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Title: Three-dimensional imaging of grain boundaries via quantitative fluorescence X-ray tomography analysis

Journal Article · · Communications Materials

Abstract Three-dimensional visualization of material composition within multiple grains and across complex networks of grain boundaries at nanoscales can provide new insight into the structure evolution and emerging functional properties of the material for diverse applications. Here, using nanoscale scanning X-ray fluorescence tomography, coupled with an advanced self-absorption correction algorithm developed in this work, we analyze the three-dimensional gain distributions and compositions in a Ce 0.8 Gd 0.2 O 2-δ -CoFe 2 O 4 mixed ionic-electronic conductor system with high accuracy and statistical significance. Our systematic investigation reveals an additional emergent phase and uncovers highly intriguing composition stability ranges for the multiple material phases within this system. The presented visualization of composition variations across complex interfaces, supported by our quantitative composition analysis, discloses mechanistic pathways of the diverse phase transformations occurring in the material synthesis, providing insights for the optimization of transport properties in the mixed ionic-electronic conductor system.

Research Organization:
Argonne National Laboratory (ANL); Argonne National Laboratory (ANL), Argonne, IL (United States); Brookhaven National Laboratory (BNL), Upton, NY (United States)
Sponsoring Organization:
USDOE; USDOE Laboratory Directed Research and Development (LDRD) Program; USDOE Office of Science (SC), Basic Energy Sciences (BES)
Grant/Contract Number:
AC02-06CH11357; SC0001061; SC0012704
OSTI ID:
1871266
Report Number(s):
BNL-223306-2022-JAAM; 37; PII: 259
Journal Information:
Communications Materials, Journal Name: Communications Materials Journal Issue: 1 Vol. 3; ISSN 2662-4443
Publisher:
Nature Publishing GroupCopyright Statement
Country of Publication:
United Kingdom
Language:
English

References (58)

