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Title: 3-dimensional characterization of polycrystalline bulk materials using high energy synchrotron radiation

Abstract

The implementation of 3-Dimensional X-Ray Diffraction (3DXRD) Microscopy at the Advanced Photon Source is described. The technique enables the non-destructive structural characterization of polycrystalline bulk materials and is therefore suitable for in situ studies during thermo-mechanical processing. High energy synchrotron radiation and area detectors are employed. First, a forward modeling approach for the reconstruction of grain boundaries from high resolution diffraction images is described. Second, a high resolution reciprocal space mapping technique of individual grains is presented. The microstructure of polycrystalline materials is characterized by a hierarchical arrangement of crystalline elements (grains, microbands, and subgrains). The arrangement is often highlyheterogeneous, especially with respect to the dynamics during processing. Conventional experimental methods either lack sufficient spatial resolution or are surface or thin foil probes, which require samples to be sectioned before investigation to obtain spatially resolved results representative of bulk behavior. This destructive procedure prohibits studies of the dynamics of the individual elements. Thus, there is a need for a nondestructive method that provides comprehensive structural information for each of the crystalline elements within macroscopic volumes of the material. Furthermore, the method should be sufficiently fast to record the dynamics of 10-1000 elements simultaneously during processing.

Authors:
; ; ; ; ; ; ; ; ;
Publication Date:
Research Org.:
Argonne National Lab. (ANL), Argonne, IL (United States)
Sponsoring Org.:
USDOE Office of Science (SC); National Science Foundation (NSF); FOR
OSTI Identifier:
982321
Report Number(s):
ANL/XFD/CP-117475
Journal ID: ISSN 1662-9752; TRN: US201013%%999
DOE Contract Number:
DE-AC02-06CH11357
Resource Type:
Conference
Resource Relation:
Journal Name: Mater. Sci. Forum; Journal Volume: 539-543; Journal Issue: 2007; Conference: International Conference on Processing & Manufacting of Advanced Materials (Thermec 2006); Jul. 4, 2006 - Jul. 8, 2006; Vancouver, Canada
Country of Publication:
United States
Language:
ENGLISH
Subject:
37 INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY; 46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND TECHNOLOGY; ADVANCED PHOTON SOURCE; BEHAVIOR; DIFFRACTION; DYNAMICS; ELEMENTS; ENERGY; FOILS; GRAIN BOUNDARIES; IMAGES; IMPLEMENTATION; INFORMATION; MAPPING; MICROSCOPY; MICROSTRUCTURE; PROBES; PROCESSING; RESOLUTION; SPACE; SPATIAL RESOLUTION; SURFACES; SYNCHROTRON RADIATION; X-RAY DIFFRACTION

Citation Formats

Lienert, U., Almer, J., Jakobsen, B., Pantleon, W., Poulsen, H. F., Hennessy, D., Xiao, C., Suter, R. M., Riso National Lab., and Carnegie Mellon Univ. 3-dimensional characterization of polycrystalline bulk materials using high energy synchrotron radiation. United States: N. p., 2007. Web. doi:10.4028/www.scientific.net/MSF.539-543.2353.
Lienert, U., Almer, J., Jakobsen, B., Pantleon, W., Poulsen, H. F., Hennessy, D., Xiao, C., Suter, R. M., Riso National Lab., & Carnegie Mellon Univ. 3-dimensional characterization of polycrystalline bulk materials using high energy synchrotron radiation. United States. doi:10.4028/www.scientific.net/MSF.539-543.2353.
Lienert, U., Almer, J., Jakobsen, B., Pantleon, W., Poulsen, H. F., Hennessy, D., Xiao, C., Suter, R. M., Riso National Lab., and Carnegie Mellon Univ. Mon . "3-dimensional characterization of polycrystalline bulk materials using high energy synchrotron radiation". United States. doi:10.4028/www.scientific.net/MSF.539-543.2353.
@article{osti_982321,
title = {3-dimensional characterization of polycrystalline bulk materials using high energy synchrotron radiation},
author = {Lienert, U. and Almer, J. and Jakobsen, B. and Pantleon, W. and Poulsen, H. F. and Hennessy, D. and Xiao, C. and Suter, R. M. and Riso National Lab. and Carnegie Mellon Univ.},
abstractNote = {The implementation of 3-Dimensional X-Ray Diffraction (3DXRD) Microscopy at the Advanced Photon Source is described. The technique enables the non-destructive structural characterization of polycrystalline bulk materials and is therefore suitable for in situ studies during thermo-mechanical processing. High energy synchrotron radiation and area detectors are employed. First, a forward modeling approach for the reconstruction of grain boundaries from high resolution diffraction images is described. Second, a high resolution reciprocal space mapping technique of individual grains is presented. The microstructure of polycrystalline materials is characterized by a hierarchical arrangement of crystalline elements (grains, microbands, and subgrains). The arrangement is often highlyheterogeneous, especially with respect to the dynamics during processing. Conventional experimental methods either lack sufficient spatial resolution or are surface or thin foil probes, which require samples to be sectioned before investigation to obtain spatially resolved results representative of bulk behavior. This destructive procedure prohibits studies of the dynamics of the individual elements. Thus, there is a need for a nondestructive method that provides comprehensive structural information for each of the crystalline elements within macroscopic volumes of the material. Furthermore, the method should be sufficiently fast to record the dynamics of 10-1000 elements simultaneously during processing.},
doi = {10.4028/www.scientific.net/MSF.539-543.2353},
journal = {Mater. Sci. Forum},
number = 2007,
volume = 539-543,
place = {United States},
year = {Mon Jan 01 00:00:00 EST 2007},
month = {Mon Jan 01 00:00:00 EST 2007}
}

