Correlative Energy-Dispersive X-Ray Spectroscopic Tomography and Atom Probe Tomography of the Phase Separation in an Alnico 8 Alloy

Guo, Wei; Sneed, Brian T.; Zhou, Lin; Tang, Wei; Kramer, Matthew J.; Cullen, David A.; Poplawsky, Jonathan D.

doi:10.1017/S1431927616012496

Title: Correlative Energy-Dispersive X-Ray Spectroscopic Tomography and Atom Probe Tomography of the Phase Separation in an Alnico 8 Alloy

Journal Article · Wed Dec 21 00:00:00 EST 2016 · Microscopy and Microanalysis

DOI:https://doi.org/10.1017/S1431927616012496· OSTI ID:1394424

Guo, Wei ^[1]; Sneed, Brian T. ^[1]; Zhou, Lin ^[2]; Tang, Wei ^[2]; Kramer, Matthew J. ^[2]; Cullen, David A. ^[1]; Poplawsky, Jonathan D. ^[1]

Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)
Ames Lab., Ames, IA (United States)

Alnico alloys have long been used as strong permanent magnets because of their ferromagnetism and high coercivity. Understanding their structural details allows for better prediction of the resulting magnetic properties. However, quantitative three-dimensional characterization of the phase separation in these alloys is still challenged by the spatial quantification of nanoscale phases. Herein, we apply a dual tomography approach, where correlative scanning transmission electron microscopy (STEM) energy-dispersive X-ray spectroscopic (EDS) tomography and atom probe tomography (APT) are used to investigate the initial phase separation process of an alnico 8 alloy upon non-magnetic annealing. STEM-EDS tomography provides information on the morphology and volume fractions of Fe–Co-rich and Νi–Al-rich phases after spinodal decomposition in addition to quantitative information of the composition of a nanoscale volume. Subsequent analysis of a portion of the same specimen by APT offers quantitative chemical information of each phase at the sub-nanometer scale. Furthermore, APT reveals small, 2–4 nm Fe-rich α₁ phases that are nucleated in the Ni-rich α₂ matrix. From this information, we show that phase separation of the alnico 8 alloy consists of both spinodal decomposition and nucleation and growth processes. Lastly, we discuss the complementary benefits and challenges associated with correlative STEM-EDS and APT.

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Research Organization:: Oak Ridge National Laboratory (ORNL), Oak Ridge, TN (United States); Ames Laboratory (AMES), Ames, IA (United States)

Sponsoring Organization:: USDOE Office of Science (SC)

Grant/Contract Number:: AC05-00OR22725; AC02-07CH11358

OSTI ID:: 1394424

Alternate ID(s):: OSTI ID: 1342944

Report Number(s):: IS-J-9002; applab

Journal Information:: Microscopy and Microanalysis, Vol. 22, Issue 06; ISSN 1431-9276

Publisher:: Microscopy Society of America (MSA)Copyright Statement

Country of Publication:: United States

Language:: English

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Cited by: 24 works

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References (38)

