Chlorine-free, monolithic lanthanide series rare earth oxide aerogels via epoxide-assisted sol-gel method

Worsley, M. A.; Ilsemann, J.; Gesing, Th. M.; Zielasek, V.; Nelson, A. J.; Ferreira, R. A.  S.; Carlos, L. D.; Gash, A. E.; Bäumer, M.

doi:10.1007/s10971-018-4811-y

Title: Chlorine-free, monolithic lanthanide series rare earth oxide aerogels via epoxide-assisted sol-gel method

Abstract

Synthesis of chlorine-free, rare earth oxide aerogels from the lanthanide series was achieved using a modified epoxide-assisted sol-gel method. An ethanolic solution of the hydrated metal nitrate, propylene oxide, and ammonium carbonate was found to gel upon heating to 333 K. Critical point drying of the wet gel in CO₂ yielded monolithic aerogels. Most of the aerogels were amorphous as-prepared, but became nano-crystalline after calcination at 923 K in air. The aerogels had high surface areas (up to 150 m²/g), low densities (40–225 mg/cm³), and were photoluminescent.

Authors:

Worsley, M. A. ^[1]; Ilsemann, J. ^[2]; Gesing, Th. M. ^[2]; Zielasek, V. ^[2]; Nelson, A. J. ^[1]; Ferreira, R. A. S. ^[3]; Carlos, L. D. ^[3]; Gash, A. E. ^[1]; Bäumer, M. ^[2]

Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States)
Univ. of Bremen (Germany)
Univ. of Aveiro (Portugal)

Publication Date:: Fri Sep 14 00:00:00 EDT 2018

Research Org.:: Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States)

Sponsoring Org.:: USDOE National Nuclear Security Administration (NNSA); German Science Foundation (DFG); Fraunhofer Institute for Manufacturing Technology and Advanced Materials

OSTI Identifier:: 1548325

Report Number(s):: LLNL-JRNL-782169
Journal ID: ISSN 0928-0707; 976425

Grant/Contract Number:: AC52-07NA27344

Resource Type:: Accepted Manuscript

Journal Name:: Journal of Sol-Gel Science and Technology

Additional Journal Information:: Journal Volume: 89; Journal Issue: 1; Journal ID: ISSN 0928-0707

Publisher:: Springer

Country of Publication:: United States

Language:: English

Subject:: 77 NANOSCIENCE AND NANOTECHNOLOGY; 36 MATERIALS SCIENCE; rare earth oxide; aerogel; sol-gel; monolith; catalyst; photoluminescence; Rietveld refinement

Citation Formats


                    Worsley, M. A., Ilsemann, J., Gesing, Th. M., Zielasek, V., Nelson, A. J., Ferreira, R. A.  S., Carlos, L. D., Gash, A. E., and Bäumer, M. Chlorine-free, monolithic lanthanide series rare earth oxide aerogels via epoxide-assisted sol-gel method.  United States: N. p., 2018. 
Web.  doi:10.1007/s10971-018-4811-y.

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                    Worsley, M. A., Ilsemann, J., Gesing, Th. M., Zielasek, V., Nelson, A. J., Ferreira, R. A.  S., Carlos, L. D., Gash, A. E., & Bäumer, M. Chlorine-free, monolithic lanthanide series rare earth oxide aerogels via epoxide-assisted sol-gel method.  United States.  https://doi.org/10.1007/s10971-018-4811-y

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                    Worsley, M. A., Ilsemann, J., Gesing, Th. M., Zielasek, V., Nelson, A. J., Ferreira, R. A.  S., Carlos, L. D., Gash, A. E., and Bäumer, M. Fri .  
"Chlorine-free, monolithic lanthanide series rare earth oxide aerogels via epoxide-assisted sol-gel method".  United States.  https://doi.org/10.1007/s10971-018-4811-y.  https://www.osti.gov/servlets/purl/1548325.

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@article{osti_1548325,

  title        = {Chlorine-free, monolithic lanthanide series rare earth oxide aerogels via epoxide-assisted sol-gel method},

  author       = {Worsley, M. A. and Ilsemann, J. and Gesing, Th. M. and Zielasek, V. and Nelson, A. J. and Ferreira, R. A.  S. and Carlos, L. D. and Gash, A. E. and Bäumer, M.},

