile material. Comprehensive neutron diffraction measurements of the evolution of the textures, residual phase stresses, and dislocation densities in the individual phases of the mini-foils throughout several processing steps and following hot-isostatic pressing to the Al cladding, have been completed. Recovery and recrystallization of the bare U-10Mo fuel foil, as indicated by the dislocation density and texture, are observed depending on the state of the material prior to annealing and the duration and temperature of the annealing process. In general, the HIP procedure significantly reduces the dislocation density, but the final state of the clad plate, both texture and dislocation density, depends strongly on the final processing step of the fuel foil. In contrast, the residual stresses in the clad fuel plate do not depend strongly on the final processing step of the bare foil prior to HIP bonding. Rather, the residual stresses are dominated by the thermal expansion mismatch of the constituent materials of the fuel plate.

  2. A study of suppressed formation of low-conductivity phases in doped Li7La3Zr2O12 garnets by in situ neutron diffraction

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Chen, Yan; Rangasamy, Ezhiylmurugan; dela Cruz, Clarina R.; Liang, Chengdu; An, Ke

    2015-09-28

    Doped Li7La3Zr2O12 garnets, oxide-based solids with good Li+ conductivity and compatibility, show great potential as leading electrolyte material candidates for all-solid-state lithium ion batteries. Still yet, the conductive bulk usually suffers from the presence of secondary phases and the transition towards a low-conductivity tetragonal phase during synthesis. Dopants are designed to stabilize the high-conductive cubic phase and suppress the formation of the low-conductivity phases. In situ neutron diffraction enables a direct observation of the doping effects by monitoring the phase evolutions during garnet synthesis. It reveals the reaction mechanism involving the temporary presence of intermediate phases. The off-stoichiometry due tomore » the liquid Li2CO3 evaporation leads to the residual of the low-conductivity intermediate phase in the as-synthesized bulk. Appropriate doping of an active element may alter the component of the intermediate phases and promote the completion of the reaction. While the dopants aid to stabilize most of the cubic phase, a small amount of tetragonal phase tends to form under a diffusion process. Lastly, the in situ observations provide the guideline of process optimization to suppress the formation of unwanted low-conductivity phases.« less

  3. On the crystal energy and structure of A{sub 2}Ti{sub n}O{sub 2n+1} (A=Li, Na, K) titanates by DFT calculations and neutron diffraction

    SciTech Connect (OSTI)

    Catti, Michele; Pinus, Ilya; Scherillo, Antonella

    2013-09-15

    First-principles quantum-mechanical calculations (CRYSTAL09 code, B3LYP functional) were performed on alkali titanates A{sub 2}Ti{sub n}O{sub 2n+1} with layered structure (n=3,4,6). Monoclinic structural types with unshifted (P2{sub 1}/m) and with shifted (C2/m) layers were considered. Crystal energies and full structural details were obtained for all Li, Na, and K phases. Neutron diffraction data were collected on powder samples of P2{sub 1}/m-Li{sub 2}Ti{sub 3}O{sub 7} (a=9.3146(3), b=3.7522(1), c=7.5447(3) Å, β=97.611(4)°) and C2/m-K{sub 2}Ti{sub 4}O{sub 9} (a=18.2578(8), b=3.79160(9), c=12.0242(4) Å, β=106.459(4)°) and their structures were Rietveld-refined. Computed energies show the P2{sub 1}/m arrangement as favoured over the C2/m one for n=3, and the opposite holds for n=6. In the n=4 case the P2{sub 1}/m configuration is predicted to be more stable for Li and Na, and the C2/m one for K titanates. Analysis of Li–O and K–O crystal-chemical environments from experiment and theory shows that the alkali atom bonding is stabilized/destabilized in the different phases consistently with the energy trend. - Graphical abstract: Display Omitted - Highlights: • The P2{sub 1}/m structure-type is found to be more stable for A{sub 2}Ti{sub 3}O{sub 7} layer titanates. • The C2/m structure-type is found to be more stable for A{sub 2}Ti{sub 6}O{sub 13} layer titanates. • Tetratitanates are predicted to prefer the P2{sub 1}/m (Li and Na) or C2/m (K) structure. • Li–O and K–O bond distances follow a trend consistent with computed phase energies.

  4. Magnetic ordering in TbMn{sub 0.5}Cr{sub 0.5}O{sub 3} studied by neutron diffraction and first-principles calculations

    SciTech Connect (OSTI)

    Staruch, M.; Sharma, V.; Ramprasad, R.; Cruz, C. dela; Jain, M.

    2014-07-21

    The structure and magnetic ordering of bulk TbMn{sub 0.5}Cr{sub 0.5}O{sub 3} was revealed through bulk magnetization and neutron diffraction measurements, and first-principles calculations, respectively. G-type antiferromagnetic ordering of Mn{sup 3+} and Cr{sup 3+} moments was observed in the neutron diffraction data below Nel temperature T{sub N}???84?K. In addition, below ?40?K, short-range magnetic ordering was identified correlating to a ferromagnetic component due to the canting of the moments along the c-axis. The spin configuration is consistent with the first-principles calculations. The magnetic structure revealed in the present TbMn{sub 0.5}Cr{sub 0.5}O{sub 3} sample is distinct from that observed for both end members TbMnO{sub 3} and TbCrO{sub 3}.

  5. Unraveling the Hydrogenation of TiO 2 and Graphene Oxide/TiO 2 Composites in Real Time by in Situ Synchrotron X-ray Powder Diffraction and Pair Distribution Function Analysis

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Nguyen-Phan, Thuy-Duong; Liu, Zongyuan; Luo, Si; Gamalski, Andrew D.; Vovchok, Dimitry; Xu, Wenqian; Stach, Eric A.; Polyansky, Dmitry E.; Fujita, Etsuko; Rodriguez, José A.; et al

    2016-02-18

    The functionalization of graphene oxide (GO) and graphene by TiO2 and other metal oxides has attracted considerable attention due to numerous promising applications in catalysis, energy conversion, and storage. We propose hydrogenation of this class of materials as a promising way to tune catalytic properties by altering the structural and chemical transformations that occur upon H incorporation. We also investigate the structural changes that occur during the hydrogenation process using in situ powder X-ray diffraction and pair distribution function analysis of GO–TiO2 and TiO2 under H2 reduction. Sequential Rietveld refinement was employed to gain insight into the evolution of crystalmore » growth of TiO2 nanoparticles in the presence of two-dimensional (2D) GO nanosheets. GO sheets not only significantly retarded the nucleation and growth of rutile impurities, stabilizing the anatase structure, but was also partially reduced to hydrogenated graphene by the introduction of atomic hydrogen into the honeycomb lattice. We discuss the hydrogenation processes and the resulting composite structure that occurs during the incorporation of atomic H and the dynamic structural transformations that leads to a highly active photocatalyst.« less

  6. Neutron diffraction study of the martensitic transformation and chemical order in Heusler alloy Ni1.91Mn1.29Ga0.8

    SciTech Connect (OSTI)

    Ari-Gur, Pnina; Garlea, Vasile O.; Cao, Huibo; Ge, Y.; Aaltio, I.; Hannula, S. P.; Koledov, V.

    2015-11-05

    In this study, Heusler alloys of Ni-Mn-Ga compositions demonstrate ferromagnetic shape memory effect in the martensitic state. The transformation temperature and the chemical order depend strongly on the composition. In the current work, the structure and chemical order of the martensitic phase of Ni1.91Mn1.29Ga0.8 were studied using neutron diffraction; the diffraction pattern was refined using the FullProf software. It was determined that the structural transition occurs around 330 K. At room temperature, 300 K, which is below the martensite transformation temperature, all the Bragg reflections can be described by a monoclinic lattice with a symmetry of space group P 1 2/m 1 and lattice constants of a = 4.23047(7) [Å], b = 5.58333(6) [Å], c = 21.0179(2) [Å], beta = 90.328(1). The chemical order is of critical importance in these alloys, and it was previously studied at 363 K. Analysis of the neutron diffraction in the monoclinic phase shows that the chemical order is maintained during the martensitic transformation.

  7. Neutron diffraction, Mössbauer effect and electron paramagnetic resonance studies on multiferroic Pb(Fe{sub 2/3}W{sub 1/3})O{sub 3}

    SciTech Connect (OSTI)

    Matteppanavar, Shidaling; Angadi, Basavaraj; Rayaprol, Sudhindra; AV, Anupama; Sahoo, Balaram

    2015-06-24

    Multiferroic Pb(Fe{sub 2/3}W{sub 1/3})O{sub 3} ceramics were synthesized via a modified two-stage Columbite method. Single phase formation was confirmed from the analysis of x-ray and neutron diffraction patterns recorded at room temperature. Structural analysis of the diffraction data reveals cubic phase (space group Pm-3m) for the title compound. Magnetic structure of the title compound at room temperature exhibits G-type antiferromagnetic structure. The Mössbauer spectroscopy and Electron Paramagnetic Resonance (EPR) studies were carried out at 300 K. The isomer shift and quadrupole splitting of the Mössbauer spectra confirms the trivalent state of iron (Fe{sup 3+}). The Mössbauer spectra also suggest that the iron and tungsten are randomly distributed at the octahedral, B site. EPR spectra show a single broad line associated with Fe{sup 3+} ions. Both spectra clearly exhibit weak ferromagnetic behaviour of Pb(Fe{sub 2/3}W{sub 1/3})O{sub 3} ceramic at 300 K. Considering neutron diffraction, Mössbauer and EPR results together, it may be stated here that Pb(Fe{sub 2/3}W{sub 1/3})O{sub 3} exhibits antiferromagnetic behavior along with weak ferromagnetism at room temperature.

  8. Portable X-Ray Diffraction (XRD) | Open Energy Information

    Open Energy Info (EERE)

    X-ray powder diffraction, which has traditionally been used in geology, environmental science, material science, and engineering to rapidly identify unknown crystalline...

  9. X-Ray Diffraction (XRD) | Open Energy Information

    Open Energy Info (EERE)

    under investigation. X-ray powder diffraction is widely used in geology, environmental science, material science, and engineering to rapidly identify unknown crystalline substances...

  10. A neutron diffraction study and mode analysis of compounds of the system La{sub 1−x}Sr{sub x}FeO{sub 3−x}F{sub x} (x=1, 0.8, 0.5, 0.2) and an investigation of their magnetic properties

    SciTech Connect (OSTI)

    Clemens, Oliver; Berry, Frank J.; Wright, Adrian J.; Knight, Kevin S.; Perez-Mato, J.M.; Igartua, J.M.; Slater, Peter R.

    2013-10-15

    We report here a detailed study of the system La{sub 1−x}Sr{sub x}FeO{sub 3−x}F{sub x}, by neutron powder diffraction- and magnetic-measurements. All the compounds are robust antiferromagnetics with ordering temperatures well above room temperature. Magnetic moments are shown to align parallel to the c-axis. FC-ZFC measurements indicate a small canting of the magnetic moments, resulting in a ferromagnetic component with a maximum for La{sub 0.5}Sr{sub 0.5}FeO{sub 2.5}F{sub 0.5}. We show that the system exhibits a composition-driven transition from a phase, for low fluorination levels (x≤0.5), with Pnma symmetry and the usual system of octahedral tiltings, to a phase with space group Imma for higher fluorine contents, where a correlated distortion of the oxygen octahedra plays a significant role. The consistency of the structural models, with respect to the expected continuity of the amplitudes of the different distortion modes and the invariance of their internal form, was monitored through the symmetry mode decomposition of the structures. - Graphical abstract: The crystal and magnetic structure of La{sub 0.5}Sr{sub 0.5}FeO{sub 2.5}F{sub 0.5}. Display Omitted - Highlights: • The compounds La{sub 1−x}Sr{sub x}FeO{sub 3−x}F{sub x} (x=1, 0.8, 0.5, 0.2) were studied by neutron diffraction. • A mode analysis shows lower symmetry for Sr rich compounds than previously reported. • SrFeO{sub 2}F crystallizes in the orthorhombic space group Imma. • Magnetic moments resulting from canting depend on metric distortion. • The magnetic structure was determined for La{sub 0.5}Sr{sub 0.5}FeO{sub 2.5}F{sub 0.5}.

  11. Neutron diffraction study of the crystal structure and structural phase transition of La{sub 0.7}Ca{sub 0.3-x}Sr{sub x}CrO{sub 3} (0<=x<=0.3)

    SciTech Connect (OSTI)

    Omoto, Kazuki; Norberg, Stefan T.; Hull, Steve; Aoto, Akimitsu; Hashimoto, Takuya

    2010-02-15

    The crystal structure of the La{sub 0.7}Ca{sub 0.3-x}Sr{sub x}CrO{sub 3} series, including the compositional and temperature dependence of the structural parameters, has been studied by variable temperature neutron diffraction measurements. The extent of the distortions from the ideal cubic perovskite structure has been evaluated quantitatively using the average bond lengths and the mean volumes of the [CrO{sub 6}] octahedron and [(La/Ca/Sr)O{sub 12}] polyhedron, and has been shown to decrease with increase of Sr content or temperature. At the structural phase transition from the orthorhombic (Pnma) structure to the rhombohedral (R3-barc) one, the volume of the [CrO{sub 6}] octahedron decreases whereas that of the [(La/Ca/Sr)O{sub 12}] polyhedron shows little difference, resulting in an overall decrease in the level of distortion. The change in the degree of distortion at the phase transition decreases with increase of Sr content, in agreement with the smaller variation of the enthalpy and volume for the specimens with higher Sr content. - Graphical abstract: Temperature dependence of parameter, PHI, representing the extent of distortion from the ideal cubic perovskite structure, for La{sub 0.7}Ca{sub 0.3}CrO{sub 3} (diamonds) and La{sub 0.7}Ca{sub 0.15}Sr{sub 0.15}CrO{sub 3} (circles) calculated from neutron diffraction patterns.