Atomic scale study of CU clustering and pseudo-homogeneous Fe–Si nanocrystallization in soft magnetic FeSiNbB(CU) alloys Pradeep, K. G.; Herzer, G.; Raabe, D. Ultramicroscopy, Vol. 159 https://doi.org/10.1016/j.ultramic.2015.04.006	journal	December 2015
STEM tomography for thick biological specimens Aoyama, Kazuhiro; Takagi, Tomoko; Hirase, Ai Ultramicroscopy, Vol. 109, Issue 1 https://doi.org/10.1016/j.ultramic.2008.08.005	journal	December 2008
Crystallographic structural analysis in atom probe microscopy via 3D Hough transformation Yao, L.; Moody, M. P.; Cairney, J. M. Ultramicroscopy, Vol. 111, Issue 6 https://doi.org/10.1016/j.ultramic.2010.11.018	journal	May 2011
Enhanced Detection Sensitivity with a New Windowless XEDS System for AEM Based on Silicon Drift Detector Technology Schlossmacher, P.; Klenov, D. O.; Freitag, B. Microscopy Today, Vol. 18, Issue 4 https://doi.org/10.1017/s1551929510000404	journal	July 2010
Early-stage nucleation of manganese sulfide particle and its processing evolution in Fe—3wt.%Si alloys Guo, Wei; Meng, Li; Wang, Hongcai Frontiers of Materials Science, Vol. 10, Issue 1 https://doi.org/10.1007/s11706-016-0325-0	journal	December 2015
Correlative Tomography Burnett, T. L.; McDonald, S. A.; Gholinia, A. Scientific Reports, Vol. 4, Issue 1 https://doi.org/10.1038/srep04711	journal	April 2014
The quantitative analysis of thin specimens: a review of progress from the Cliff-Lorimer to the new zeta-factor methods Watanabe, M.; Williams, D. B. Journal of Microscopy, Vol. 221, Issue 2 https://doi.org/10.1111/j.1365-2818.2006.01549.x	journal	February 2006
An atom probe perspective on phase separation and precipitation in duplex stainless steels Guo, Wei; Garfinkel, David A.; Tucker, Julie D. Nanotechnology, Vol. 27, Issue 25 https://doi.org/10.1088/0957-4484/27/25/254004	journal	May 2016
Evolution of Fe–Co rich particles in Alnico 8 alloy thermomagnetically treated at 800°C Chu, W. G.; Fei, W. D.; Li, X. H. Materials Science and Technology, Vol. 16, Issue 9 https://doi.org/10.1179/026708300101508810	journal	September 2000
Phase separation in metallic glasses Kim, D. H.; Kim, W. T.; Park, E. S. Progress in Materials Science, Vol. 58, Issue 8 https://doi.org/10.1016/j.pmatsci.2013.04.002	journal	October 2013
Electron tomography and holography in materials science Midgley, Paul A.; Dunin-Borkowski, Rafal E. Nature Materials, Vol. 8, Issue 4 https://doi.org/10.1038/nmat2406	journal	April 2009
BoneJ: Free and extensible bone image analysis in ImageJ Doube, Michael; Kłosowski, Michał M.; Arganda-Carreras, Ignacio Bone, Vol. 47, Issue 6 https://doi.org/10.1016/j.bone.2010.08.023	journal	December 2010
A numerical model for multiple detector energy dispersive X-ray spectroscopy in the transmission electron microscope Xu, W.; Dycus, J. H.; Sang, X. Ultramicroscopy, Vol. 164 https://doi.org/10.1016/j.ultramic.2016.02.004	journal	May 2016
Monitoring Galvanic Replacement Through Three-Dimensional Morphological and Chemical Mapping Goris, Bart; Polavarapu, Lakshminarayana; Bals, Sara Nano Letters, Vol. 14, Issue 6 https://doi.org/10.1021/nl500593j	journal	May 2014
Performance of a local electrode atom probe Miller, M. K.; Russell, K. F. Surface and Interface Analysis, Vol. 39, Issue 2-3 https://doi.org/10.1002/sia.2488	journal	January 2007
Microstructural Characterization of an Al-Li-Mg-Cu Alloy by Correlative Electron Tomography and Atom Probe Tomography Xiong, Xiangyuan; Weyland, Matthew Microscopy and Microanalysis, Vol. 20, Issue 4 https://doi.org/10.1017/s1431927614000798	journal	May 2014
Calculation of the surface energy of bcc transition metals by using the second nearest–neighbor modified embedded atom method Zhang, Jian-Min; Wang, Dou-Dou; Xu, Ke-Wei Applied Surface Science, Vol. 252, Issue 23 https://doi.org/10.1016/j.apsusc.2005.10.043	journal	September 2006
Four-dimensional spectral low-loss energy-filtered transmission electron tomography of silicon nanowire-based capacitors Haberfehlner, G.; Bayle-Guillemaud, P.; Audoit, G. Applied Physics Letters, Vol. 101, Issue 6 https://doi.org/10.1063/1.4742932	journal	August 2012
3D analysis of advanced nano-devices using electron and atom probe tomography Grenier, A.; Duguay, S.; Barnes, J. P. Ultramicroscopy, Vol. 136 https://doi.org/10.1016/j.ultramic.2013.10.001	journal	January 2014
Local Electrode Atom Probe Tomography: A User's Guide Larson, David J.; Prosa, Ty J.; Ulfig, Robert M. https://doi.org/10.1007/978-1-4614-8721-0	book	January 2013