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  • The microstructure of polycrystalline materials is characterized by a hierarchical arrangement of crystalline elements (grains, microbands, and subgrains). The arrangement is often highly heterogeneous, especially with respect to dynamics during processing. Conventional experimental methods either lack sufficient spatial resolution or are surface or thin foil probes. To obtain three dimensional spatially resolved results with these latter techniques requires that samples be sectioned. This destructive procedure prohibits studies of the dynamics of the individual crystalline elements. Thus, there is a need for a nondestructive method that provides comprehensive structural information for each of the crystalline elements within macroscopic volumes of themore » material. Furthermore, the method should be sufficiently fast to record the dynamics of 10-1000 elements simultaneously during processing. Three-dimensional x-ray diffraction (3DXRD) microscopy is an emerging method that aims to fulfill these requirements. The method is distinguished by two principles. The first is the use of a beam of high-energy x-rays generated by a synchrotron source for transmission studies. Hard x-rays (in the range 50-100 keV) can penetrate 4 cm of aluminum or 5 mm of steel. The second principle is a 'tomographic' approach to diffraction. The conventional approach for providing spatially resolved information with diffraction is to scan the sample with respect to the beam. However, probing the sample point-by-point is generally too slow for dynamic studies. Hence, it has been replaced by an approach that provides information on many parts of the material simultaneously. Here we report on activities establishing 3DXRD capabilities at The Advanced Photon Source (Argonne National Laboratory) within the high-energy program at beamline 1-ID.« less
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  • We report a multipurpose furnace designed for studies using synchrotron radiation on polycrystalline materials, namely, metals, ceramics, and (semi)crystalline polymers. The furnace has been designed to carry out three-dimensional (3D) x-ray diffraction measurements but can also be used for other types of synchrotron radiation research. The furnace has a very low thermal gradient across the specimen (<0.2 degree sign C/mm). Accurate determination of the temperature can be carried out by welding a thermocouple to the specimen. The furnace can be rotated over an angle of 90 degree sign in order to determine the crystallographic orientation of each individual grain. Itmore » is possible to follow growth kinetics of all grains in the illuminated volume of the specimen. The specimen environment can be controlled varying from vacuum (up to 10{sup -5} mbar) to gas or air filled. The maximum temperature of operation is 1500 degree sign C, with the possibility of achieving high heating (up to 20 deg. C/s) and cooling rates (up to 30 deg. C/s without quenching gas). 3D maps of the microstructure of the specimen can be generated at elevated temperatures by bringing the high-resolution detector close to the specimen. We show an example of a simulation of the heat affected zone during the thermal cycle of a weld in a transformation-induced plasticity steel carried out using the furnace. The unique characteristics of the furnace open possibility of new fields in materials research using synchrotron radiation.« less