  abstractNote = {Synthesis of chlorine-free, rare earth oxide aerogels from the lanthanide series was achieved using a modified epoxide-assisted sol-gel method. An ethanolic solution of the hydrated metal nitrate, propylene oxide, and ammonium carbonate was found to gel upon heating to 333 K. Critical point drying of the wet gel in CO2 yielded monolithic aerogels. Most of the aerogels were amorphous as-prepared, but became nano-crystalline after calcination at 923 K in air. The aerogels had high surface areas (up to 150 m2/g), low densities (40–225 mg/cm3), and were photoluminescent.},

  doi          = {10.1007/s10971-018-4811-y},

  journal      = {Journal of Sol-Gel Science and Technology},

  number       = 1,

  volume       = 89,

  place        = {United States},

  year         = {Fri Sep 14 00:00:00 EDT 2018},

  month        = {Fri Sep 14 00:00:00 EDT 2018}

}

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journal, June 1969

Singh, H. P.; Dayal, B.
Journal of the Less Common Metals, Vol. 18, Issue 2
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On the phase interval PrO1.50 to PrO1.71 in the praseodymium oxide-oxygen system
journal, May 1971

Turcotte, Rhéal P.; Warmkessel, Joyce M.; Tilley, Richard J. D.
Journal of Solid State Chemistry, Vol. 3, Issue 2
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Synthesis and characterization of spherical and rod like nanocrystalline Nd2O3 phosphors
journal, January 2011

Umesh, B.; Eraiah, B.; Nagabhushana, H.
Journal of Alloys and Compounds, Vol. 509, Issue 4
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Structural and oxide ion conductivity studies on Yb1−xBixO1.5 (0.00⩽x⩽0.50) composites
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Vasundhara, K.; Achary, S. N.; Patwe, S. J.
Journal of Alloys and Compounds, Vol. 596
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Core and shell structure of ytterbium sesquioxide nanoparticles
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Vucinic-Vasic, Milica; Kremenovic, Aleksandar; Nikolic, Aleksandar S.
Journal of Alloys and Compounds, Vol. 502, Issue 1
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Ytterbium L _III -edge anomalous scattering measured with synchrotron radiation powder diffraction
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Will, G.; Masciocchi, N.; Hart, M.
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Eine Notiz zum A-Typ der Lanthanoidoxide: �ber Pr2O3
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Wolf, H. C. R.; Hoppe, R.
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Single Crystals of B-Type Er ₂ O ₃
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Wontcheu, Joseph; Schleid, Thomas
Zeitschrift für anorganische und allgemeine Chemie, Vol. 634, Issue 11
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A refinement of the crystal structure of monoclinic europium sesquioxide
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Yakel, H. L.
Acta Crystallographica Section B Structural Crystallography and Crystal Chemistry, Vol. 35, Issue 3
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Structural phase transitions of cubic ${Gd}_{2} O_{3}$ at high pressures
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Zhang, F. X.; Lang, M.; Wang, J. W.
Physical Review B, Vol. 78, Issue 6
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Er ³⁺ -Based Diureasil Organic−Inorganic Hybrids
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Molina, C.; Ferreira, R. A. S.; Poirier, G.
The Journal of Physical Chemistry C, Vol. 112, Issue 49
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Synthesis, characterization and optical studies on lanthanide-doped CdS quantum dots: new insights on CdS → lanthanide energy transfer mechanisms
journal, January 2011

Planelles-Aragó, José; Cordoncillo, Eloisa; Ferreira, Rute A. S.
J. Mater. Chem., Vol. 21, Issue 4
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Spectral study of the stimulated emission of Nd^3+ in fluorotellurite bulk glass
journal, January 2013

Miguel, A.; Azkargorta, J.; Morea, R.
Optics Express, Vol. 21, Issue 8
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Abstract

Citation Formats

Catalysis by Doped Oxides journal, December 2012

Rare Earth Oxide Coating of the Walls of SBA-15 journal, January 2002

Low-Temperature Destruction of Chlorinated Hydrocarbons over Lanthanide Oxide Based Catalysts journal, December 2002

Nanostructured Praseodymium Oxide: Preparation, Structure, and Catalytic Properties journal, February 2008

Structural Characteristics and Catalytic Activity of Nanocrystalline Ceria−Praseodymia Solid Solutions journal, August 2009

Synthesis and characterization of monolithic Gd2O3 aerogels journal, September 2008

A new route to three-dimensionally well-ordered macroporous rare-earth oxides journal, January 2001

Synthesis of lanthanide and lanthanide-silicate aerogels journal, January 1994

A sol–gel methodology for the preparation of lanthanide-oxide aerogels: preparation and characterization journal, August 2012

Influence of chlorine poisoning of copper/alumina catalyst on the selective hydrogenation of crotonaldehyde journal, March 1994

