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Title: Three-Dimensional FIB/EBSD Characterization of Irradiated HfAl3-Al Composite

Abstract

A thermal neutron absorbing material, comprised of 28.4 vol% HfAl3 in an Al matrix, was developed to serve as a conductively cooled thermal neutron filter to enable fast flux materials and fuels testing in a pressurized water reactor. In order to observe the microstructural change of the HfAl3-Al composite due to neutron irradiation, an EBSD-FIB characterization approach is developed and presented in this paper. Using the focused ion beam (FIB), the sample was fabricated to 25µm × 25µm × 20 µm and mounted on the grid. A series of operations were carried out repetitively on the sample top surface to prepare it for scanning electron microscopy (SEM). First, a ~100-nm layer was removed by high voltage FIB milling. Then, several cleaning passes were performed on the newly exposed surface using low voltage FIB milling to improve the SEM image quality. Last, the surface was scanned by Electron Backscattering Diffraction (EBSD) to obtain the two-dimensional image. After 50 to 100 two-dimensional images were collected, the images were stacked to reconstruct a three-dimensional model using DREAM.3D software. Two such reconstructed three-dimensional models were obtained from samples of the original and post-irradiation HfAl3-Al composite respectively, from which the most significant microstructural change causedmore » by neutron irradiation apparently is the size reduction of both HfAl3 and Al grains. The possible reason is the thermal expansion and related thermal strain from the thermal neutron absorption. This technique can be applied to three-dimensional microstructure characterization of irradiated materials.« less

Authors:
; ; ;
Publication Date:
Research Org.:
Idaho National Lab. (INL), Idaho Falls, ID (United States)
Sponsoring Org.:
USDOE Office of Nuclear Energy (NE)
OSTI Identifier:
1358236
Report Number(s):
INL/CON-16-37835
DOE Contract Number:
DE-AC07-05ID14517
Resource Type:
Conference
Resource Relation:
Conference: Top Fuel 2016, Boise, ID, USA, September 11–15, 2016
Country of Publication:
United States
Language:
English
Subject:
21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS; 3D microstructural reconstruction; focused ion beam milling; neutron absorber

Citation Formats

Hua, Zilong, Guillen, Donna Post, Harris, William, and Ban, Heng. Three-Dimensional FIB/EBSD Characterization of Irradiated HfAl3-Al Composite. United States: N. p., 2016. Web.
Hua, Zilong, Guillen, Donna Post, Harris, William, & Ban, Heng. Three-Dimensional FIB/EBSD Characterization of Irradiated HfAl3-Al Composite. United States.
Hua, Zilong, Guillen, Donna Post, Harris, William, and Ban, Heng. Thu . "Three-Dimensional FIB/EBSD Characterization of Irradiated HfAl3-Al Composite". United States. doi:. https://www.osti.gov/servlets/purl/1358236.
@article{osti_1358236,
title = {Three-Dimensional FIB/EBSD Characterization of Irradiated HfAl3-Al Composite},
author = {Hua, Zilong and Guillen, Donna Post and Harris, William and Ban, Heng},
abstractNote = {A thermal neutron absorbing material, comprised of 28.4 vol% HfAl3 in an Al matrix, was developed to serve as a conductively cooled thermal neutron filter to enable fast flux materials and fuels testing in a pressurized water reactor. In order to observe the microstructural change of the HfAl3-Al composite due to neutron irradiation, an EBSD-FIB characterization approach is developed and presented in this paper. Using the focused ion beam (FIB), the sample was fabricated to 25µm × 25µm × 20 µm and mounted on the grid. A series of operations were carried out repetitively on the sample top surface to prepare it for scanning electron microscopy (SEM). First, a ~100-nm layer was removed by high voltage FIB milling. Then, several cleaning passes were performed on the newly exposed surface using low voltage FIB milling to improve the SEM image quality. Last, the surface was scanned by Electron Backscattering Diffraction (EBSD) to obtain the two-dimensional image. After 50 to 100 two-dimensional images were collected, the images were stacked to reconstruct a three-dimensional model using DREAM.3D software. Two such reconstructed three-dimensional models were obtained from samples of the original and post-irradiation HfAl3-Al composite respectively, from which the most significant microstructural change caused by neutron irradiation apparently is the size reduction of both HfAl3 and Al grains. The possible reason is the thermal expansion and related thermal strain from the thermal neutron absorption. This technique can be applied to three-dimensional microstructure characterization of irradiated materials.},
doi = {},
journal = {},
number = ,
volume = ,
place = {United States},
year = {Thu Sep 01 00:00:00 EDT 2016},
month = {Thu Sep 01 00:00:00 EDT 2016}
}

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