  12. FABRICATION OF NEUTRON SOURCES

    DOE Patents [OSTI]

    Birden, J.H.

    1959-01-20

    A method is presented for preparing a more efficient neutron source comprising inserting in a container a quantity of Po-210, inserting B powder coated with either Ag, Pt, or Ni. The container is sealed and then slowly heated to about 450 C to volatilize the Po and effect combination of the coated powder with the Po. The neutron flux emitted by the unit is moritored and the heating step is terminated when the flux reaches a maximum or selected level.

  13. NEUTRON SHIELDING STRUCTURE

    DOE Patents [OSTI]

    Mattingly, J.T.

    1962-09-25

    A lightweight neutron shielding structure comprises a honeycomb core which is filled with a neutron absorbing powder. The honeycomb core is faced with parallel planar facing sheets to form a lightweight rigid unit. Suitable absorber powders are selected from among the following: B, B/sub 4/C, B/sub 2/O/ sub 3/, CaB/sub 6/, Li/sub 2/CO3, LiOH, LiBO/sub 2/, Li/s ub 2/O. The facing sheets are constructed of a neutron moderating material, so that fast neutrons will be moderated while traversing the facing sheets, and ultimately be absorbed by the absorber powder in the honeycomb. Beryllium is a preferred moderator material for use in the facing sheets. The advantage of the structure is that it combines the rigidity and light weight of a honeycomb construction with the neutron absorption properties of boron and lithium. (AEC)

  14. Phase stability study of Bi{sub 0.15}Sr{sub 0.85-x}Ae{sub x}CoO{sub 3-{delta}} (x = 0 and Ae = Ba{sub 0.28}; Ca{sub 0.17}) perovskites by in-situ neutron diffraction

    SciTech Connect (OSTI)

    Eriksson, A.K.; Eriksson, S.G.; Chapon, L.C.; Knee, C.S.

    2010-12-15

    The oxygen deficient perovskites, Bi{sub 0.15}Sr{sub 0.85-x}Ae{sub x}CoO{sub 3-{delta}}, x = 0 and Ae{sub x} = Ba{sub 0.28}, Ca{sub 0.17}, were studied with in-situ neutron powder diffraction and combined TGA/DSC in order to investigate their behaviour at elevated temperatures in oxidising conditions. The phase stability of the I4/mmm supercell structure adopted by Bi{sub 0.15}Sr{sub 0.85}CoO{sub 3-{delta}} is shown to be dependent on temperature and the oxygen content of the phase, with three structural events, at T {approx} 250, 590 and 880 {sup o}C, detected. The first transition occurs as the perovskite supercell vanishes due to oxygen absorption; the second transition is also associated with oxidation and involves the decomposition of the perovskite phase via an exothermic process to yield a dominant hexagonal phase. Finally, at T {approx} 900 {sup o}C the perovskite phase re-forms. For the Ba and Ca containing materials the decomposition to the hexagonal phase occurs at T {approx} 600 {sup o}C and {approx} 650 {sup o}C respectively. The presence of Ca at the A-site is found to stabilise the I4/mmm supercell structure in the range RT - 650 {sup o}C. The antiferromagnetic to paramagnetic transitions occur at T{sub N} {approx} 250 {sup o}C, T{sub N} {approx} 175 {sup o}C and T{sub N} {approx} 145 {sup o}C for the samples with Ae{sub x} = Ba{sub 0.28}, x = 0 and Ae{sub x} = Ca{sub 0.17}, respectively.

  15. Quantum Model of Catalysis Based on a Mobile Proton Revealed by Subatomic X-ray and Neutron Diffraction Studies of h-aldose Reductase

    SciTech Connect (OSTI)

    Blakeley, M. P.; Ruiz, Fredrico; Cachau, Raul; Hazemann, I.; Meilleur, Flora; Mitschler, A.; Ginell, Stephan; Afonine, Pavel; Ventura, Oscar; Cousido-Siah, Alexandra; Haertlein, M.; Joachimiak, Andrzej; Myles, Dean A A; Podjarny, A.

    2008-01-01

    We present results of combined studies of the enzyme human aldose reductase (h-AR, 36 kDa) using single-crystal x-ray data (0.66 Angstroms, 100K; 0.80 Angstroms, 15K; 1.75 Angstroms, 293K), neutron Laue data (2.2 Angstroms, 293K), and quantum mechanical modeling. These complementary techniques unveil the internal organization and mobility of the hydrogen bond network that defines the properties of the catalytic engine, explaining how this promiscuous enzyme overcomes the simultaneous requirements of efficiency and promiscuity offering a general mechanistic view for this class of enzymes.

  16. Neutron activation analysis system

    DOE Patents [OSTI]

    Taylor, M.C.; Rhodes, J.R.

    1973-12-25

    A neutron activation analysis system for monitoring a generally fluid media, such as slurries, solutions, and fluidized powders, including two separate conduit loops for circulating fluid samples within the range of radiation sources and detectors is described. Associated with the first loop is a neutron source that emits s high flux of slow and thermal neutrons. The second loop employs a fast neutron source, the flux from which is substantially free of thermal neutrons. Adjacent to both loops are gamma counters for spectrographic determination of the fluid constituents. Other gsmma sources and detectors are arranged across a portion of each loop for deterMining the fluid density. (Official Gazette)

  17. FABRICATION OF NEUTRON SOURCES

    DOE Patents [OSTI]

    Birden, J.H.

    1959-04-21

    A method is presented for preparing a neutron source from polonium-210 and substances, such as beryllium and boron, characterized by emission of neutrons upon exposure to alpha particles from the polonium. According to the invention, a source is prepared by placing powdered beryllium and a platinum foil electroplated with polonium-2;.0 in a beryllium container. The container is sealed and then heated by induction to a temperature of 450 to 1100 deg C to volatilize the polonium off the foil into the powder. The heating step is terminated upon detection of a maximum in the neutron flux level.

  18. Schoenborn wins Bau Neutron Award

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    Schoenborn wins Bau Neutron Award Schoenborn wins Bau Neutron Award The American Crystallographic Association (ACA) has selected retired Laboratory Senior Fellow Benno Schoenborn to receive the 2016 Bau Neutron Diffraction Award. August 12, 2015 Benno Schoenborn Benno Schoenborn Communications Office (505) 667-7000 Schoenborn is honored for his pioneering research in macromolecular neutron crystallography and the design and development of the neutron crystallography beamline (Protein

  19. Neutron diffraction study of the magnetic ordering of the Cu sup ++ spins in Nd sub 1. 5 Ba sub 1. 5 Cu sub 3 O sub 6+x

    SciTech Connect (OSTI)

    Moudden, A.H.; Hennion, B. - Centre d'Etudes Nucleaires de Saclay, 91 - Gif-sur-Yvette ); Schweiss, P. - Centre d'Etudes Nucleaires de Saclay, 91 - Gif-sur-Yvette Kernforschungszentrum Karlsruhe GmbH . Inst. fuer Nukleare Festkoerperphysik); Gehring, P.M.; Shirane, G. (Brookhaven National Lab., Upton, NY (

    1991-01-01

    Elastic neutron scattering experiments performed on single crystals of Nd{sub 1.5}Ba{sub 1.5}Cu{sub 3}O{sub 6+y} reveal successive antiferromagnetic (AF) ordering of the Cu{sup ++} spins. The as grown single crystals show an AF structure characterized by a Neel temperature T{sub N1} {approximately} 390K and a magnetic wave vector (1/2 1/2 0) referring to the tetragonal structure of NdBa{sub 2}Cu{sub 3}O{sub 6}. As the temperature is lowered below T{sub N2} {approximately} 150K, a spin reorientation develops and a second AF ordering with (1/2 1/2 1/2) wave vector is stabilized. When the samples are oxygenated the tetragonal symmetry and the Neel temperature T{sub N1} remain unchanged, whereas the spin reorientation at T{sub N2} is suppressed. The results indicate that the Nd/Ba substitution increases the stability of the tetragonal structure upon the oxygen content. This may induce new possibilities of local oxygen ordering that favour the presence of holes in the deficient layer.

  20. Energetic powder

    DOE Patents [OSTI]

    Jorgensen, Betty S.; Danen, Wayne C.

    2003-12-23

    Fluoroalkylsilane-coated metal particles. The particles have a central metal core, a buffer layer surrounding the core, and a fluoroalkylsilane layer attached to the buffer layer. The particles may be prepared by combining a chemically reactive fluoroalkylsilane compound with an oxide coated metal particle having a hydroxylated surface. The resulting fluoroalkylsilane layer that coats the particles provides them with excellent resistance to aging. The particles can be blended with oxidant particles to form energetic powder that releases chemical energy when the buffer layer is physically disrupted so that the reductant metal core can react with the oxidant.

  1. Preparation and structural study from neutron diffraction data of Pr{sub 5}Mo{sub 3}O{sub 16}

    SciTech Connect (OSTI)

    Martinez-Lope, M.J.; Alonso, J.A.; Sheptyakov, D.; Pomjakushin, V.

    2010-12-15

    The title compound has been prepared as polycrystalline powder by thermal treatments of mixtures of Pr{sub 6}O{sub 11} and MoO{sub 2} in air. In the literature, an oxide with a composition Pr{sub 2}MoO{sub 6} has been formerly described to present interesting catalytic properties, but its true stoichiometry and crystal structure are reported here for the first time. It is cubic, isostructural with CdTm{sub 4}Mo{sub 3}O{sub 16} (space group Pn-3n, Z=8), with a=11.0897(1) A. The structure contains MoO{sub 4} tetrahedral units, with Mo-O distances of 1.788(2) A, fully long-range ordered with PrO{sub 8} polyhedra; in fact it can be considered as a superstructure of fluorite (M{sub 8}O{sub 16}), containing 32 MO{sub 2} fluorite formulae per unit cell, with a lattice parameter related to that of cubic fluorite (a{sub f}=5.5 A) as a{approx}2a{sub f}. A bond valence study indicates that Mo exhibits a mixed oxidation state between 5+ and 6+ (perhaps accounting for the excellent catalytic properties). One kind of Pr atoms is trivalent whereas the second presents a mixed Pr{sup 3+}-Pr{sup 4+} oxidation state. The similarity of the XRD pattern with that published for Ce{sub 2}MoO{sub 6} suggests that this compound also belongs to the same structural type, with an actual stoichiometry Ce{sub 5}Mo{sub 3}O{sub 16}. -- Graphical Abstract: Formerly formulated as Pr{sub 2}MoO{sub 6}, the title compound is a cubic superstructure of fluorite (a=11.0897(1) A, space group Pn-3n) due to the long-range ordering of PrO{sub 8} scalenohedra and MoO{sub 4} tetrahedral units, showing noticeable shifts of the oxygen positions in order to provide a tetrahedral coordination for Mo ions. A mixed valence Mo{sup 5+}-Mo{sup 6+} is identified, which could account for the excellent catalytic properties of this material. Display Omitted

  2. Incommensurate magnetic ordering in Cu{sub 2}Te{sub 2}O{sub 5}X{sub 2} (X=Cl,Br) studied by single crystal neutron diffraction

    SciTech Connect (OSTI)

    Zaharko, O.; Roennow, H.; Mesot, J.; Crowe, S. J.; Paul, D. McK.; Brown, P. J.; Daoud-Aladine, A.; Meents, A.; Wagner, A.; Prester, M.; Berger, H.

    2006-02-01

    Polarized and unpolarized neutron-diffraction studies have been carried out on single crystals of the coupled spin tetrahedra systems Cu{sub 2}Te{sub 2}O{sub 5}X{sub 2} (X=Cl,Br). A model of the magnetic structure associated with the propagation vectors k{sup '}{sub Cl}{approx_equal}(-0.150,0.422,(1/2)) and k{sup '}{sub Br}{approx_equal}(-0.172,0.356,(1/2)) and stable below T{sub N}=18 K for X=Cl and T{sub N}=11 K for X=Br is proposed. A feature of the model, common to both the bromide and chloride, is a canted coplanar motif for the four Cu{sup 2+} spins on each tetrahedron which rotates on a helix from cell to cell following the propagation vector. The Cu{sup 2+} magnetic moment determined for X=Br,0.395(5){mu}{sub B}, is significantly less than for X=Cl,0.88(1){mu}{sub B} at 2 K. The magnetic structure of the chloride associated with the wave vector k{sup '} differs from that determined previously for the wave vector k{approx_equal}(0.150,0.422,(1/2)) [O. Zaharko et al., Phys. Rev. Lett. 93, 217206(E) (2004)].