Chlorine-Containing compounds as copper catalyst poisons journal, September 1982

Chlorine–nickel interactions in gas phase catalytic hydrodechlorination: catalyst deactivation and the nature of reactive hydrogen journal, January 1999

Use of Epoxides in the Sol−Gel Synthesis of Porous Iron(III) Oxide Monoliths from Fe(III) Salts journal, March 2001

Strong Akaganeite Aerogel Monoliths Using Epoxides: Synthesis and Characterization journal, August 2003

Synthesis of High-Surface-Area Alumina Aerogels without the Use of Alkoxide Precursors journal, January 2005

Synthesis of high porosity, monolithic alumina aerogels journal, June 2001

Structural and spectroscopic comparison between polycrystalline, nanocrystalline and quantum dot visible light photo-catalyst Bi 2 WO 6 journal, October 2017

Etude par diffraction neutronique des structures de haute temperature de La2O3 et Nd2O3 journal, March 1979

Structure properties and magnetic susceptibility of diluted magnetic semiconductor Y2−xHoxO3 journal, March 1995

The structure characteristics of the diluted magnetic semiconductor Y 2−x Dy x O 3 journal, December 1993

Structural study of Nd oxidation by means of in-situ synchrotron X-ray diffraction (400≤T≤700°C) journal, April 2014

Shock-induced phase transition of M2O3 (M = Sc, Y, Sm, Gd, and In)-type compounds journal, December 1990

Reversible B-type - A-type transition of Sm2O3 under high pressure journal, September 1989

Refinement of atomic positions in bixbyite oxides using perturbed angular correlation spectroscopy journal, April 1993

Structural and vibrational study of C-type doped rare earth sesquioxide Yb2−xCoxO3 journal, June 2009

Synthesis, structure and magnetic properties of the Lu2O3–CoO mixed system journal, October 2010

Ordered intermediate phases in the system CeO2Ce2O3 journal, March 1955

Crystal growth of ytterbium dihydride and the phase relations in the Yb-H system journal, October 1983

The crystal structure refinement and magnetic susceptibility study of La2−xErxO3 journal, July 2003

An X-ray diffraction and magnetic susceptibility study of TmxY2−xO3 journal, April 2000

Die Gitterkonstanten der C-Formen der Oxyde der seltenen Erdmetalle journal, May 1939

Refinement of the Nd 2 O 3 structure and determination of the neutron scattering length of neodymium journal, November 1975

Etude de couches minces de sesquioxyde de samarium type B par microscopie et diffraction électroniques journal, January 1971

Comparison of structural and luminescence properties of Dy2O3 nanopowders synthesized by co-precipitation and green combustion routes journal, July 2014

Structural and phase dependent thermo and photoluminescent properties of Dy(OH)3 and Dy2O3 nanorods journal, August 2012

An Energy-Dispersive X-Ray Diffraction Study of Monoclinic Eu2O3 under Pressure journal, August 1994

Polymorphic Modifications of Pm2O3 journal, August 1972

The Crystal Structure of Monoclinic Sm 2 0 2 journal, June 1957

Comparative structural and photoluminescent study of Eu3+-doped La2O3 and La(OH)3 nanocrystalline powders journal, February 2014

Refinement of the Nd 2 O 3 and Nd 2 O 2 S structures at 4 K journal, January 1982

A new form of La2O3 journal, April 1969

The formation of rare earth oxides far from equilibrium journal, February 1986

Raman spectra of lanthanide sesquioxide single crystals: Correlation between A and B-type structures journal, July 1981

The crystal structure of the low-temperature A-type modification of Pr2O3 from X-ray powder and electron single crystal diffraction journal, January 1995

Thermal Expansion of CeO2, Ho2O3, and Lu2O3 from 100o to 300oK by an X-Ray Method journal, December 1970

Structural Investigations of Lu 2 O 3 as Single Crystal and Polycrystalline Transparent Ceramic journal, May 2014

Neutronographische Bestimmung der Kristallstrukturparameter von Dy2O3, Tm2O3 und α -Mn2O3 journal, January 1963

X-ray structure determination of the rare earth oxides (Er 1− u Gd u ) 2 O 3 applying the Rietveld method journal, September 2002

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R�ntgenographische Untersuchung an Einkristallen von monoklinem Tb2O3 journal, December 1968

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Crystal structure of monoclinic samarium and cubic europium sesquioxides and bound coherent neutron scattering lengths of the isotopes 154Sm and 153Eu journal, January 2016

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Elaboration et proprietes magnetiques de monocristaux d'oxyde de praseodyme Pr2O3 journal, January 1976

