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Title: Mesoscale response of individual grains of polycrystalline BaTiO{sub 3}to electrical loading.

Abstract

Ranging from sub-grain structures to grain clusters, the mesoscale is critical in understanding the constitutive behavior of ferroelectrics. The interaction of domains with grain boundaries and grain-to-grain constraints largely determine the overall response of a ferroelectric. Unfortunately, the most severe paucity of quantitative data also exists at the mesoscale. The newly developed 3-D XRD technique offers a unique opportunity to study the response of ferroelectrics to external stimuli at this scale by allowing the investigation of individual grains within a polycrystal. To demonstrate the feasibility of 3-D XRD in ferroelectrics research for the first time, a polycrystalline BaTiO{sub 3} was subjected to quasi-statically cycled electric field. The experiments were performed at beamlines 1-ID-C of the Advanced Photon Source (APS) and ID-11 of the European Synchrotron Radiation Facility (ESRF), Grenoble, France. In both cases, nominally the same polycrystalline BaTiO{sub 3} samples (about 1 x 1 x 5 mm{sup 3}) were employed. The specimens were held upright in the geometry shown in Fig. 1 and run in transmission mode using {approx}80 keV X-rays. The direction of the electric field was perpendicular to the X-ray beam and it was stepped up to a maximum of {+-} 20 kV/cm, well above the nominal coercivemore » field of the material ({approx}5 kV/cm). At each applied field value, the specimen was rotated perpendicular to the beam in 0.1{sup o} {omega} steps (Fig. 1) up to {+-} 45{sup o} (at ESRF) and {+-} 65{sup o} (at APS). The X-ray spot size was about 150 x 150 {micro}m{sup 2} at ESRF and 30 x 30 {micro}m{sup 2} at APS. Since the grain size of the BaTiO{sub 3} samples was measured to be {approx}20-30 {micro}m from SEM images, either sampling volume was large enough to capture a reasonable number of grains. The diffraction data were analyzed using the GRAINDEX software from Risoe. This analysis attempted to identify individual grains and track their response to electric field. In a parallel study, the macroscopic (polycrystalline) response of the material was obrained by integrating data within {+-} 10{sup o} {omega} around the {omega} = 0{sup o} position (perpendicular to the beam) and parallel to the electric field using the Fit2D software from ESRF (Fig. 2). The macroscopic behavior of the material (Fig. 2) was as expected from a polycrystalline ferroelectric: the electric field led to an increase of the 002 intensity due to domain alignment along the field direction. Fig. 2 also displays the MRD value (multiples of random distribution relative to an unpoled sample) obtained from this equation: MRD = 3I{sub 002}/(I{sub 002} + 2I{sub 200}). The MRD is a better measure of texture evolution due to domain reorientation and should be 1.0 for a random polycrystal. In Fig. 2, while the initial state of the specimen is not random (MRD {approx} 0.7), the applied field leads to significant domain re-alignment (MRD {approx} 1.5 at 2000 V). Unfortunately, the GRAINDEX analysis has not been successful so far in identifying individual grains. This is largely due to the presence of domain variants which results in closely spaced multiple Laue spots. However, a close inspection of the diffraction patterns does confirm the presence of significant variations in the response of grains to electrical loading (Fig. 3).« less

Authors:
; ; ; ; ; ;
Publication Date:
Research Org.:
Argonne National Lab. (ANL), Argonne, IL (United States)
Sponsoring Org.:
USDOE
OSTI Identifier:
971929
Report Number(s):
ANL/XSD/CP-118778
TRN: US1001420
DOE Contract Number:  
DE-AC02-06CH11357
Resource Type:
Conference
Resource Relation:
Conference: 5th International Conference on Synchrotron Radiation in Materials Science (SRMS 5); Jul. 30, 2006 - Aug. 2, 2006; Chicago, IL
Country of Publication:
United States
Language:
ENGLISH
Subject:
43 PARTICLE ACCELERATORS; ADVANCED PHOTON SOURCE; ALIGNMENT; DIFFRACTION; DISTRIBUTION; ELECTRIC FIELDS; EUROPEAN SYNCHROTRON RADIATION FACILITY; GEOMETRY; GRAIN BOUNDARIES; GRAIN SIZE; SAMPLING; STIMULI; SYNCHROTRON RADIATION; TEXTURE; X-RAY DIFFRACTION