Micromechanical Characterization of Ce 0.8 Gd 0.2 O 2‐ δ –FeCo 2 O 4 Dual Phase Oxygen Transport Membranes journal March 2020
Making Li-Air Batteries Rechargeable: Material Challenges journal May 2012
A Self-Forming Composite Electrolyte for Solid-State Sodium Battery with Ultralong Cycle Life journal October 2016
Rational Design of Lower-Temperature Solid Oxide Fuel Cell Cathodes via Nanotailoring of Co-Assembled Composite Structures journal October 2014
Defect cluster formation in M2O3-doped CeO2 journal January 1999
Dense ceramic membranes for methane conversion journal July 2003
The effect of Fe doping on the sintering behavior of commercial CeO2 powder journal June 2001
Hierarchical Defect Engineering for LiCoO2 through Low-Solubility Trace Element Doping journal October 2020
Synthesis of Co1.5Fe1.5O4 spinel ferrite with high magnetic squareness and study its magnetic property by annealing the chemical routed sample at different temperatures journal May 2013
Phase and microstructural characterizations for Ce0.8Gd0.2O2--FeCo2O4 dual phase oxygen transport membranes journal December 2020
Structural characterization of the CeO2/Gd2O3 mixed system by synchrotron X-ray diffraction journal June 2012
Phase relations, lattice thermal expansion in CeO2–Gd2O3 system, and stabilization of cubic gadolinia journal May 2004
Enhancing oxygen permeation of solid-state reactive sintered Ce0.8Gd0.2O2--FeCo2O4 composite by optimizing the powder preparation method journal June 2021
Progress in material selection for solid oxide fuel cell technology: A review journal July 2015
Numerical methods in tomography journal January 1999
Measuring Three-Dimensional Strain and Structural Defects in a Single InGaAs Nanowire Using Coherent X-ray Multiangle Bragg Projection Ptychography journal January 2018
Enhanced Oxygen Reduction Activity on Ruddlesden–Popper Phase Decorated La 0.8 Sr 0.2 FeO 3−δ 3D Heterostructured Cathode for Solid Oxide Fuel Cells journal March 2017
In Situ Formation of Er 0.4 Bi 1.6 O 3 Protective Layer at Cobaltite Cathode/Y 2 O 3 –ZrO 2 Electrolyte Interface under Solid Oxide Fuel Cell Operation Conditions journal November 2018
Lanthanide-Binding Tags for 3D X-ray Imaging of Proteins in Cells at Nanoscale Resolution journal January 2020
Effects of Concentration, Crystal Structure, Magnetism, and Electronic Structure Method on First-Principles Oxygen Vacancy Formation Energy Trends in Perovskites journal November 2014
Three-dimensional X-ray structural microscopy with submicrometre resolution journal February 2002
Stabilizing nanostructures in metals using grain and twin boundary architectures journal March 2016
High-resolution non-destructive three-dimensional imaging of integrated circuits journal March 2017
Relating structure and composition with accessibility of a single catalyst particle using correlative 3-dimensional micro-spectroscopy journal August 2016
Dark-field X-ray microscopy for multiscale structural characterization journal January 2015
Enhancing grain boundary ionic conductivity in mixed ionic–electronic conductors journal April 2015
Trace doping of multiple elements enables stable battery cycling of LiCoO2 at 4.6 V journal June 2019
Long-range symmetry breaking in embedded ferroelectrics journal June 2018
11 nm hard X-ray focus from a large-aperture multilayer Laue lens journal December 2013
Bi-continuous pattern formation in thin films via solid-state interfacial dealloying studied by multimodal characterization journal January 2019
Electrochemistry and energy conversion features of protonic ceramic cells with mixed ionic-electronic electrolytes journal January 2022
Phase formation and performance of solid state reactive sintered Ce 0.8 Gd 0.2 O 2− δ –FeCo 2 O 4 composites journal January 2022
Characterization of 3D interconnected microstructural network in mixed ionic and electronic conducting ceramic composites journal January 2014
Reconstructing x-ray fluorescence microtomograms journal September 2001
Internal elemental microanalysis combining x-ray fluorescence, Compton and transmission tomography journal July 2003
Quantitative X-ray fluorescence computed tomography for low-Z samples using an iterative absorption correction algorithm journal May 2017
Two-dimensional detector software: From real detector to idealised image or two-theta scan journal January 1996
Inversion of the attenuated Radon transform journal January 2001
Fast numerical inversion of the attenuated Radon transform with full and partial measurements journal May 2004
Multimodal hard x-ray imaging with resolution approaching 10 nm for studies in material science journal March 2018
Focused ion beam preparation of samples for X-ray nanotomography journal July 2012
TomoPy: a framework for the analysis of synchrotron tomographic data journal August 2014
Design and performance of an X-ray scanning microscope at the Hard X-ray Nanoprobe beamline of NSLS-II journal October 2017
Monotonic penalized-likelihood image reconstruction for X-ray fluorescence computed tomography journal September 2006
Iterative Reconstruction in X-ray Fluorescence Tomography Based on Radon Inversion journal February 2011
Fluorescent Computer Tomography: A Model For Correction Of X-ray Absorption journal December 1991
Influence of Microstructure and Surface Activation of Dual-Phase Membrane Ce 0.8 Gd 0.2 O 2−δ -FeCo 2 O 4 on Oxygen Permeation journal September 2015
Penalized-likelihood image reconstruction for x-ray fluorescence computed tomography journal July 2006
High-sensitivity nanoscale chemical imaging with hard x-ray nano-XANES journal September 2020
High-Resolution Scanning X-ray Diffraction Microscopy journal July 2008
Dense dislocation arrays embedded in grain boundaries for high-performance bulk thermoelectrics journal April 2015
Selective increase in CO 2 electroreduction activity at grain-boundary surface terminations journal November 2017
Optimization-Based Approach for Joint X-Ray Fluorescence and Transmission Tomographic Inversion journal January 2016
Quantitative Nanoscale 3D Imaging of Intergranular Corrosion of 304 Stainless Steel Using Hard X-Ray Nanoprobe journal January 2019
Hyperspectral image reconstruction for x-ray fluorescence tomography journal January 2015
Joint reconstruction of x-ray fluorescence and transmission tomography journal January 2017
Tunable hard x-ray nanofocusing with Fresnel zone plates fabricated using deep etching journal January 2020
Efficient concentration of high-energy x-rays for diffraction-limited imaging resolution journal January 2017