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

Abstract

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 α 1 phases that are nucleated in the Ni-rich α 2 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.

Authors:
 [1];  [1];  [2];  [2];  [2];  [3];  [1]
  1. Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Center for Nanophase Materials Science (CNMS)
  2. Ames Lab., Ames, IA (United States). Division of Materials Science and Engineering
  3. Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Materials Science & Technology Division
Publication Date:
Research Org.:
Ames Laboratory (AMES), Ames, IA (United States); Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)
Sponsoring Org.:
USDOE Office of Science (SC)
OSTI Identifier:
1394424
Alternate Identifier(s):
OSTI ID: 1342944
Report Number(s):
IS-J-9002
Journal ID: ISSN 1431-9276; PII: S1431927616012496
Grant/Contract Number:  
AC02-07CH11358; AC05-00OR22725
Resource Type:
Journal Article: Accepted Manuscript
Journal Name:
Microscopy and Microanalysis
Additional Journal Information:
Journal Volume: 22; Journal Issue: 06; Journal ID: ISSN 1431-9276
Publisher:
Microscopy Society of America (MSA)
Country of Publication:
United States
Language:
English
Subject:
36 MATERIALS SCIENCE; phase separation; atom probe tomography (APT); electron tomography; alnico alloy; correlative tomography

Citation Formats

Guo, Wei, Sneed, Brian T., Zhou, Lin, Tang, Wei, Kramer, Matthew J., Cullen, David A., and Poplawsky, Jonathan D. Correlative Energy-Dispersive X-Ray Spectroscopic Tomography and Atom Probe Tomography of the Phase Separation in an Alnico 8 Alloy. United States: N. p., 2016. Web. doi:10.1017/S1431927616012496.
Guo, Wei, Sneed, Brian T., Zhou, Lin, Tang, Wei, Kramer, Matthew J., Cullen, David A., & Poplawsky, Jonathan D. Correlative Energy-Dispersive X-Ray Spectroscopic Tomography and Atom Probe Tomography of the Phase Separation in an Alnico 8 Alloy. United States. doi:10.1017/S1431927616012496.
Guo, Wei, Sneed, Brian T., Zhou, Lin, Tang, Wei, Kramer, Matthew J., Cullen, David A., and Poplawsky, Jonathan D. Wed . "Correlative Energy-Dispersive X-Ray Spectroscopic Tomography and Atom Probe Tomography of the Phase Separation in an Alnico 8 Alloy". United States. doi:10.1017/S1431927616012496. https://www.osti.gov/servlets/purl/1394424.
@article{osti_1394424,
title = {Correlative Energy-Dispersive X-Ray Spectroscopic Tomography and Atom Probe Tomography of the Phase Separation in an Alnico 8 Alloy},
author = {Guo, Wei and Sneed, Brian T. and Zhou, Lin and Tang, Wei and Kramer, Matthew J. and Cullen, David A. and Poplawsky, Jonathan D.},
abstractNote = {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.},
doi = {10.1017/S1431927616012496},
journal = {Microscopy and Microanalysis},
number = 06,
volume = 22,
place = {United States},
year = {Wed Dec 21 00:00:00 EST 2016},
month = {Wed Dec 21 00:00:00 EST 2016}
}

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Works referenced in this record:

Recent Advances in Electron Tomography: TEM and HAADF-STEM Tomography for Materials Science and Semiconductor Applications
journal, September 2005

  • K�bel, Christian; Voigt, Andreas; Schoenmakers, Remco
  • Microscopy and Microanalysis, Vol. 11, Issue 5, p. 378-400
  • DOI: 10.1017/S1431927605050361