  3. Powder treatment process

    DOE Patents [OSTI]

    Weyand, John D. (Greensburg, PA)

    1988-01-01

    (1) A process comprising spray drying a powder-containing slurry, the slurry containing a powder constituent susceptible of oxidizing under the temperature conditions of the spray drying, while reducing the tendency for oxidation of the constituent by including as a liquid constituent of the slurry an organic liquid; (2) a process comprising spray drying a powder-containing slurry, the powder having been pretreated to reduce content of a powder constituent susceptible of oxidizing under the temperature conditions of the spray drying, the pretreating comprising heating the powder to react the constituent; and (3) a process comprising reacting ceramic powder, grinding the reacted powder, slurrying the ground powder, spray drying the slurried powder, and blending the dried powder with metal powder.

  4. Powder treatment process

    DOE Patents [OSTI]

    Weyand, J.D.

    1988-02-09

    Disclosed are: (1) a process comprising spray drying a powder-containing slurry, the slurry containing a powder constituent susceptible of oxidizing under the temperature conditions of the spray drying, while reducing the tendency for oxidation of the constituent by including as a liquid constituent of the slurry an organic liquid; (2) a process comprising spray drying a powder-containing slurry, the powder having been pretreated to reduce content of a powder constituent susceptible of oxidizing under the temperature conditions of the spray drying, the pretreating comprising heating the powder to react the constituent; and (3) a process comprising reacting ceramic powder, grinding the reacted powder, slurrying the ground powder, spray drying the slurried powder, and blending the dried powder with metal powder. 2 figs.

  5. Powder dispersion system

    DOE Patents [OSTI]

    Gorenz, Heather M.; Brockmann, John E.; Lucero, Daniel A.

    2011-09-20

    A powder dispersion method and apparatus comprising an air eductor and a powder dispensing syringe inserted into a suction connection of the air eductor.

  6. Preparing titanium nitride powder

    DOE Patents [OSTI]

    Bamberger, Carlos E.

    1989-07-04

    A process for making titanium nitride powder by reaction of titanium phosphates with sodium cyanide.

  7. Preparing titanium nitride powder

    DOE Patents [OSTI]

    Bamberger, Carlos E.

    1989-01-01

    A process for making titanium nitride powder by reaction of titanium phosphates with sodium cyanide.

  8. Preparation of metal diboride powders

    DOE Patents [OSTI]

    Brynestad, J.; Bamberger, C.E.

    Finely-divided titanium diboride or zirconium diboride powders are formed by reacting gaseous boron trichloride with a material selected from the group of consisting of titanium powder, zirconium powder, titanium dichloride powder, titanium trichloride powder, and gaseous titanium trichloride.

  9. Preparation of titanium diboride powder

    DOE Patents [OSTI]

    Brynestad, Jorulf; Bamberger, Carlos E.

    1985-01-01

    Finely-divided titanium diboride or zirconium diboride powders are formed by reacting gaseous boron trichloride with a material selected from the group consisting of titanium powder, zirconium powder, titanium dichloride powder, titanium trichloride powder, and gaseous titanium trichloride.

  10. Structural study of (N{sub 2}H{sub 5},H){sub 2.9}U{sub 1.1}Ce{sub 0.9}(C{sub 2}O{sub 4}){sub 5}·10H{sub 2}O from a conventional X-ray diffraction diagram obtained on a powder synthesized by a fast vortex process

    SciTech Connect (OSTI)

    Brackx, E.; Laval, J.P.; Dugne, O.; Feraud, J.P.; Arab-Chapelet, B.

    2015-01-15

    In the context of research on U/minor actinides for nuclear fuel reprocessing in the transmutation process, developments are first studied with surrogates containing uranium and lanthanides to facilitate testing. The tests consist of precipitating and calcining a hydrazinium uranium/cerium oxalate. The structure of this oxalate had not been previously determined, but was necessary to validate the physicochemical mechanisms involved. The present study, firstly demonstrates the structural similarity of the U/Ce oxalate phase (N{sub 2}H{sub 5},H){sub 2.9}U{sub 1.1}Ce{sub 0.9}(C{sub 2}O{sub 4}){sub 5}·10H{sub 2}O, synthesized using a vortex precipitator for continuous synthesis of actinide oxalates, with previously known oxalates, crystallizing in P6{sub 3}/mmc symmetry, obtained by more classical methods. This fast precipitation process induces massive nucleation of fine powders. Their structural and microstructural determination confirms that the raw and dried phases belong to the same structural family as (NH{sub 4}){sub 2}U{sub 2}(C{sub 2}O{sub 4}){sub 5}·0.7H{sub 2}O whose structure was described by Chapelet-Arab in P6{sub 3}/mmc symmetry, using single crystal data. However, they present an extended disorder inside the tunnels of the structure, even after drying at 100 °C, between water and hydrazinium ions. This disorder is directly related to the fast vortex method. This structure determination can be used as a basis for further semi-quantitative analysis on the U/minor actinides products formed under various experimental conditions. - Highlights: • Uranium cerium oxalate precipitate characterization by X-ray powder diffraction. • Morphology characterization by SEM analysis. • Structure determination by unit cell Rietveld refinement.

  11. Clifford G. Shull, Neutron Diffraction, Hydrogen Atoms, and Neutron...

    Office of Scientific and Technical Information (OSTI)

    can then be obtained. Understanding where atoms are in a material and how they interact with one another is the key to understanding a material's properties. "Then we can...

  12. Clifford G. Shull, Neutron Diffraction, Hydrogen Atoms, and Neutron...

    Office of Scientific and Technical Information (OSTI)

    In Professor Shull's opinion the most important problem he worked on at the time dealt with determining the positions of hydrogen atoms in materials. "Hydrogen atoms are ubiquitous ...

  13. Precision powder feeder

    DOE Patents [OSTI]

    Schlienger, M. Eric; Schmale, David T.; Oliver, Michael S.

    2001-07-10

    A new class of precision powder feeders is disclosed. These feeders provide a precision flow of a wide range of powdered materials, while remaining robust against jamming or damage. These feeders can be precisely controlled by feedback mechanisms.

  14. A high temperature diffraction-resistance study of chalcopyrite, CuFeS{sub 2}

    SciTech Connect (OSTI)

    Engin, T.E.; Powell, A.V.; Hull, S.

    2011-08-15

    The electrical, magnetic and structural properties of synthetic chalcopyrite, CuFeS{sub 2}, have been studied up to 873 K using DC resistance measurements performed in-situ during neutron powder diffraction experiments. Under ambient conditions the material adopts the accepted structural model for CuFeS{sub 2} in the space group I4-bar 2d, with the magnetic moment of the Fe{sup 3+} cations aligned along [001]. The electrical resistivity is around 0.3 {Omega} cm under ambient conditions, consistent with semiconductor character, and decreases slightly with increase in temperature until a more abrupt fall occurs in the region 750-800 K. This abrupt change in resistivity is accompanied by a structural transition to a cubic zinc blende structured phase (space group F4-bar 3m) in which Cu{sup +} and Fe{sup 3+} cations are disordered over the same tetrahedral crystallographic sites and by a simultaneous loss of long-range magnetic order. The implications of these results are discussed in the context of previous studies of the chalcopyrite system. - Graphical abstract: Structural, magnetic and electrical properties of CuFeS{sub 2} to 873 K have been investigated using DC resistance measurements, performed in-situ during the collection of powder neutron diffraction data. Highlights: > Structural, magnetic and electronic properties are probed simultaneously. > A fall in resistivity at high temperatures is associated with cation disorder. > The order-disorder transition is accompanied by the loss of magnetic order. > The structural and magnetic phase transition is preceded by a 2-phase region. > Sulphur loss at high temperatures causes the phase transitions to be irreversible.

  15. Multiple feed powder splitter

    DOE Patents [OSTI]

    Lewis, Gary K. (Los Alamos, NM); Less, Richard M. (Los Alamos, NM)

    2002-01-01

    A device for providing uniform powder flow to the nozzles when creating solid structures using a solid fabrication system such as the directed light fabrication (DLF) process. In the DLF process, gas entrained powders are passed through the focal point of a moving high-power laser light which fuses the particles in the powder to a surface being built up in layers. The invention is a device providing uniform flow of gas entrained powders to the nozzles of the DLF system. The device comprises a series of modular splitters which are slidably interconnected and contain an integral flow control mechanism. The device can take the gas entrained powder from between one to four hoppers and split the flow into eight tubular lines which feed the powder delivery nozzles of the DLF system.

  16. Multiple feed powder splitter

    DOE Patents [OSTI]

    Lewis, Gary K. (Los Alamos, NM); Less, Richard M. (Los Alamos, NM)

    2001-01-01

    A device for providing uniform powder flow to the nozzles when creating solid structures using a solid fabrication system such as the directed light fabrication (DLF) process. In the DLF process, gas entrained powders are passed through the focal point of a moving high-power laser light which fuses the particles in the powder to a surface being built up in layers. The invention is a device providing uniform flow of gas entrained powders to the nozzles of the DLF system. The device comprises a series of modular splitters which are slidably interconnected and contain an integral flow control mechanism. The device can take the gas entrained powder from between one to four hoppers and split the flow into eight tubular lines which feed the powder delivery nozzles of the DLF system.

  17. Biaxially textured articles formed by powder metallurgy

    DOE Patents [OSTI]

    Goyal, Amit; Williams, Robert K.; Kroeger, Donald M.

    2003-08-05

    A biaxially textured alloy article having a magnetism less than pure Ni includes a rolled and annealed compacted and sintered powder-metallurgy preform article, the preform article having been formed from a powder mixture selected from the group of ternary mixtures consisting of: Ni powder, Cu powder, and Al powder, Ni powder, Cr powder, and Al powder; Ni powder, W powder and Al powder; Ni powder, V powder, and Al powder; Ni powder, Mo powder, and Al powder; the article having a fine and homogeneous grain structure; and having a dominant cube oriented {100}<100> orientation texture; and further having a Curie temperature less than that of pure Ni.

  18. Defectiveness of the crystal structure of electroerosion powders

    SciTech Connect (OSTI)

    Fominskii, L.P.; Myuller, A.S.; Levchuk, M.V.

    1988-03-01

    The fine structure and defectiveness of metal powder crystal lattices produced by electroerosion dispersion were examined. Dispersion was performed on granulated aluminum, Armco iron, carbon steels, and tungsten. The fine structure was examined by x-ray diffraction. Harmonic analysis was performed using a computer and a program which calculates not only the expansion coefficients of the functions into a Fourier series but also the microdistortions and the dimensions of the mosaic blocks. Electroerosion powders were found to have higher density of crystal lattice defects which can increase their chemical and catalytic activity, improve the metallic electroerosion powder passivation, and increase their corrosion resistance.

  19. Neutronic reactor

    DOE Patents [OSTI]

    Wende, Charles W. J.; Babcock, Dale F.; Menegus, Robert L.

    1983-01-01

    A nuclear reactor includes an active portion with fissionable fuel and neutron moderating material surrounded by neutron reflecting material. A control element in the active portion includes a group of movable rods constructed of neutron-absorbing material. Each rod is movable with respect to the other rods to vary the absorption of neutrons and effect control over neutron flux.

  20. Three-dimensional boron particle loaded thermal neutron detector

    DOE Patents [OSTI]

    Nikolic, Rebecca J.; Conway, Adam M.; Graff, Robert T.; Kuntz, Joshua D.; Reinhardt, Catherine; Voss, Lars F.; Cheung, Chin Li; Heineck, Daniel

    2014-09-09

    Three-dimensional boron particle loaded thermal neutron detectors utilize neutron sensitive conversion materials in the form of nano-powders and micro-sized particles, as opposed to thin films, suspensions, paraffin, etc. More specifically, methods to infiltrate, intersperse and embed the neutron nano-powders to form two-dimensional and/or three-dimensional charge sensitive platforms are specified. The use of nano-powders enables conformal contact with the entire charge-collecting structure regardless of its shape or configuration.

  1. Pyrotechnic filled molding powder

    DOE Patents [OSTI]

    Hartzel, Lawrence W.; Kettling, George E.

    1978-01-01

    The disclosure relates to thermosetting molding compounds and more particularly to a pyrotechnic filled thermosetting compound comprising a blend of unfilled diallyl phthalate molding powder and a pyrotechnic mixture.

  2. Biaxially textured articles formed by powder metallurgy

    DOE Patents [OSTI]

    Goyal, Amit; Williams, Robert K.; Kroeger, Donald M.

    2004-09-14

    A biaxially textured alloy article having a magnetism less than pure Ni includes a rolled and annealed compacted and sintered powder-metallurgy preform article, the preform article having been formed from a powder mixture selected from the group of mixtures consisting of: at least 60 at % Ni powder and at least one of Cr powder, W powder, V powder, Mo powder, Cu powder, Al powder, Ce powder, YSZ powder, Y powder, Mg powder, and RE powder; the article having a fine and homogeneous grain structure; and having a dominant cube oriented {100}<100> orientation texture; and further having a Curie temperature less than that of pure Ni.

  3. Biaxially textured articles formed by powder metallurgy

    DOE Patents [OSTI]

    Goyal, Amit; Williams, Robert K.; Kroeger, Donald M.