A synchrotron X-ray study of the electron density in C-type rare earth oxides journal, June 1996

Crystal data on C -type terbium sesquioxide (Tb 2 O 3 ) journal, October 1971

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Rapid and Energy-Saving Microwave-Assisted Solid-State Synthesis of Pr 3+ -, Eu 3+ -, or Tb 3+ -Doped Lu 2 O 3 Persistent Luminescence Materials journal, July 2016

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Structural Change of C-Rare Earth Sesquioxides Yb2O3 and Er2O3 as a Function of Temperature [C型希土類酸化物Yb2O3及びEr2O3の高温構造変化] journal, January 1985

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journal, December 2012

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journal, January 2002

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journal, January 1994

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Influence of chlorine poisoning of copper/alumina catalyst on the selective hydrogenation of crotonaldehyde
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Chlorine-Containing compounds as copper catalyst poisons
journal, September 1982

Chlorine–nickel interactions in gas phase catalytic hydrodechlorination: catalyst deactivation and the nature of reactive hydrogen
journal, January 1999

Use of Epoxides in the Sol−Gel Synthesis of Porous Iron(III) Oxide Monoliths from Fe(III) Salts
journal, March 2001

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journal, August 2003

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journal, January 2005

Synthesis of high porosity, monolithic alumina aerogels
journal, June 2001

Structural and spectroscopic comparison between polycrystalline, nanocrystalline and quantum dot visible light photo-catalyst Bi 2 WO 6
journal, October 2017

Etude par diffraction neutronique des structures de haute temperature de La2O3 et Nd2O3
journal, March 1979

Structure properties and magnetic susceptibility of diluted magnetic semiconductor Y2−xHoxO3
journal, March 1995

The structure characteristics of the diluted magnetic semiconductor Y _2−x Dy _x O ₃
journal, December 1993

Structural study of Nd oxidation by means of in-situ synchrotron X-ray diffraction (400≤T≤700°C)
journal, April 2014

Shock-induced phase transition of M2O3 (M = Sc, Y, Sm, Gd, and In)-type compounds
journal, December 1990

Reversible B-type - A-type transition of Sm2O3 under high pressure
journal, September 1989

Refinement of atomic positions in bixbyite oxides using perturbed angular correlation spectroscopy
journal, April 1993

Structural and vibrational study of C-type doped rare earth sesquioxide Yb2−xCoxO3
journal, June 2009

Synthesis, structure and magnetic properties of the Lu2O3–CoO mixed system
journal, October 2010

Ordered intermediate phases in the system CeO2Ce2O3
journal, March 1955

Crystal growth of ytterbium dihydride and the phase relations in the Yb-H system
journal, October 1983

The crystal structure refinement and magnetic susceptibility study of La2−xErxO3
journal, July 2003

An X-ray diffraction and magnetic susceptibility study of TmxY2−xO3
journal, April 2000

Die Gitterkonstanten der C-Formen der Oxyde der seltenen Erdmetalle
journal, May 1939

Refinement of the Nd ₂ O ₃ structure and determination of the neutron scattering length of neodymium
journal, November 1975

Etude de couches minces de sesquioxyde de samarium type B par microscopie et diffraction électroniques
journal, January 1971

Comparison of structural and luminescence properties of Dy2O3 nanopowders synthesized by co-precipitation and green combustion routes
journal, July 2014

Structural and phase dependent thermo and photoluminescent properties of Dy(OH)3 and Dy2O3 nanorods
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journal, August 1994

Polymorphic Modifications of Pm2O3
journal, August 1972

The Crystal Structure of Monoclinic Sm ₂ 0 ₂
journal, June 1957

Comparative structural and photoluminescent study of Eu3+-doped La2O3 and La(OH)3 nanocrystalline powders
journal, February 2014

Refinement of the Nd ₂ O ₃ and Nd ₂ O ₂ S structures at 4 K
journal, January 1982

A new form of La2O3
journal, April 1969

The formation of rare earth oxides far from equilibrium
journal, February 1986

Raman spectra of lanthanide sesquioxide single crystals: Correlation between A and B-type structures
journal, July 1981

The crystal structure of the low-temperature A-type modification of Pr2O3 from X-ray powder and electron single crystal diffraction
journal, January 1995

Thermal Expansion of CeO2, Ho2O3, and Lu2O3 from 100o to 300oK by an X-Ray Method
journal, December 1970

Structural Investigations of Lu ₂ O ₃ as Single Crystal and Polycrystalline Transparent Ceramic
journal, May 2014

