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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 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.

Authors:
 [1];  [1];  [2];  [2];  [2];  [1];  [1]
  1. Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)
  2. Ames Lab., Ames, IA (United States)
Publication Date:
Research Org.:
Oak Ridge National Laboratory (ORNL), Oak Ridge, TN (United States); Ames Laboratory (AMES), Ames, IA (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; applab
Grant/Contract Number:  
AC05-00OR22725; AC02-07CH11358
Resource Type:
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; correlative tomography; alnico alloy

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. https://doi.org/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. https://doi.org/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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Cited by: 24 works
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Figures / Tables:

Figure 1 Figure 1: Schematic experimental workflow for conducting correlative STEM-EDS and APT tomography. (a) Electropolishing adapter and set up; (b) The ideal geometry of the rod-shaped holder and the SEM/FIB adapter that is suitable for dual SEM/FIB imaging; (c) Lift out process of a (100) targeted grain. (d) Final tip shapemore » after sample preparation; (e) The Fischione tomography holder containing the needle shaped specimen; (f) APT puck holder dedicated for rod specimens.« less

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Works referenced in this record:

STEM tomography for thick biological specimens
journal, December 2008


Crystallographic structural analysis in atom probe microscopy via 3D Hough transformation
journal, May 2011


Enhanced Detection Sensitivity with a New Windowless XEDS System for AEM Based on Silicon Drift Detector Technology
journal, July 2010


Early-stage nucleation of manganese sulfide particle and its processing evolution in Fe—3wt.%Si alloys
journal, December 2015


Correlative Tomography
journal, April 2014

  • Burnett, T. L.; McDonald, S. A.; Gholinia, A.
  • Scientific Reports, Vol. 4, Issue 1
  • DOI: 10.1038/srep04711

The quantitative analysis of thin specimens: a review of progress from the Cliff-Lorimer to the new zeta-factor methods
journal, February 2006


An atom probe perspective on phase separation and precipitation in duplex stainless steels
journal, May 2016


Evolution of Fe–Co rich particles in Alnico 8 alloy thermomagnetically treated at 800°C
journal, September 2000


Phase separation in metallic glasses
journal, October 2013


Electron tomography and holography in materials science
journal, April 2009

  • Midgley, Paul A.; Dunin-Borkowski, Rafal E.
  • Nature Materials, Vol. 8, Issue 4
  • DOI: 10.1038/nmat2406

BoneJ: Free and extensible bone image analysis in ImageJ
journal, December 2010


Monitoring Galvanic Replacement Through Three-Dimensional Morphological and Chemical Mapping
journal, May 2014

  • Goris, Bart; Polavarapu, Lakshminarayana; Bals, Sara
  • Nano Letters, Vol. 14, Issue 6
  • DOI: 10.1021/nl500593j

Performance of a local electrode atom probe
journal, January 2007

  • Miller, M. K.; Russell, K. F.
  • Surface and Interface Analysis, Vol. 39, Issue 2-3
  • DOI: 10.1002/sia.2488

Microstructural Characterization of an Al-Li-Mg-Cu Alloy by Correlative Electron Tomography and Atom Probe Tomography
journal, May 2014


Calculation of the surface energy of bcc transition metals by using the second nearest–neighbor modified embedded atom method
journal, September 2006


Four-dimensional spectral low-loss energy-filtered transmission electron tomography of silicon nanowire-based capacitors
journal, August 2012

  • Haberfehlner, G.; Bayle-Guillemaud, P.; Audoit, G.
  • Applied Physics Letters, Vol. 101, Issue 6
  • DOI: 10.1063/1.4742932

3D analysis of advanced nano-devices using electron and atom probe tomography
journal, January 2014


Local Electrode Atom Probe Tomography: A User's Guide
book, January 2013


Experimental study on modulated structure in Alnico alloys under high magnetic field and comparison with phase-field simulation
journal, December 2013


Formation of bimetallic clusters in superfluid helium nanodroplets analysed by atomic resolution electron tomography
journal, October 2015

  • Haberfehlner, Georg; Thaler, Philipp; Knez, Daniel
  • Nature Communications, Vol. 6, Issue 1
  • DOI: 10.1038/ncomms9779

In situ site-specific specimen preparation for atom probe tomography
journal, February 2007


Architecture and magnetism of alnico
journal, August 2014


Three-Dimensional Elemental Mapping at the Atomic Scale in Bimetallic Nanocrystals
journal, August 2013

  • Goris, Bart; De Backer, Annick; Van Aert, Sandra
  • Nano Letters, Vol. 13, Issue 9
  • DOI: 10.1021/nl401945b

The Physics of Ferromagnetism
book, January 2012


Nanoscale doping profiles within CdTe grain boundaries and at the CdS/CdTe interface revealed by atom probe tomography and STEM EBIC
journal, June 2016


Contamination-Free Transmission Electron Microscopy for High-Resolution Carbon Elemental Mapping of Polymers
journal, April 2009

  • Horiuchi, Shin; Hanada, Takeshi; Ebisawa, Masaharu
  • ACS Nano, Vol. 3, Issue 5
  • DOI: 10.1021/nn9001598

Towards better 3-D reconstructions by combining electron tomography and atom-probe tomography
journal, November 2008


A Model Based Iterative Reconstruction Algorithm For High Angle Annular Dark Field-Scanning Transmission Electron Microscope (HAADF-STEM) Tomography
journal, November 2013

  • Venkatakrishnan, S. V.; Drummy, L. F.; Jackson, M. A.
  • IEEE Transactions on Image Processing, Vol. 22, Issue 11
  • DOI: 10.1109/TIP.2013.2277784

Atom probe crystallography
journal, September 2012


Moment-preserving thresolding: A new approach
journal, March 1985


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

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

Nanoscale voxel spectroscopy by simultaneous EELS and EDS tomography
journal, January 2014

  • Haberfehlner, Georg; Orthacker, Angelina; Albu, Mihaela
  • Nanoscale, Vol. 6, Issue 23
  • DOI: 10.1039/C4NR04553J

Micro-CT data of early physiological cancellous bone formation in the lumbar spine of female C57BL/6 mice
journal, May 2021


Monitoring Galvanic Replacement Through Three-Dimensional Morphological and Chemical Mapping
text, January 2014


Works referencing / citing this record:

PtCo Cathode Catalyst Morphological and Compositional Changes after PEM Fuel Cell Accelerated Stress Testing
journal, January 2018

  • Sneed, Brian T.; Cullen, David A.; Mukundan, R.
  • Journal of The Electrochemical Society, Vol. 165, Issue 6
  • DOI: 10.1149/2.0091806jes

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