    2003-07-29

    A biaxially textured alloy article having a magnetism less than pure Ni includes a rolled and annealed compacted and sintered powder-metallurgy preform article, the preform article having been formed from a powder mixture selected from the group of mixtures consisting of: at least 60 at % Ni powder and at least one of Cr powder, W powder, V powder, Mo powder, Cu powder, Al powder, Ce powder, YSZ powder, Y powder, Mg powder, and RE powder; the article having a fine and homogeneous grain structure; and having a dominant cube oriented {100}<100> orientation texture; and further having a Curie temperature less than that of pure Ni.

  4. Biaxially textured articles formed by powder metallurgy

    DOE Patents [OSTI]

    Goyal, Amit; Williams, Robert K.; Kroeger, Donald M.

    2003-08-19

    A biaxially textured alloy article having a magnetism less than pure Ni includes a rolled and annealed compacted and sintered powder-metallurgy preform article, the preform article having been formed from a powder mixture selected from the group of mixtures consisting of: at least 60 at % Ni powder and at least one of Cr powder, W powder, V powder, Mo powder, Cu powder, Al powder, Ce powder, YSZ powder, Y powder, Mg powder, and RE powder; the article having a fine and homogeneous grain structure; and having a dominant cube oriented {100}<100> orientation texture; and further having a Curie temperature less than that of pure Ni.

  5. Biaxially textured articles formed by powder metallurgy

    DOE Patents [OSTI]

    Goyal, Amit; Williams, Robert K.; Kroeger, Donald M.

    2003-08-26

    A biaxially textured alloy article having a magnetism less than pure Ni includes a rolled and annealed compacted and sintered powder-metallurgy preform article, the preform article having been formed from a powder mixture selected from the group of mixtures consisting of: at least 60 at % Ni powder and at least one of Cr powder, W powder, V powder, Mo powder, Cu powder, Al powder, Ce powder, YSZ powder, Y powder, Mg powder, and RE powder; the article having a fine and homogeneous grain structure; and having a dominant cube oriented {100}<100> orientation texture; and further having a Curie temperature less than that of pure Ni.

  6. Biaxially textured articles formed by powder metallurgy

    DOE Patents [OSTI]

    Goyal, Amit; Williams, Robert K.; Kroeger, Donald M.

    2005-01-25

    A biaxially textured alloy article having a magnetism less than pure Ni includes a rolled and annealed compacted and sintered powder-metallurgy preform article, the preform article having been formed from a powder mixture selected from the group of mixtures consisting of: at least 60 at % Ni powder and at least one of Cr powder, W powder, V powder, Mo powder, Cu powder, Al powder, Ce powder, YSZ powder, Y powder, Mg powder, and RE powder; the article having a fine and homogeneous grain structure; and having a dominant cube oriented {100}<100> orientation texture; and further having a Curie temperature less than that of pure Ni.

  7. Biaxially textured articles formed by powder metallurgy

    DOE Patents [OSTI]

    Goval, Amit; Williams, Robert K.; Kroeger, Donald M.

    2005-06-07

    A biaxially textured alloy article having a magnetism less than pure Ni includes a rolled and annealed compacted and sintered powder-metallurgy preform article, the preform article having been formed from a powder mixture selected from the group of mixtures consisting of: at least 60 at % Ni powder and at least one of Cr powder, W powder, V powder, Mo powder, Cu powder, Al powder, Ce powder, YSZ powder, Y powder, Mg powder, and RE powder; the article having a fine and homogeneous grain structure; and having a dominant cube oriented {100}<100> orientation texture; and further having a Curie temperature less than that of pure Ni.

  8. Biaxially textured articles formed by powder metallurgy

    DOE Patents [OSTI]

    Goyal, Amit; Williams, Robert K.; Kroeger, Donald M.

    2005-05-10

    A biaxially textured alloy article having a magnetism less than pure Ni includes a rolled and annealed compacted and sintered powder-metallurgy preform article, the preform article having been formed from a powder mixture selected from the group of mixtures consisting of at least 60 at % Ni powder and at least one of Cr powder, W powder, V powder, Mo powder, Cu powder, Al powder, Ce powder, YSZ powder, Y powder, Mg powder, and RE powder; the article having a fine and homogeneous grain structure; and having a dominant cube oriented {100}<100> orientation texture; and further having a Curie temperature less than that of pure Ni.

  9. Biaxially textured articles formed by powder metallurgy

    DOE Patents [OSTI]

    Goyal, Amit; Williams, Robert K.; Kroeger, Donald M.

    2004-09-28

    A biaxially textured alloy article having a magnetism less than pure Ni includes a rolled and annealed compacted and sintered powder-metallurgy preform article, the preform article having been formed from a powder mixture selected from the group of mixtures consisting of: at least 60 at % Ni powder and at least one of Cr powder, W powder, V powder, Mo powder, Cu powder, Al powder, Ce powder, YSZ powder, Y powder, Mg powder, and RE powder; the article having a fine and homogeneous grain structure; and having a dominant cube oriented {100}<100> orientation texture; and further having a Curie temperature less than that of pure Ni.

  10. Ultrafine hydrogen storage powders

    DOE Patents [OSTI]

    Anderson, Iver E.; Ellis, Timothy W.; Pecharsky, Vitalij K.; Ting, Jason; Terpstra, Robert; Bowman, Robert C.; Witham, Charles K.; Fultz, Brent T.; Bugga, Ratnakumar V.

    2000-06-13

    A method of making hydrogen storage powder resistant to fracture in service involves forming a melt having the appropriate composition for the hydrogen storage material, such, for example, LaNi.sub.5 and other AB.sub.5 type materials and AB.sub.5+x materials, where x is from about -2.5 to about +2.5, including x=0, and the melt is gas atomized under conditions of melt temperature and atomizing gas pressure to form generally spherical powder particles. The hydrogen storage powder exhibits improved chemcial homogeneity as a result of rapid solidfication from the melt and small particle size that is more resistant to microcracking during hydrogen absorption/desorption cycling. A hydrogen storage component, such as an electrode for a battery or electrochemical fuel cell, made from the gas atomized hydrogen storage material is resistant to hydrogen degradation upon hydrogen absorption/desorption that occurs for example, during charging/discharging of a battery. Such hydrogen storage components can be made by consolidating and optionally sintering the gas atomized hydrogen storage powder or alternately by shaping the gas atomized powder and a suitable binder to a desired configuration in a mold or die.

  11. Multilayer dielectric diffraction gratings

    DOE Patents [OSTI]

    Perry, M.D.; Britten, J.A.; Nguyen, H.T.; Boyd, R.; Shore, B.W.

    1999-05-25

    The design and fabrication of dielectric grating structures with high diffraction efficiency used in reflection or transmission is described. By forming a multilayer structure of alternating index dielectric materials and placing a grating structure on top of the multilayer, a diffraction grating of adjustable efficiency, and variable optical bandwidth can be obtained. Diffraction efficiency into the first order in reflection varying between 1 and 98 percent has been achieved by controlling the design of the multilayer and the depth, shape, and material comprising the grooves of the grating structure. Methods for fabricating these gratings without the use of ion etching techniques are described. 7 figs.

  12. Multilayer dielectric diffraction gratings

    DOE Patents [OSTI]

    Perry, Michael D.; Britten, Jerald A.; Nguyen, Hoang T.; Boyd, Robert; Shore, Bruce W.

    1999-01-01

    The design and fabrication of dielectric grating structures with high diffraction efficiency used in reflection or transmission is described. By forming a multilayer structure of alternating index dielectric materials and placing a grating structure on top of the multilayer, a diffraction grating of adjustable efficiency, and variable optical bandwidth can be obtained. Diffraction efficiency into the first order in reflection varying between 1 and 98 percent has been achieved by controlling the design of the multilayer and the depth, shape, and material comprising the grooves of the grating structure. Methods for fabricating these gratings without the use of ion etching techniques are described.

  13. LANSCE | Lujan Center | Instruments | Neutron Radiography

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    Neutron Radiography The recently acquired energy-dispersive neutron imaging detector can be used on various Lujan Center beam-lines to combine scattering with imaging. In most cases, FP5 is the default beam-line for the unique energy-dispersive neutron imaging capabilities, but for instance experiments could benefit from combined diffraction on HIPPO, SMARTS, and NPDF. Please contact Sven Vogel (sven@lanl.gov, 505.667.7016) for further discussions of dedicated or combined energy-dispersive

  14. Diffraction with CMS

    SciTech Connect (OSTI)

    Pereira, Antonio Vilela

    2011-07-15

    The observation of diffraction at LHC with the CMS detector at {radical}(s) = 900 and 2360 GeV is presented, along with a comparison of the data with the predictions of the PYTHIA and PHOJET generators.

  15. SAXS-Diffraction_Workshop

    Broader source: All U.S. Department of Energy (DOE) Office Webpages (Extended Search)

    Workshop on Small-angle X-ray ScatteringDiffraction in Biology October 21, 1998 SPEAKERS Dimitri Svergun, EMBL-Hamburg John E. Johnson, The Scripps Research Institute Wah Chiu, ...

  16. Iowa Powder Atomization Technologies

    ScienceCinema (OSTI)

    None

    2013-03-01

    The same atomization effect seen in a fuel injector is being applied to titanium metal resulting in fine titanium powders that are less than half the width of a human hair. Titanium melts above 3,000°F and is highly corrosive therefore requiring specialized containers. The liquid titanium is poured through an Ames Laboratory - USDOE patented tube which is intended to increase the energy efficiency of the atomization process, which has the ability to dramatically decrease the cost of fine titanium powders. This novel process could open markets for green manufacturing of titanium components from jet engines to biomedical implants.

  17. Iowa Powder Atomization Technologies

    SciTech Connect (OSTI)

    2012-01-01

    The same atomization effect seen in a fuel injector is being applied to titanium metal resulting in fine titanium powders that are less than half the width of a human hair. Titanium melts above 3,000°F and is highly corrosive therefore requiring specialized containers. The liquid titanium is poured through an Ames Laboratory - USDOE patented tube which is intended to increase the energy efficiency of the atomization process, which has the ability to dramatically decrease the cost of fine titanium powders. This novel process could open markets for green manufacturing of titanium components from jet engines to biomedical implants.

  18. Reflective diffraction grating

    DOE Patents [OSTI]

    Lamartine, Bruce C.

    2003-06-24

    Reflective diffraction grating. A focused ion beam (FIB) micromilling apparatus is used to store color images in a durable medium by milling away portions of the surface of the medium to produce a reflective diffraction grating with blazed pits. The images are retrieved by exposing the surface of the grating to polychromatic light from a particular incident bearing and observing the light reflected by the surface from specified reception bearing.

  19. Correlating sampling and intensity statistics in nanoparticle diffraction experiments

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Öztürk, Hande; Yan, Hanfei; Hill, John P.; Noyan, I. Cevdet

    2015-07-28

    It is shown in a previous article [Öztürk, Yan, Hill & Noyan (2014).J. Appl. Cryst.47, 1016–1025] that the sampling statistics of diffracting particle populations within a polycrystalline ensemble depended on the size of the constituent crystallites: broad X-ray peak breadths enabled some nano-sized particles to contribute more than one diffraction spot to Debye–Scherrer rings. Here it is shown that the equations proposed by Alexander, Klug & Kummer [J. Appl. Phys.(1948),19, 742–753] (AKK) to link diffracting particle and diffracted intensity statistics are not applicable if the constituent crystallites of the powder are below 10 nm. In this size range, (i) themore » one-to-one correspondence between diffracting particles and Laue spots assumed in the AKK analysis is not satisfied, and (ii) the crystallographic correlation between Laue spots originating from the same grain invalidates the assumption that all diffracting plane normals are randomly oriented and uncorrelated. Such correlation produces unexpected results in the selection of diffracting grains. For example, three or more Laue spots from a given grain for a particular reflection can only be observed at certain wavelengths. In addition, correcting the diffracted intensity values by the traditional Lorentz term, 1/cos θ, to compensate for the variation of particles sampled within a reflection band does not maintain fidelity to the number of poles contributing to the diffracted signal. A new term, cos θB/cos θ, corrects this problem.« less

  20. Method for synthesizing powder materials

    DOE Patents [OSTI]

    Buss, R.J.; Ho, P.

    1988-01-21

    A method for synthesizing ultrafine powder materials, for example, ceramic and metal powders, comprises admitting gaseous reactants from which the powder material is to be formed into a vacuum reaction chamber maintained at a pressure less than atmospheric and at a temperature less than about 400/degree/K (127/degree/C). The gaseous reactants are directed through a glow discharge provided in the vacuum reaction chamber to form the ultrafine powder material. 1 fig.

  1. Method to blend separator powders

    SciTech Connect (OSTI)

    Guidotti, Ronald A.; Andazola, Arthur H.; Reinhardt, Frederick W.

    2007-12-04

    A method for making a blended powder mixture, whereby two or more powders are mixed in a container with a liquid selected from nitrogen or short-chain alcohols, where at least one of the powders has an angle of repose greater than approximately 50 degrees. The method is useful in preparing blended powders of Li halides and MgO for use in the preparation of thermal battery separators.

  2. Design and implementation of a multiaxial loading capability during heating on an engineering neutron diffractometer

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Benafan, O.; Padula, S. A.; Skorpenske, H. D.; An, K.; Vaidyanathan, R.