Neutronographische Bestimmung der Kristallstrukturparameter von Dy2O3, Tm2O3 und α -Mn2O3
journal, January 1963

X-ray structure determination of the rare earth oxides (Er _{1− u} Gd _u ) ₂ O ₃ applying the Rietveld method
journal, September 2002

X-ray structure and microstructure determination of the mixed sesquioxides (Eu _{1− x} Yb _x ) ₂ O ₃ prepared by a sol–gel process
journal, November 2003

X-ray diffraction analysis of powder and thin film of (Gd1-xYx)2O3 prepared by sol-gel process
journal, March 2008

Structure and microstructure characterization of the mixed sesquioxides (Gd _{1− x} Yb _x ) ₂ O ₃ and (Gd _{1− x} Ho _x ) ₂ O ₃ prepared by sol–gel process
journal, March 2005

XRD, IR, and Raman investigations of structural properties of Dy2-xHox O3 prepared by sol gel procedure
journal, March 2012

High-pressure Syntheses and Crystal Structures of Monoclinic B-Ho2O3 and Orthorhombic HoGaO3
journal, September 2009

R�ntgenographische Untersuchung an Einkristallen von monoklinem Tb2O3
journal, December 1968

Electron density distribution and chemical bonding of Ln2O3 (Ln = Y, Tm, Yb) from powder X-ray diffraction data by the maximum-entropy method
journal, September 1994

Effect of Annealing Environment on Low-Temperature Magnetic and Dielectric Properties of EuCo _0.5 Mn _0.5 O ₃
journal, July 2014

The Structure of C-type Gd2O3. A Powder Neutron Diffraction Study using Enriched 160Gd
journal, January 2011

The structure of B-type Sm2O3. A powder neutron diffraction study using enriched 154Sm
journal, September 2011

Neutron-diffraction study of the structure of the A-form of the rare earth sesquioxides
journal, September 1953

Paramagnetic and Nuclear Scattering Cross Sections of Holmium Sesquioxide
journal, April 1958

Crystal structure of monoclinic samarium and cubic europium sesquioxides and bound coherent neutron scattering lengths of the isotopes 154Sm and 153Eu
journal, January 2016

Structural and spectroscopic studies of Eu3+ doped Lu2O3–Gd2O3 solid solutions
journal, April 2014

Elaboration et proprietes magnetiques de monocristaux d'oxyde de praseodyme Pr2O3
journal, January 1976

A synchrotron X-ray study of the electron density in C-type rare earth oxides
journal, June 1996

Crystal data on C -type terbium sesquioxide (Tb ₂ O ₃ )
journal, October 1971

Magnetic properties of trivalent Sm ions in SmxY2−xO3
journal, October 2009

Magnetic Structures of ${Er}_{2}$ $O_{3}$ and ${Yb}_{2}$ $O_{3}$
journal, December 1968

Zur Struktur der A-Form der Sesquioxide der Seltenen Erden. II. Strukturuntersuchung an Nd2O3
journal, February 1966

Zur Struktur der A-Form der Sesquioxide der Seltenen Erden. Strukturuntersuchungen an La2O3
journal, November 1965

Rapid and Energy-Saving Microwave-Assisted Solid-State Synthesis of Pr ³⁺ -, Eu ³⁺ -, or Tb ³⁺ -Doped Lu ₂ O ₃ Persistent Luminescence Materials
journal, July 2016

New X-ray powder diffraction data and Rietveld refinement for Gd 2 O 3 monodispersed fine spherical particles
journal, February 2003

The observation of face centred cubic Gd, Tb, Dy, Ho, Er and Tm in the form of thin films and their oxidation
journal, January 1973

Structural Change of C-Rare Earth Sesquioxides Yb2O3 and Er2O3 as a Function of Temperature [C型希土類酸化物Yb₂O₃及びEr₂O₃の高温構造変化]
journal, January 1985

Probing Complex Disorder in Ce _{1- x} Gd _x O _{2- x /2} Using the Pair Distribution Function Analysis
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Crystal Structure and Phase Transitions of Gd(CO ₃ )OH Studied by Synchrotron Powder Diffraction
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Precise determination of the lattice parameters of holmium and erbium sesquioxides at elevated temperatures
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On the phase interval PrO1.50 to PrO1.71 in the praseodymium oxide-oxygen system
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Synthesis and characterization of spherical and rod like nanocrystalline Nd2O3 phosphors
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Structural and oxide ion conductivity studies on Yb1−xBixO1.5 (0.00⩽x⩽0.50) composites
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