Experimental study on modulated structure in Alnico alloys under high magnetic field and comparison with phase-field simulation Sun, X. Y.; Chen, C. L.; Yang, L. Journal of Magnetism and Magnetic Materials, Vol. 348 https://doi.org/10.1016/j.jmmm.2013.07.050	journal	December 2013
Formation of bimetallic clusters in superfluid helium nanodroplets analysed by atomic resolution electron tomography Haberfehlner, Georg; Thaler, Philipp; Knez, Daniel Nature Communications, Vol. 6, Issue 1 https://doi.org/10.1038/ncomms9779	journal	October 2015
In situ site-specific specimen preparation for atom probe tomography Thompson, K.; Lawrence, D.; Larson, D. J. Ultramicroscopy, Vol. 107, Issue 2-3 https://doi.org/10.1016/j.ultramic.2006.06.008	journal	February 2007
Architecture and magnetism of alnico Zhou, Lin; Miller, M. K.; Lu, Ping Acta Materialia, Vol. 74 https://doi.org/10.1016/j.actamat.2014.04.044	journal	August 2014
Combining structural and chemical information at the nanometer scale by correlative transmission electron microscopy and atom probe tomography Herbig, M.; Choi, P.; Raabe, D. Ultramicroscopy, Vol. 153 https://doi.org/10.1016/j.ultramic.2015.02.003	journal	June 2015
Combined atom probe tomography and density functional theory investigation of the Al off-stoichiometry of κ-carbides in an austenitic Fe–Mn–Al–C low density steel Yao, M. J.; Dey, P.; Seol, J. -B. Acta Materialia, Vol. 106 https://doi.org/10.1016/j.actamat.2016.01.007	journal	March 2016
Three-Dimensional Elemental Mapping at the Atomic Scale in Bimetallic Nanocrystals Goris, Bart; De Backer, Annick; Van Aert, Sandra Nano Letters, Vol. 13, Issue 9 https://doi.org/10.1021/nl401945b	journal	August 2013
The Physics of Ferromagnetism Miyazaki, Terunobu; Jin, Hanmin Springer Series in Materials Science https://doi.org/10.1007/978-3-642-25583-0	book	January 2012
Nanoscale doping profiles within CdTe grain boundaries and at the CdS/CdTe interface revealed by atom probe tomography and STEM EBIC Poplawsky, Jonathan D.; Li, Chen; Paudel, Naba R. Solar Energy Materials and Solar Cells, Vol. 150 https://doi.org/10.1016/j.solmat.2016.02.004	journal	June 2016
Contamination-Free Transmission Electron Microscopy for High-Resolution Carbon Elemental Mapping of Polymers Horiuchi, Shin; Hanada, Takeshi; Ebisawa, Masaharu ACS Nano, Vol. 3, Issue 5 https://doi.org/10.1021/nn9001598	journal	April 2009
Towards better 3-D reconstructions by combining electron tomography and atom-probe tomography Arslan, Ilke; Marquis, Emmanuelle A.; Homer, Mark Ultramicroscopy, Vol. 108, Issue 12 https://doi.org/10.1016/j.ultramic.2008.05.008	journal	November 2008
A Model Based Iterative Reconstruction Algorithm For High Angle Annular Dark Field-Scanning Transmission Electron Microscope (HAADF-STEM) Tomography Venkatakrishnan, S. V.; Drummy, L. F.; Jackson, M. A. IEEE Transactions on Image Processing, Vol. 22, Issue 11 https://doi.org/10.1109/TIP.2013.2277784	journal	November 2013
Atom probe crystallography Gault, Baptiste; Moody, Michael P.; Cairney, Julie M. Materials Today, Vol. 15, Issue 9 https://doi.org/10.1016/S1369-7021(12)70164-5	journal	September 2012
Moment-preserving thresolding: A new approach Tsai, Wen-Hsiang Computer Vision, Graphics, and Image Processing, Vol. 29, Issue 3 https://doi.org/10.1016/0734-189X(85)90133-1	journal	March 1985
Recent Advances in Electron Tomography: TEM and HAADF-STEM Tomography for Materials Science and Semiconductor Applications Kübel, Christian; Voigt, Andreas; Schoenmakers, Remco Microscopy and Microanalysis, Vol. 11, Issue 5, p. 378-400 https://doi.org/10.1017/S1431927605050361	journal	September 2005
Nanoscale voxel spectroscopy by simultaneous EELS and EDS tomography Haberfehlner, Georg; Orthacker, Angelina; Albu, Mihaela Nanoscale, Vol. 6, Issue 23 https://doi.org/10.1039/C4NR04553J	journal	January 2014
Micro-CT data of early physiological cancellous bone formation in the lumbar spine of female C57BL/6 mice Zenzes, Michael; Zaslansky, Paul Scientific Data, Vol. 8, Issue 1 https://doi.org/10.1038/s41597-021-00913-y	journal	May 2021
Monitoring Galvanic Replacement Through Three-Dimensional Morphological and Chemical Mapping Goris, Bart; Polavarapu, Lakshminarayana; Bals, Sara arXiv https://doi.org/10.48550/arxiv.1411.4276	text	January 2014

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