    2014-10-02

    Here we discuss a gripping capability that was designed, implemented, and tested for in situ neutron diffraction measurements during multiaxial loading and heating on the VULCAN engineering materials diffractometer at the spallation neutron source at Oak Ridge National Laboratory.

  3. Neutron skins and neutron stars

    SciTech Connect (OSTI)

    Piekarewicz, J.

    2013-11-07

    The neutron-skin thickness of heavy nuclei provides a fundamental link to the equation of state of neutron-rich matter, and hence to the properties of neutron stars. The Lead Radius Experiment ('PREX') at Jefferson Laboratory has recently provided the first model-independence evidence on the existence of a neutron-rich skin in {sup 208}Pb. In this contribution we examine how the increased accuracy in the determination of neutron skins expected from the commissioning of intense polarized electron beams may impact the physics of neutron stars.

  4. Neutron guide

    DOE Patents [OSTI]

    Greene, Geoffrey L.

    1999-01-01

    A neutron guide in which lengths of cylindrical glass tubing have rectangular glass plates properly dimensioned to allow insertion into the cylindrical glass tubing so that a sealed geometrically precise polygonal cross-section is formed in the cylindrical glass tubing. The neutron guide provides easier alignment between adjacent sections than do the neutron guides of the prior art.

  5. Neutron dosimetry

    DOE Patents [OSTI]

    Quinby, Thomas C.

    1976-07-27

    A method of measuring neutron radiation within a nuclear reactor is provided. A sintered oxide wire is disposed within the reactor and exposed to neutron radiation. The induced radioactivity is measured to provide an indication of the neutron energy and flux within the reactor.

  6. Phase Concentration Determination of Fe16N2 Using State of the Art Neutron Scattering Techniques

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Bennett, S. P.; Feygenson, M.; Jiang, Y.; Zande, B. J.; Zhang, X.; Sankar, S. G.; Wang, J. P.; Lauter, V.

    2016-03-25

    Limitation on the availability of rare earth elements have made it imperative that new high energy product rare earth free permanent magnet materials are developed for the next generation of energy systems. One promising low cost permanent magnet candidate for a high energy magnet is -Fe16N2, whose giant magnetic moment has been predicted to be well above any other from conventional first principles calculations. Despite its great promise, the phase is metastable; making synthesis of the pure phase difficult, resulting in less than ideal magnetic characteristics. This instability gives way to a slew of possible secondary phases (i.e. -Fe, Fe2O3,more » Fe8N, Fe4N ) whose concentrations are difficult to detect by conventional x-ray diffraction. Moreover, we show how high resolution neutron diffraction and polarized neutron reflectometry can be used to extract the phase concentration ratio of the giant magnetic phase from ultra-small powder sample sizes (~0.1g) and thin films. These studies have led to the discovery of promising fabrication methods for both homogeneous thin films, and nanopowders containing the highest reported to date (>95%) phase concentrations of room temperature stable -Fe16N2.« less

  7. The Macromolecular Neutron Diffractometer MaNDi at the Spallation Neutron Source

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Coates, Leighton; Cuneo, Matthew J.; Frost, Matthew J.; He, Junhong; Weiss, Kevin L.; McFeeters, Hana; Tomanicek, Stephen J.; Vandavasi, Venu Gopal; Langan, Paul; Iverson, Erik B.

    2015-07-18

    The Macromolecular Neutron Diffractometer (MaNDi) is located on beamline 11B of the Spallation Neutron Source at Oak Ridge National Laboratory. Moreover, the instrument is a neutron time-of-flight wavelength-resolved Laue diffractometer optimized to collect diffraction data from single crystals. Finally, the instrument has been designed to provide flexibility in several instrumental parameters, such as beam divergence and wavelength bandwidth, to allow data collection from a range of macromolecular systems.

  8. The Macromolecular Neutron Diffractometer MaNDi at the Spallation Neutron Source

    SciTech Connect (OSTI)

    Coates, Leighton; Cuneo, Matthew J.; Frost, Matthew J.; He, Junhong; Weiss, Kevin L.; McFeeters, Hana; Tomanicek, Stephen J.; Vandavasi, Venu Gopal; Langan, Paul; Iverson, Erik B.

    2015-07-18

    The Macromolecular Neutron Diffractometer (MaNDi) is located on beamline 11B of the Spallation Neutron Source at Oak Ridge National Laboratory. Moreover, the instrument is a neutron time-of-flight wavelength-resolved Laue diffractometer optimized to collect diffraction data from single crystals. Finally, the instrument has been designed to provide flexibility in several instrumental parameters, such as beam divergence and wavelength bandwidth, to allow data collection from a range of macromolecular systems.

  9. Preparation of superconductor precursor powders

    DOE Patents [OSTI]

    Bhattacharya, Raghunath

    1998-01-01

    A process for the preparation of a precursor metallic powder composition for use in the subsequent formation of a superconductor. The process comprises the steps of providing an electrodeposition bath comprising an electrolyte medium and a cathode substrate electrode, and providing to the bath one or more soluble salts of one or more respective metals which are capable of exhibiting superconductor properties upon subsequent appropriate treatment. The bath is continually energized to cause the metallic and/or reduced particles formed at the electrode to drop as a powder from the electrode into the bath, and this powder, which is a precursor powder for superconductor production, is recovered from the bath for subsequent treatment. The process permits direct inclusion of all metals in the preparation of the precursor powder, and yields an amorphous product mixed on an atomic scale to thereby impart inherent high reactivity. Superconductors which can be formed from the precursor powder include pellet and powder-in-tube products.

  10. Silicon nitride/silicon carbide composite powders

    DOE Patents [OSTI]

    Dunmead, Stephen D.; Weimer, Alan W.; Carroll, Daniel F.; Eisman, Glenn A.; Cochran, Gene A.; Susnitzky, David W.; Beaman, Donald R.; Nilsen, Kevin J.

    1996-06-11

    Prepare silicon nitride-silicon carbide composite powders by carbothermal reduction of crystalline silica powder, carbon powder and, optionally, crystalline silicon nitride powder. The crystalline silicon carbide portion of the composite powders has a mean number diameter less than about 700 nanometers and contains nitrogen. The composite powders may be used to prepare sintered ceramic bodies and self-reinforced silicon nitride ceramic bodies.

  11. A simple procedure to prepare spherical {alpha}-alumina powders

    SciTech Connect (OSTI)

    Liu Hongyu [State Key Laboratory of Fine Chemicals, Dalian University of Technology, Dalian 116012 (China); Ning Guiling [State Key Laboratory of Fine Chemicals, Dalian University of Technology, Dalian 116012 (China)], E-mail: ninggl@dlut.edu.cn; Gan Zhihong; Lin Yuan [State Key Laboratory of Fine Chemicals, Dalian University of Technology, Dalian 116012 (China)

    2009-04-02

    Spherical {alpha}-alumina powders were prepared by the controlled hydrolysis of aluminum isopropoxide in a hydrolysis system consisting of octanol and acetonitrile. Diverse solvents to dissolve reactant formed diverse hydrolysis systems and affected particle shape of {alpha}-alumina powders. The precursors crystallized to {gamma}-alumina at 1000 deg. C and converted to {alpha}-alumina at 1150 deg. C without intermediate phases. The particle morphology of precursor was retained after it crystallized to {alpha}-alumina. The heating rate influenced the particle shape and the state of agglomeration during calcination process. The thermal properties of the precursors were characterized by thermal gravimetric and differential thermal analysis. X-ray diffraction technique was used to confirm the conversion of crystalline phase of alumina powders from amorphous to {alpha}-phase. Transmission electron microscopy was used to investigate the morphologies and size of the precursors and products.

  12. Neutron detector

    DOE Patents [OSTI]

    Stephan, Andrew C.; Jardret; Vincent D.

    2011-04-05

    A neutron detector has a volume of neutron moderating material and a plurality of individual neutron sensing elements dispersed at selected locations throughout the moderator, and particularly arranged so that some of the detecting elements are closer to the surface of the moderator assembly and others are more deeply embedded. The arrangement captures some thermalized neutrons that might otherwise be scattered away from a single, centrally located detector element. Different geometrical arrangements may be used while preserving its fundamental characteristics. Different types of neutron sensing elements may be used, which may operate on any of a number of physical principles to perform the function of sensing a neutron, either by a capture or a scattering reaction, and converting that reaction to a detectable signal. High detection efficiency, an ability to acquire spectral information, and directional sensitivity may be obtained.

  13. Ultracold neutrons

    SciTech Connect (OSTI)

    Saunders, Alexander

    2015-06-22

    This series of slides describes ultracold neutrons (UCN) and their properties, various UCN sources, and an overview of UCN-based experiments. Numerous diagrams and photographs are included.

  14. Conversion method of powder inelastic scattering data for one-dimensional systems

    SciTech Connect (OSTI)

    Tomiyasu, Dr. Keisuke; Fujita, Prof. Masaki; Kolesnikov, Alexander I; Bewley, Robert I.; Bull, Dr. Martyn J.; Bennington, Dr. Stephen M.

    2009-01-01

    Extracting dispersive magnetic excitations from inelastic neutron scattering data usually requires large single crystals. We present a simple yet powerful method for extracting such information from polycrystalline or powder data for one-dimensional systems. We demonstrate the effectiveness of this data treatment by extracting dispersion curves from powder inelastic neutron scattering data on the one-dimensional spin-half systems: CuGeO3 and Rb2Cu2Mo3O12. For many such materials it is not possible to grow sufficiently large crystals and this method offers a quick and efficient way to study their magnetic excitations.

  15. The application of inelastic neutron scattering to explore the significance of a magnetic transition in an iron based Fischer-Tropsch catalyst that is active for the hydrogenation of CO

    SciTech Connect (OSTI)

    Warringham, Robbie; McFarlane, Andrew R.; Lennon, David; MacLaren, Donald A.; Webb, Paul B.; Tooze, Robert P.; Taylor, Jon; Ewings, Russell A.; Parker, Stewart F.

    2015-11-07

    An iron based Fischer-Tropsch synthesis catalyst is evaluated using CO hydrogenation at ambient pressure as a test reaction and is characterised by a combination of inelastic neutron scattering (INS), powder X-ray diffraction, temperature-programmed oxidation, Raman scattering, and transmission electron microscopy. The INS spectrum of the as-prepared bulk iron oxide pre-catalyst (hematite, α-Fe{sub 2}O{sub 3}) is distinguished by a relatively intense band at 810 cm{sup −1}, which has previously been tentatively assigned as a magnon (spinon) feature. An analysis of the neutron scattering intensity of this band as a function of momentum transfer unambiguously confirms this assignment. Post-reaction, the spinon feature disappears and the INS spectrum is characterised by the presence of a hydrocarbonaceous overlayer. A role for the application of INS in magnetic characterisation of iron based FTS catalysts is briefly considered.

  16. NEUTRONIC REACTOR

    DOE Patents [OSTI]

    Fermi, E.; Zinn, W.H.; Anderson, H.L.

    1958-09-16

    Means are presenied for increasing the reproduction ratio of a gaphite- moderated neutronic reactor by diminishing the neutron loss due to absorption or capture by gaseous impurities within the reactor. This means comprised of a fluid-tight casing or envelope completely enclosing the reactor and provided with a valve through which the casing, and thereby the reactor, may be evacuated of atmospheric air.

  17. Neutronic reactor

    DOE Patents [OSTI]

    Wende, Charles W. J.

    1976-08-17

    A safety rod for a nuclear reactor has an inner end portion having a gamma absorption coefficient and neutron capture cross section approximately equal to those of the adjacent shield, a central portion containing materials of high neutron capture cross section and an outer end portion having a gamma absorption coefficient at least equal to that of the adjacent shield.

  18. Neutron source

    DOE Patents [OSTI]

    Cason, J.L. Jr.; Shaw, C.B.

    1975-10-21

    A neutron source which is particularly useful for neutron radiography consists of a vessel containing a moderating media of relatively low moderating ratio, a flux trap including a moderating media of relatively high moderating ratio at the center of the vessel, a shell of depleted uranium dioxide surrounding the moderating media of relatively high moderating ratio, a plurality of guide tubes each containing a movable source of neutrons surrounding the flux trap, a neutron shield surrounding one part of each guide tube, and at least one collimator extending from the flux trap to the exterior of the neutron source. The shell of depleted uranium dioxide has a window provided with depleted uranium dioxide shutters for each collimator. Reflectors are provided above and below the flux trap and on the guide tubes away from the flux trap.

  19. Neutron tubes

    DOE Patents [OSTI]

    Leung, Ka-Ngo; Lou, Tak Pui; Reijonen, Jani

    2008-03-11

    A neutron tube or generator is based on a RF driven plasma ion source having a quartz or other chamber surrounded by an external RF antenna. A deuterium or mixed deuterium/tritium (or even just a tritium) plasma is generated in the chamber and D or D/T (or T) ions are extracted from the plasma. A neutron generating target is positioned so that the ion beam is incident thereon and loads the target. Incident ions cause D-D or D-T (or T-T) reactions which generate neutrons. Various embodiments differ primarily in size of the chamber and position and shape of the neutron generating target. Some neutron generators are small enough for implantation in the body. The target may be at the end of a catheter-like drift tube. The target may have a tapered or conical surface to increase target surface area.