Citation Formats

Varlioglu, M, Lienert, U, Ustundag, E, Bernier, J, Rogan, R C, Margulies, L, Poulsen, H, Iowa State Univ., and Risoe National Lab. Mesoscale response of individual grains of polycrystalline BaTiO{sub 3}to electrical loading.. United States: N. p., 2006. Web.
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Varlioglu, M, Lienert, U, Ustundag, E, Bernier, J, Rogan, R C, Margulies, L, Poulsen, H, Iowa State Univ., & Risoe National Lab. Mesoscale response of individual grains of polycrystalline BaTiO{sub 3}to electrical loading.. United States.
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Varlioglu, M, Lienert, U, Ustundag, E, Bernier, J, Rogan, R C, Margulies, L, Poulsen, H, Iowa State Univ., and Risoe National Lab. 2006. "Mesoscale response of individual grains of polycrystalline BaTiO{sub 3}to electrical loading.". United States.
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@article{osti_971929,
title = {Mesoscale response of individual grains of polycrystalline BaTiO{sub 3}to electrical loading.},
author = {Varlioglu, M and Lienert, U and Ustundag, E and Bernier, J and Rogan, R C and Margulies, L and Poulsen, H and Iowa State Univ. and Risoe National Lab.},
abstractNote = {Ranging from sub-grain structures to grain clusters, the mesoscale is critical in understanding the constitutive behavior of ferroelectrics. The interaction of domains with grain boundaries and grain-to-grain constraints largely determine the overall response of a ferroelectric. Unfortunately, the most severe paucity of quantitative data also exists at the mesoscale. The newly developed 3-D XRD technique offers a unique opportunity to study the response of ferroelectrics to external stimuli at this scale by allowing the investigation of individual grains within a polycrystal. To demonstrate the feasibility of 3-D XRD in ferroelectrics research for the first time, a polycrystalline BaTiO{sub 3} was subjected to quasi-statically cycled electric field. The experiments were performed at beamlines 1-ID-C of the Advanced Photon Source (APS) and ID-11 of the European Synchrotron Radiation Facility (ESRF), Grenoble, France. In both cases, nominally the same polycrystalline BaTiO{sub 3} samples (about 1 x 1 x 5 mm{sup 3}) were employed. The specimens were held upright in the geometry shown in Fig. 1 and run in transmission mode using {approx}80 keV X-rays. The direction of the electric field was perpendicular to the X-ray beam and it was stepped up to a maximum of {+-} 20 kV/cm, well above the nominal coercive field of the material ({approx}5 kV/cm). At each applied field value, the specimen was rotated perpendicular to the beam in 0.1{sup o} {omega} steps (Fig. 1) up to {+-} 45{sup o} (at ESRF) and {+-} 65{sup o} (at APS). The X-ray spot size was about 150 x 150 {micro}m{sup 2} at ESRF and 30 x 30 {micro}m{sup 2} at APS. Since the grain size of the BaTiO{sub 3} samples was measured to be {approx}20-30 {micro}m from SEM images, either sampling volume was large enough to capture a reasonable number of grains. The diffraction data were analyzed using the GRAINDEX software from Risoe. This analysis attempted to identify individual grains and track their response to electric field. In a parallel study, the macroscopic (polycrystalline) response of the material was obrained by integrating data within {+-} 10{sup o} {omega} around the {omega} = 0{sup o} position (perpendicular to the beam) and parallel to the electric field using the Fit2D software from ESRF (Fig. 2). The macroscopic behavior of the material (Fig. 2) was as expected from a polycrystalline ferroelectric: the electric field led to an increase of the 002 intensity due to domain alignment along the field direction. Fig. 2 also displays the MRD value (multiples of random distribution relative to an unpoled sample) obtained from this equation: MRD = 3I{sub 002}/(I{sub 002} + 2I{sub 200}). The MRD is a better measure of texture evolution due to domain reorientation and should be 1.0 for a random polycrystal. In Fig. 2, while the initial state of the specimen is not random (MRD {approx} 0.7), the applied field leads to significant domain re-alignment (MRD {approx} 1.5 at 2000 V). Unfortunately, the GRAINDEX analysis has not been successful so far in identifying individual grains. This is largely due to the presence of domain variants which results in closely spaced multiple Laue spots. However, a close inspection of the diffraction patterns does confirm the presence of significant variations in the response of grains to electrical loading (Fig. 3).},
doi = {},
url = {https://www.osti.gov/biblio/971929}, journal = {},
number = ,
volume = ,
place = {United States},
year = {Sun Jan 01 00:00:00 EST 2006},
month = {Sun Jan 01 00:00:00 EST 2006}
}
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