  20. High-Energy X-Ray Diffraction Analysis Tool

    Energy Science and Technology Software Center (OSTI)

    2011-11-29

    The functionality of heRXD includes the following: distance and angular calibration and viewing flat-panel detector images used for X-ray diffraction; image (polar) rebinning or "caking"; line position fitting in powder diffraction images; image segmentation or "blob finding"; crystal orentation indesing; and lattice vector refinement. These functionalities encompass a critical set analyzing teh data for high-energy diffraction measurements that are currently performed at synchrotron sources such as the Advanced Photon Source (APS). The software design modularmore » and open source under LGPL. The intent is to provide a common framework and graphical user interface that has the ability to utillize internal as well as external subroutines to provide various optins for performing the fuctionalities listed above. The software will initially be deployed at several national user facilities--including APS, ALS, and CHESS--and then made available for download using a hosting service such as sourceforge.« less

  1. Correlating sampling and intensity statistics in nanoparticle diffraction experiments

    SciTech Connect (OSTI)

    Öztürk, Hande; Yan, Hanfei; Hill, John P.; Noyan, I. Cevdet

    2015-07-28

    It is shown in a previous article [Öztürk, Yan, Hill & Noyan (2014).J. Appl. Cryst.47, 1016–1025] that the sampling statistics of diffracting particle populations within a polycrystalline ensemble depended on the size of the constituent crystallites: broad X-ray peak breadths enabled some nano-sized particles to contribute more than one diffraction spot to Debye–Scherrer rings. Here it is shown that the equations proposed by Alexander, Klug & Kummer [J. Appl. Phys.(1948),19, 742–753] (AKK) to link diffracting particle and diffracted intensity statistics are not applicable if the constituent crystallites of the powder are below 10 nm. In this size range, (i) the one-to-one correspondence between diffracting particles and Laue spots assumed in the AKK analysis is not satisfied, and (ii) the crystallographic correlation between Laue spots originating from the same grain invalidates the assumption that all diffracting plane normals are randomly oriented and uncorrelated. Such correlation produces unexpected results in the selection of diffracting grains. For example, three or more Laue spots from a given grain for a particular reflection can only be observed at certain wavelengths. In addition, correcting the diffracted intensity values by the traditional Lorentz term, 1/cos θ, to compensate for the variation of particles sampled within a reflection band does not maintain fidelity to the number of poles contributing to the diffracted signal. A new term, cos θB/cos θ, corrects this problem.

  2. Multilayer diffraction grating

    DOE Patents [OSTI]

    Barbee, Jr., Troy W.

    1990-01-01

    This invention is for a reflection diffraction grating that functions at X-ray to VUV wavelengths and at normal angles of incidence. The novel grating is comprised of a laminar grating of period D with flat-topped grating bars. A multiplicity of layered synthetic microstructures, of period d and comprised of alternating flat layers of two different materials, are disposed on the tops of the grating bars of the laminar grating. In another embodiment of the grating, a second multiplicity of layered synthetic microstructures are also disposed on the flat faces, of the base of the grating, between the bars. D is in the approximate range from 3,000 to 50,000 Angstroms, but d is in the approximate range from 10 to 400 Angstroms. The laminar grating and the layered microstructures cooperatively interact to provide many novel and beneficial instrumentational advantages.

  3. Multilayer diffraction grating

    DOE Patents [OSTI]

    Barbee, T.W. Jr.

    1990-04-10

    This invention is for a reflection diffraction grating that functions at X-ray to VUV wavelengths and at normal angles of incidence. The novel grating is comprised of a laminar grating of period D with flat-topped grating bars. A multiplicity of layered synthetic microstructures, of period d and comprised of alternating flat layers of two different materials, are disposed on the tops of the grating bars of the laminar grating. In another embodiment of the grating, a second multiplicity of layered synthetic microstructures are also disposed on the flat faces, of the base of the grating, between the bars. D is in the approximate range from 3,000 to 50,000 Angstroms, but d is in the approximate range from 10 to 400 Angstroms. The laminar grating and the layered microstructures cooperatively interact to provide many novel and beneficial instrumentational advantages. 2 figs.

  4. Phase shifting diffraction interferometer

    DOE Patents [OSTI]

    Sommargren, Gary E.

    1996-01-01

    An interferometer which has the capability of measuring optical elements and systems with an accuracy of .lambda./1000 where .lambda. is the wavelength of visible light. Whereas current interferometers employ a reference surface, which inherently limits the accuracy of the measurement to about .lambda./50, this interferometer uses an essentially perfect spherical reference wavefront generated by the fundamental process of diffraction. This interferometer is adjustable to give unity fringe visibility, which maximizes the signal-to-noise, and has the means to introduce a controlled prescribed relative phase shift between the reference wavefront and the wavefront from the optics under test, which permits analysis of the interference fringe pattern using standard phase extraction algorithms.

  5. Phase shifting diffraction interferometer

    DOE Patents [OSTI]

    Sommargren, G.E.

    1996-08-29

    An interferometer which has the capability of measuring optical elements and systems with an accuracy of {lambda}/1000 where {lambda} is the wavelength of visible light. Whereas current interferometers employ a reference surface, which inherently limits the accuracy of the measurement to about {lambda}/50, this interferometer uses an essentially perfect spherical reference wavefront generated by the fundamental process of diffraction. This interferometer is adjustable to give unity fringe visibility, which maximizes the signal-to-noise, and has the means to introduce a controlled prescribed relative phase shift between the reference wavefront and the wavefront from the optics under test, which permits analysis of the interference fringe pattern using standard phase extraction algorithms. 8 figs.

  6. The early development of neutron diffraction: Science in the...

    Office of Scientific and Technical Information (OSTI)

    Authors: Mason, Thom 1 ; Gawne, Timothy J 1 ; Nagler, Stephen E 1 ; Nestor, Margaret Boone 2 ; Carpenter, John M 1 + Show Author Affiliations ORNL ORNL Bonnie ORNL ...

  7. Neutron diffraction study and anomalous negative thermal expansion...

    Office of Scientific and Technical Information (OSTI)

    does not result in the emergence of superconductivity or any other new ground state. ... results suggest that the absence of superconductivity in these materials could be related ...

  8. Characterization of welding residual stresses with neutron diffraction

    SciTech Connect (OSTI)

    Wang, X.L.; Spooner, S.; Hubbard, C.R.; Taljat, B.; Feng, Z.

    1998-03-01

    Welding residual stresses are a key concern in the fabrication and use of structural components containing welds. Residual stresses in welds are caused by non-uniform expansion and shrinkage of differently heated zones during the thermal transient of a weld pass. In some alloys, solid state phase transformations occurring during the welding transient contribute additional residual stresses. Manufacturing problems arising from welding residual stresses include cracking and dimensional distortion. During use, tensile stresses in the welded zone limit the fatigue resistance of the component under cyclic loading. In an aggressive environment, tensile welding residual stresses also create a necessary condition for stress-corrosion cracking to take place.

  9. Characterization of Li-ion Batteries using Neutron Diffraction...

    Broader source: Energy.gov (indexed) [DOE]

    Materials Characterization Capabilities at the High Temperature Materials Laboratory and HTML User Program Success Stories Characterization of Materials for Li-ion Batteries: ...

  10. Finite Element Scalar Diffraction Theory Code

    Energy Science and Technology Software Center (OSTI)

    1993-08-18

    This computer code calculates the optical diffraction field for diffraction through two-dimensional apertures to aid optical system design. The code allows plotting of the diffraction field.

  11. Preparation of superconductor precursor powders

    DOE Patents [OSTI]

    Bhattacharya, R.

    1998-08-04

    A process for the preparation of a precursor metallic powder composition for use in the subsequent formation of a superconductor. The process comprises the steps of providing an electrodeposition bath comprising an electrolyte medium and a cathode substrate electrode, and providing to the bath one or more soluble salts of one or more respective metals which are capable of exhibiting superconductor properties upon subsequent appropriate treatment. The bath is continually energized to cause the metallic and/or reduced particles formed at the electrode to drop as a powder from the electrode into the bath, and this powder, which is a precursor powder for superconductor production, is recovered from the bath for subsequent treatment. The process permits direct inclusion of all metals in the preparation of the precursor powder, and yields an amorphous product mixed on an atomic scale to thereby impart inherent high reactivity. Superconductors which can be formed from the precursor powder include pellet and powder-in-tube products. 7 figs.

  12. Preparation of superconductor precursor powders

    DOE Patents [OSTI]

    Bhattacharya, Raghunath; Blaugher, Richard D.

    1995-01-01

    A process for the preparation of a precursor metallic powder composition for use in the subsequent formation of a superconductor. The process comprises the steps of providing an electrodeposition bath comprising an electrolyte medium and a cathode substrate electrode, and providing to the bath one or more soluble salts of one or more respective metals, such as nitrate salts of thallium, barium, calcium, and copper, which are capable of exhibiting superconductor properties upon subsequent appropriate treatment. The bath is continually energized to cause the metallic particles formed at the electrode to drop as a powder from the electrode into the bath, and this powder, which is a precursor powder for superconductor production, is recovered from the bath for subsequent treatment. The process permits direct inclusion of thallium in the preparation of the precursor powder, and yields an amorphous product mixed on an atomic scale to thereby impart inherent high reactivity. Superconductors which can be formed from the precursor powder include pellet and powder-in-tube products.

  13. Cryogenic Neutron Protein Crystallography: routine methods and potential benefits

    SciTech Connect (OSTI)

    Weiss, Kevin L; Tomanicek, Stephen J; NG, Joseph D

    2014-01-01

    The use of cryocooling in neutron diffraction has been hampered by several technical challenges such as the need for specialized equipment and techniques. Recently we have developed and deployed equipment and strategies that allow for routine neutron data collection on cryocooled crystals using off the shelf components. This system has several advantages, compared to a closed displex cooling system such as fast cooling coupled with easier crystal mounting and centering. The ability to routinely collect cryogenic neutron data for analysis will significantly broaden the range of scientific questions that can be examined by neutron protein crystallography. Cryogenic neutron data collection for macromolecules has recently become available at the new Biological Diffractometer BIODIFF at FRM II and the Macromolecular Diffractometer (MaNDi) at the Spallation Neutron Source, Oak Ridge National Laboratory. To evaluate the benefits of a cryocooled neutron structure we collected a full neutron data set on the BIODIFF instrument on a Toho-1 lactamase structure at 100K.

  14. Thermal neutron detection system

    DOE Patents [OSTI]

    Peurrung, Anthony J. (Richland, WA); Stromswold, David C. (West Richland, WA)

    2000-01-01

    According to the present invention, a system for measuring a thermal neutron emission from a neutron source, has a reflector/moderator proximate the neutron source that reflects and moderates neutrons from the neutron source. The reflector/moderator further directs thermal neutrons toward an unmoderated thermal neutron detector.

  15. Silica powders for powder evacuated thermal insulating panel and method

    SciTech Connect (OSTI)

    Harris, Michael T.; Basaran, Osman A.; Kollie, Thomas G.; Weaver, Fred J.

    1995-01-01

    A powder evacuated thermal insulating panel using generally spherical and porous silica particles of a median size less than about 100 nanometers in diameter, a pour packing density of about 0.4 to 0.6 g/cm.sup.3 and an external surface area in the range of about 90 to 600 m.sup.2/ g is described. The silica powders are prepared by reacting a tetraakyl silicate with ammonia and water in an alcohol solvent, distilling the solution after the reaction to remove the ammonia and recover the alcohol. The resulting aqueous slurry was dried, ball-milled, and dried again to provide the silica particles with defined internal and external porosity. The nanometer size and the large external surface area of the silica particles along with the internal and external porosity of the silica particles provide powder evacuated thermal insulating panels with significantly higher R-values than obtainable using previously known silica powders.

  16. Silica powders for powder evacuated thermal insulating panel and method

    SciTech Connect (OSTI)

    Harris, M.T.; Basaran, O.A.; Kollie, T.G.; Weaver, F.J.

    1996-01-02

    A powder evacuated thermal insulating panel using generally spherical and porous silica particles of a median size less than about 100 nanometers in diameter, a pour packing density of about 0.4 to 0.6 g/cm{sup 3} and an external surface area in the range of about 90 to 600 m{sup 2}/g is described. The silica powders are prepared by reacting a tetraalkyl silicate with ammonia and water in an alcohol solvent, distilling the solution after the reaction to remove the ammonia and recover the alcohol. The resulting aqueous slurry was dried, ball-milled, and dried again to provide the silica particles with defined internal and external porosity. The nanometer size and the large external surface area of the silica particles along with the internal and external porosity of the silica particles provide powder evacuated thermal insulating panels with significantly higher R-values than obtainable using previously known silica powders. 2 figs.

  17. Silica powders for powder evacuated thermal insulating panel and method

    SciTech Connect (OSTI)

    Harris, Michael T.; Basaran, Osman A.; Kollie, Thomas G.; Weaver, Fred J.

    1994-01-01

    A powder evacuated thermal insulating panel using generally spherical and porous silica particles of a median size less than about 100 nanometers in diameter, a pour packing density of about 0.4 to 0.6 g/cm.sup.3 and an external surface area in the range of about 90 to 600 m.sup.2 /g is described. The silica powders are prepared by reacting a tetraakyl silicate with ammonia and water in an alcohol solvent, distilling the solution after the reaction to remove the ammonia and recover the alcohol. The resulting aqueous slurry was dried, ball-milled, and dried again to provide the silica particles with defined internal and external porosity. The nanometer size and the large external surface area of the silica particles along with the internal and external porosity of the silica particles provide powder evacuated thermal insulating panels with significantly higher R-values than obtainable using previously known silica powders.

  18. Silica powders for powder evacuated thermal insulating panel and method

    SciTech Connect (OSTI)

    Harris, Michael T.; Basaran, Osman A.; Kollie, Thomas G.; Weaver, Fred J.

    1996-01-01

    A powder evacuated thermal insulating panel using generally spherical and porous silica particles of a median size less than about 100 nanometers in diameter, a pour packing density of about 0.4 to 0.6 g/cm.sup.3 and an external surface area in the range of about 90 to 600 m.sup.2/ g is described. The silica powders are prepared by reacting a tetraakyl silicate with ammonia and water in an alcohol solvent, distilling the solution after the reaction to remove the ammonia and recover the alcohol. The resulting aqueous slurry was dried, ball-milled, and dried again to provide the silica particles with defined internal and external porosity. The nanometer size and the large external surface area of the silica particles along with the internal and external porosity of the silica particles provide powder evacuated thermal insulating panels with significantly higher R-values than obtainable using previously known silica powders.

  19. Method for molding ceramic powders

    DOE Patents [OSTI]

    Janney, Mark A.

    1990-01-01

    A method for molding ceramic powders comprises forming a slurry mixture including ceramic powder, a dispersant for the metal-containing powder, and a monomer solution. The monomer solution includes at least one multifunctional monomer, a free-radical initiator, and an organic solvent. The slurry mixture is transferred to a mold, and the mold containing the slurry mixture is heated to polymerize and crosslink the monomer and form a firm polymer-solvent gel matrix. The solid product may be removed from the mold and heated to first remove the solvent and subsequently remove the polymer, whereafter the product may be sintered.

  20. Method for molding ceramic powders

    DOE Patents [OSTI]

    Janney, M.A.

    1990-01-16

    A method for molding ceramic powders comprises forming a slurry mixture including ceramic powder, a dispersant for the metal-containing powder, and a monomer solution. The monomer solution includes at least one multifunctional monomer, a free-radical initiator, and an organic solvent. The slurry mixture is transferred to a mold, and the mold containing the slurry mixture is heated to polymerize and crosslink the monomer and form a firm polymer-solvent gel matrix. The solid product may be removed from the mold and heated to first remove the solvent and subsequently remove the polymer, where after the product may be sintered.

  1. NEUTRONIC REACTORS

    DOE Patents [OSTI]

    Wigner, E.P.

    1960-11-22

    A nuclear reactor is described wherein horizontal rods of thermal- neutron-fissionable material are disposed in a body of heavy water and extend through and are supported by spaced parallel walls of graphite.

  2. NEUTRONIC REACTOR

    DOE Patents [OSTI]

    Wade, E.J.

    1958-09-16

    This patent relates to a reflector means for a neutronic reactor. A reflector comprised of a plurality of vertically movable beryllium control members is provided surrounding the sides of the reactor core. An absorber of fast neutrons comprised of natural uramum surrounds the reflector. An absorber of slow neutrons surrounds the absorber of fast neutrons and is formed of a plurality of beryllium blocks having natural uranium members distributcd therethrough. in addition, a movable body is positioned directly below the core and is comprised of a beryllium reflector and an absorbing member attached to the botiom thereof, the absorbing member containing a substance selected from the goup consisting of natural urantum and Th/sup 232/.

  3. NEUTRONIC REACTOR

    DOE Patents [OSTI]

    Fraas, A.P.; Mills, C.B.

    1961-11-21

    A neutronic reactor in which neutron moderation is achieved primarily in its reflector is described. The reactor structure consists of a cylindrical central "island" of moderator and a spherical moderating reflector spaced therefrom, thereby providing an annular space. An essentially unmoderated liquid fuel is continuously passed through the annular space and undergoes fission while contained therein. The reactor, because of its small size, is particularly adapted for propulsion uses, including the propulsion of aircraft. (AEC)

  4. NEUTRON SOURCES

    DOE Patents [OSTI]

    Richmond, J.L.; Wells, C.E.

    1963-01-15

    A neutron source is obtained without employing any separate beryllia receptacle, as was formerly required. The new method is safer and faster, and affords a source with both improved yield and symmetry of neutron emission. A Be container is used to hold and react with Pu. This container has a thin isolating layer that does not obstruct the desired Pu--Be reaction and obviates procedures previously employed to disassemble and remove a beryllia receptacle. (AEC)

  5. Search for neutrons from deuterated palladium subject to high electrical currents

    SciTech Connect (OSTI)

    Taylor, S.F. |; Claytor, T.N.; Tuggle, D.G.; Jones, S.E.

    1994-04-01

    Tritium has been detected evolving from samples of deuteriated palladium wires and powders subject to pulsed high voltage at Los Alamos. They wanted to measure whether these samples were emitting neutrons. The idea of pulsing current through the wires and powders was to drive the deuterium in and out by rapid electrical heating. With promising tritium results in hand, the experiments were prepared at Los Alamos, and then taken to BYU and run in the neutron detector located in a tunnel in Provo canyon under 35 m of rock and dirt overburden. The neutrons detector and sample setup are described. Results including total neutron counts, time distributions, and an indication of the energy distributions are discussed. The results do not provide compelling evidence of neutron production, but are not inconsistent with earlier measurements of neutrons and tritium. Difficulties in explaining the difference in tritium and neutron measurements are also discussed. Plans for further work are presented.

  6. Neutron range spectrometer

    DOE Patents [OSTI]

    Manglos, S.H.

    1988-03-10

    A neutron range spectrometer and method for determining the neutron energy spectrum of a neutron emitting source are disclosed. Neutrons from the source are colliminated along a collimation axis and a position sensitive neutron counter is disposed in the path of the collimated neutron beam. The counter determines positions along the collimation axis of interactions between the neutrons in the neutron beam and a neutron-absorbing material in the counter. From the interaction positions, a computer analyzes the data and determines the neutron energy spectrum of the neutron beam. The counter is preferably shielded and a suitable neutron-absorbing material is He-3. 1 fig.

  7. Electrically-programmable diffraction grating

    DOE Patents [OSTI]

    Ricco, Antonio J.; Butler, Michael A.; Sinclair, Michael B.; Senturia, Stephen D.

    1998-01-01

    An electrically-programmable diffraction grating. The programmable grating includes a substrate having a plurality of electrodes formed thereon and a moveable grating element above each of the electrodes. The grating elements are electrostatically programmable to form a diffraction grating for diffracting an incident beam of light as it is reflected from the upper surfaces of the grating elements. The programmable diffraction grating, formed by a micromachining process, has applications for optical information processing (e.g. optical correlators and computers), for multiplexing and demultiplexing a plurality of light beams of different wavelengths (e.g. for optical fiber communications), and for forming spectrometers (e.g. correlation and scanning spectrometers).

  8. Study of optical Laue diffraction

    SciTech Connect (OSTI)

    Chakravarthy, Giridhar E-mail: aloksharan@email.com; Allam, Srinivasa Rao E-mail: aloksharan@email.com; Satyanarayana, S. V. M. E-mail: aloksharan@email.com; Sharan, Alok E-mail: aloksharan@email.com

    2014-10-15

    We present the study of the optical diffraction pattern of one and two-dimensional gratings with defects, designed using desktop pc and printed on OHP sheet using laser printer. Gratings so prepared, using novel low cost technique provides good visual aid in teaching. Diffraction pattern of the monochromatic light (632.8nm) from the grating so designed is similar to that of x-ray diffraction pattern of crystal lattice with point defects in one and two-dimensions. Here both optical and x-ray diffractions are Fraunhofer. The information about the crystalline lattice structure and the defect size can be known.

  9. Rotary powder feed through apparatus

    DOE Patents [OSTI]

    Lewis, Gary K. (Los Alamos, NM); Less, Richard M. (Los Alamos, NM)

    2001-01-01

    A device for increasing the uniformity of solids within a solids fabrication system, such as a direct light fabrication (DLF) system in which gas entrained powders are passed through the focal point of a moving high-power light which fuses the particles in the powder to a surface being built up in layers. The invention provides a feed through interface wherein gas entrained powders input from stationary input lines are coupled to a rotating head of the fabrication system. The invention eliminates the need to provide additional slack in the feed lines to accommodate head rotation, and therefore reduces feed line bending movements which induce non-uniform feeding of gas entrained powder to a rotating head.

  10. Powder collection apparatus/method

    DOE Patents [OSTI]

    Anderson, I.E.; Terpstra, R.L.; Moore, J.A.

    1994-01-11

    Device for separating and collecting ultrafine atomized powder from the gas stream of a gas atomizing apparatus comprises a housing having an interior wall oriented at an angle relative to horizontal so as to form a downwardly converging, conical expansion chamber, an inlet conduit communicated to the expansion chamber proximate an upper region thereof for receiving the gas stream, and an outlet proximate a lower region of the expansion chamber. The inlet conduit is oriented at a compound inclined angle (with respect to horizontal) selected to promote separation and collection of powder from the gas stream in the expansion chamber. The compound angle comprises a first entrance angle that is greater than the angle of repose of the powder on the housing interior wall such that any powder accumulation in the inlet conduit tends to flow down the wall toward the outlet. The second angle is selected generally equal to the angle of the housing interior wall measured from the same horizontal plane so as to direct the gas stream into the expansion chamber generally tangent to the housing interior wall to establish a downward swirling gas stream flow in the expansion chamber. A powder collection container is communicated to the outlet of the expansion chamber to collect the powder for further processing. 4 figures.

  11. Neutron diffraction investigation of the evolution of the crystal structure of oxygen-conducting solid solutions (Yb{sub 1-x}Ca{sub x}){sub 2}Ti{sub 2}O{sub 7} (x = 0, 0.05, 0.10)

    SciTech Connect (OSTI)

    Shlyakhtina, A. V.; Sokolov, A. E.; Ul'yanov, V. A.; Trunov, V. A.; Boguslavskii, M. V.; Levchenko, A. V.; Shcherbakova, L. G.

    2009-01-15

    The crystal structure of pyrochlore-like solid solutions (Yb{sub 1-x}Ca{sub x}){sub 2}Ti{sub 2}O{sub 7} (x = 0, 0.05, 0.10) synthesized by high-temperature annealing of mechanically activated initial oxides at temperatures of 1300-1500 deg. C is studied using neutron diffraction. It is found that the Ca{sup 2+} cations are located in the ytterbium sublattice, which apparently favors the splitting of one of the oxygen sublattices [O(2) (48f)] of the pyrochlore structure: the decrease in the occupancy of this sublattice is accompanied by the formation of a new sublattice O(3) (8b), whereas the other oxygen sublattice O(1) (8a) remains unchanged. This rearrangement of the anions in the oxygen subsystem due to the incorporation of an alkaline-earth cation explains the high ionic conductance ({approx}0.2 S/cm at 1000 deg. C) for (Yb{sub 0.9}Ca{sub 0.1}){sub 2}Ti{sub 2}O{sub 7} {approx} 0.2, which is the maximum value observed to date for pyrochlores of the A{sub 2}B{sub 2}O{sub 7} type, where A = Ln and B is a Subgroup IVA element of the periodic system. The bulk and grain-boundary components of the conductivity of (Yb{sub 0.95}Ca{sub 0.05}){sub 2}Ti{sub 2}O{sub 7} synthesized at temperatures of 1300, 1400, and 1500 deg. C are studied using impedance spectroscopy. It is found that the (Yb{sub 0.95}Ca{sub 0.05}){sub 2}Ti{sub 2}O{sub 7} sample synthesized at 1500 deg. C has the highest total conductivity due to the increased grain-boundary component. The bulk component of the ionic conductivity of (Yb{sub 0.95}Ca{sub 0.05}){sub 2}Ti{sub 2}O{sub 7} is hardly affected by the synthesis temperature and depends mainly on the degree of heterovalent substitution.

  12. Ceramic oxide powders and the formation thereof

    DOE Patents [OSTI]

    Katz, Joseph L.; Hung, Cheng-Hung

    1993-01-01

    Ceramic oxide powders and a method for their preparation. Ceramic oxide powders are obtained using a flame process whereby two or more precursors of ceramic oxides are introduced into a counterflow diffusion flame burner wherein said precursors are converted into ceramic oxide powders. The morphology, particle size, and crystalline form of the ceramic oxide powders are determined by process conditions.

  13. Ceramic oxide powders and the formation thereof

    DOE Patents [OSTI]

    Katz, J.L.; Chenghung Hung.

    1993-12-07

    Ceramic oxide powders and a method for their preparation. Ceramic oxide powders are obtained using a flame process whereby two or more precursors of ceramic oxides are introduced into a counterflow diffusion flame burner wherein said precursors are converted into ceramic oxide powders. The morphology, particle size, and crystalline form of the ceramic oxide powders are determined by process conditions. 14 figures.

  14. NEUTRONIC REACTOR

    DOE Patents [OSTI]

    Hurwitz, H. Jr.; Brooks, H.; Mannal, C.; Payne, J.H.; Luebke, E.A.

    1959-03-24

    A reactor of the heterogeneous, liquid cooled type is described. This reactor is comprised of a central region of a plurality of vertically disposed elongated tubes surrounded by a region of moderator material. The central region is comprised of a central core surrounded by a reflector region which is surrounded by a fast neutron absorber region, which in turn is surrounded by a slow neutron absorber region. Liquid sodium is used as the primary coolant and circulates through the core which contains the fuel elements. Control of the reactor is accomplished by varying the ability of the reflector region to reflect neutrons back into the core of the reactor. For this purpose the reflector is comprised of moderator and control elements having varying effects on reactivity, the control elements being arranged and actuated by groups to give regulation, shim, and safety control.

  15. Neutron irradiation induced amorphization of silicon carbide

    SciTech Connect (OSTI)

    Snead, L.L.; Hay, J.C.

    1998-09-01

    This paper provides the first known observation of silicon carbide fully amorphized under neutron irradiation. Both high purity single crystal hcp and high purity, highly faulted (cubic) chemically vapor deposited (CVD) SiC were irradiated at approximately 60 C to a total fast neutron fluence of 2.6 {times} 10{sup 25} n/m{sup 2}. Amorphization was seen in both materials, as evidenced by TEM, electron diffraction, and x-ray diffraction techniques. Physical properties for the amorphized single crystal material are reported including large changes in density ({minus}10.8%), elastic modulus as measured using a nanoindentation technique ({minus}45%), hardness as measured by nanoindentation ({minus}45%), and standard Vickers hardness ({minus}24%). Similar property changes are observed for the critical temperature for amorphization at this neutron dose and flux, above which amorphization is not possible, is estimated to be greater than 130 C.

  16. Neutron absorbing room temperature vulcanizable silicone rubber compositions

    DOE Patents [OSTI]

    Zoch, Harold L.

    1979-11-27

    A neutron absorbing composition comprising a one-component room temperature vulcanizable silicone rubber composition or a two-component room temperature vulcanizable silicone rubber composition in which the composition contains from 25 to 300 parts by weight based on the base silanol or vinyl containing diorganopolysiloxane polymer of a boron compound or boron powder as the neutron absorbing ingredient. An especially useful boron compound in this application is boron carbide.

  17. NEUTRONIC REACTOR

    DOE Patents [OSTI]

    Fermi, E.; Szilard, L.

    1957-09-24

    Reactors of the type employing plates of natural uranium in a moderator are discussed wherein the plates are um-formly disposed in parallel relationship to each other thereby separating the moderator material into distinct and individual layers. Each plate has an uninterrupted sunface area substantially equal to the cross-sectional area of the active portion of the reactor, the particular size of the plates and the volume ratio of moderator to uranium required to sustain a chain reaction being determinable from the known purity of these materials and other characteristics such as the predictable neutron losses due to the formation of radioactive elements of extremely high neutron capture cross section.

  18. NEUTRONIC REACTOR

    DOE Patents [OSTI]

    Wigner, E.P.; Weinberg, A.W.; Young, G.J.

    1958-04-15

    A nuclear reactor which uses uranium in the form of elongated tubes as fuel elements and liquid as a coolant is described. Elongated tubular uranium bodies are vertically disposed in an efficient neutron slowing agent, such as graphite, for example, to form a lattice structure which is disposed between upper and lower coolant tanks. Fluid coolant tubes extend through the uranium bodies and communicate with the upper and lower tanks and serve to convey the coolant through the uranium body. The reactor is also provided with means for circulating the cooling fluid through the coolant tanks and coolant tubes, suitable neutron and gnmma ray shields, and control means.

  19. PROCESS OF FORMING POWDERED MATERIAL

    DOE Patents [OSTI]

    Glatter, J.; Schaner, B.E.

    1961-07-14

    A process of forming high-density compacts of a powdered ceramic material is described by agglomerating the powdered ceramic material with a heat- decompossble binder, adding a heat-decompossble lubricant to the agglomerated material, placing a quantity of the material into a die cavity, pressing the material to form a compact, pretreating the compacts in a nonoxidizing atmosphere to remove the binder and lubricant, and sintering the compacts. When this process is used for making nuclear reactor fuel elements, the ceramic material is an oxide powder of a fissionsble material and after forming, the compacts are placed in a cladding tube which is closed at its ends by vapor tight end caps, so that the sintered compacts are held in close contact with each other and with the interior wall of the cladding tube.

  20. Pressure-Induced Structural Phase Transition in CeNi: X-ray and Neutron Scattering Studies and First-Principles Calculations

    SciTech Connect (OSTI)

    Mirmelstein, A.; Podlesnyak, Andrey A.; dos Santos, Antonio M.; Ehlers, Georg; Kerbel, O.; Matvienko, V.; Sefat, A. S.; Saporov, B.; Halder, G. J.; Tobin, J. G.

    2015-08-03

    The pressure-induced structural phase transition in the intermediate-valence compound CeNi has been investigated by x-ray and neutron powder diffraction techniques. It is shown that the structure of the pressure-induced CeNi phase (phases) can be described in terms of the Pnma space group. Equations of state for CeNi on both sides of the phase transition are derived and an approximate P-T phase diagram is suggested for P<8 GPa and T<300 K. The observed Cmcm→Pnma structural transition is then analyzed using density functional theory calculations, which successfully reproduce the ground state volume, the phase transition pressure, and the volume collapse associated with the phase transition.

  1. Pressure-Induced Structural Phase Transition in CeNi: X-ray and Neutron Scattering Studies and First-Principles Calculations

    DOE Public Access Gateway for Energy & Science Beta (PAGES Beta)

    Mirmelstein, A.; Podlesnyak, Andrey A.; dos Santos, Antonio M.; Ehlers, Georg; Kerbel, O.; Matvienko, V.; Sefat, A. S.; Saporov, B.; Halder, G. J.; Tobin, J. G.

    2015-08-03

    The pressure-induced structural phase transition in the intermediate-valence compound CeNi has been investigated by x-ray and neutron powder diffraction techniques. It is shown that the structure of the pressure-induced CeNi phase (phases) can be described in terms of the Pnma space group. Equations of state for CeNi on both sides of the phase transition are derived and an approximate P-T phase diagram is suggested for P<8 GPa and T<300 K. The observed Cmcm→Pnma structural transition is then analyzed using density functional theory calculations, which successfully reproduce the ground state volume, the phase transition pressure, and the volume collapse associated withmore » the phase transition.« less

  2. NEUTRONIC REACTORS

    DOE Patents [OSTI]

    Anderson, H.L.

    1958-10-01

    The design of control rods for nuclear reactors are described. In this design the control rod consists essentially of an elongated member constructed in part of a neutron absorbing material and having tube means extending therethrough for conducting a liquid to cool the rod when in use.

  3. Neutronic reactor

    DOE Patents [OSTI]

    Carleton, John T.

    1977-01-25

    A graphite-moderated nuclear reactor includes channels between blocks of graphite and also includes spacer blocks between adjacent channeled blocks with an axis of extension normal to that of the axis of elongation of the channeled blocks to minimize changes in the physical properties of the graphite as a result of prolonged neutron bombardment.

  4. Electrically-programmable diffraction grating

    DOE Patents [OSTI]

    Ricco, A.J.; Butler, M.A.; Sinclair, M.B.; Senturia, S.D.

    1998-05-26

    An electrically-programmable diffraction grating is disclosed. The programmable grating includes a substrate having a plurality of electrodes formed thereon and a moveable grating element above each of the electrodes. The grating elements are electrostatically programmable to form a diffraction grating for diffracting an incident beam of light as it is reflected from the upper surfaces of the grating elements. The programmable diffraction grating, formed by a micromachining process, has applications for optical information processing (e.g. optical correlators and computers), for multiplexing and demultiplexing a plurality of light beams of different wavelengths (e.g. for optical fiber communications), and for forming spectrometers (e.g. correlation and scanning spectrometers). 14 figs.

  5. Methods for absorbing neutrons

    DOE Patents [OSTI]

    Guillen, Donna P.; Longhurst, Glen R.; Porter, Douglas L.; Parry, James R.

    2012-07-24

    A conduction cooled neutron absorber may include a metal matrix composite that comprises a metal having a thermal neutron cross-section of at least about 50 barns and a metal having a thermal conductivity of at least about 1 W/cmK. Apparatus for providing a neutron flux having a high fast-to-thermal neutron ratio may include a source of neutrons that produces fast neutrons and thermal neutrons. A neutron absorber positioned adjacent the neutron source absorbs at least some of the thermal neutrons so that a region adjacent the neutron absorber has a fast-to-thermal neutron ratio of at least about 15. A coolant in thermal contact with the neutron absorber removes heat from the neutron absorber.

  6. Neutron reflecting supermirror structure

    DOE Patents [OSTI]

    Wood, James L.

    1992-01-01

    An improved neutron reflecting supermirror structure comprising a plurality of stacked sets of bilayers of neutron reflecting materials. The improved neutron reflecting supermirror structure is adapted to provide extremely good performance at high incidence angles, i.e. up to four time the critical angle of standard neutron mirror structures. The reflection of neutrons striking the supermirror structure at a high critical angle provides enhanced neutron throughput, and hence more efficient and economical use of neutron sources.

  7. Neutron reflecting supermirror structure

    DOE Patents [OSTI]

    Wood, J.L.

    1992-12-01

    An improved neutron reflecting supermirror structure comprising a plurality of stacked sets of bilayers of neutron reflecting materials. The improved neutron reflecting supermirror structure is adapted to provide extremely good performance at high incidence angles, i.e. up to four time the critical angle of standard neutron mirror structures. The reflection of neutrons striking the supermirror structure at a high critical angle provides enhanced neutron throughput, and hence more efficient and economical use of neutron sources. 2 figs.

  8. Polymer quenched prealloyed metal powder

    DOE Patents [OSTI]

    Hajaligol, Mohammad R.; Fleischhauer, Grier; German, Randall M.

    2001-01-01

    A powder metallurgical process of preparing a sheet from a powder having an intermetallic alloy composition such as an iron, nickel or titanium aluminide. The sheet can be manufactured into electrical resistance heating elements having improved room temperature ductility, electrical resistivity, cyclic fatigue resistance, high temperature oxidation resistance, low and high temperature strength, and/or resistance to high temperature sagging. The iron aluminide has an entirely ferritic microstructure which is free of austenite and can include, in weight %, 4 to 32% Al, and optional additions such as .ltoreq.1% Cr, .gtoreq.0.05% Zr .ltoreq.2% Ti, .ltoreq.2% Mo, .ltoreq.1% Ni, .ltoreq.0.75% C, .ltoreq.0.1% B, .ltoreq.1% submicron oxide particles and/or electrically insulating or electrically conductive covalent ceramic particles, .ltoreq.1% rare earth metal, and/or .ltoreq.3 % Cu. The process includes forming a non-densified metal sheet by consolidating a powder having an intermetallic alloy composition such as by roll compaction, tape casting or plasma spraying, forming a cold rolled sheet by cold rolling the non-densified metal sheet so as to increase the density and reduce the thickness thereof and annealing the cold rolled sheet. The powder can be a water, polymer or gas atomized powder which is subjecting to sieving and/or blending with a binder prior to the consolidation step. After the consolidation step, the sheet can be partially sintered. The cold rolling and/or annealing steps can be repeated to achieve the desired sheet thickness and properties. The annealing can be carried out in a vacuum furnace with a vacuum or inert atmosphere. During final annealing, the cold rolled sheet recrystallizes to an average grain size of about 10 to 30 .mu.m. Final stress relief annealing can be carried out in the B2 phase temperature range.

  9. NEUTRONIC REACTORS

    DOE Patents [OSTI]

    Vernon, H.C.

    1959-01-13

    A neutronic reactor of the heterogeneous, fluid cooled tvpe is described. The reactor is comprised of a pressure vessel containing the moderator and a plurality of vertically disposed channels extending in spaced relationship through the moderator. Fissionable fuel material is placed within the channels in spaced relationship thereto to permit circulation of the coolant fluid. Separate means are provided for cooling the moderator and for circulating a fluid coolant thru the channel elements to cool the fuel material.

  10. X-ray diffraction study of crystalline barium titanate ceramics

    SciTech Connect (OSTI)

    Zali, Nurazila Mat; Mahmood, Che Seman; Mohamad, Siti Mariam; Foo, Choo Thye; Murshidi, Julie Adrianny

    2014-02-12

    In this study, BaTiO{sub 3} ceramics have been prepared via solid-state reaction method. The powders were calcined for 2 hours at different temperatures ranging from 600C to 1200C. Using X-ray diffraction with a Rietveld analysis, the phase formation and crystal structure of the BaTiO{sub 3} powders were studied. Change in crystallite size and tetragonality as a function of calcination temperature were also discussed. It has been found that the formation of pure perovskite phase of BaTiO{sub 3} began at calcination condition of 1000 C for 2 hours. The crystal structure of BaTiO{sub 3} formed is in the tetragonal structure. The second phases of BaCO{sub 3} and TiO{sub 2} existed with calcination temperature below 1000 C. Purity, crystallite size and tetragonality of BaTiO{sub 3} powders were found to increase with increasing calcination temperature.