Correlating sampling and intensity statistics in nanoparticle diffraction experiments

Öztürk, Hande; Yan, Hanfei; Hill, John P.; Noyan, I. Cevdet

doi:10.1107/S1600576715011747

Title: Correlating sampling and intensity statistics in nanoparticle diffraction experiments

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Abstract

It is shown in a previous article [Öztürk, Yan, Hill & Noyan (2014).J. Appl. Cryst.47, 1016–1025] that the sampling statistics of diffracting particle populations within a polycrystalline ensemble depended on the size of the constituent crystallites: broad X-ray peak breadths enabled some nano-sized particles to contribute more than one diffraction spot to Debye–Scherrer rings. Here it is shown that the equations proposed by Alexander, Klug & Kummer [J. Appl. Phys.(1948),19, 742–753] (AKK) to link diffracting particle and diffracted intensity statistics are not applicable if the constituent crystallites of the powder are below 10 nm. In this size range, (i) the one-to-one correspondence between diffracting particles and Laue spots assumed in the AKK analysis is not satisfied, and (ii) the crystallographic correlation between Laue spots originating from the same grain invalidates the assumption that all diffracting plane normals are randomly oriented and uncorrelated. Such correlation produces unexpected results in the selection of diffracting grains. For example, three or more Laue spots from a given grain for a particular reflection can only be observed at certain wavelengths. In addition, correcting the diffracted intensity values by the traditional Lorentz term, 1/cos θ, to compensate for the variation of particles sampled within a reflectionmore »« less

Authors:

Öztürk, Hande ^[1]; Yan, Hanfei ^[2]; Hill, John P. ^[2]; Noyan, I. Cevdet ^[1]

Columbia Univ., New York, NY (United States)
Brookhaven National Lab. (BNL), Upton, NY (United States)

Publication Date:: Tue Jul 28 00:00:00 EDT 2015

Research Org.:: Brookhaven National Lab. (BNL), Upton, NY (United States)

Sponsoring Org.:: USDOE Office of Science (SC)

OSTI Identifier:: 1239776

Report Number(s):: BNL-108471-2015-JA
Journal ID: ISSN 1600-5767; JACGAR; R&D Project: LS001

Grant/Contract Number:: AC02-98CH10886

Resource Type:: Accepted Manuscript

Journal Name:: Journal of Applied Crystallography (Online)

Additional Journal Information:: Journal Name: Journal of Applied Crystallography (Online); Journal Volume: 48; Journal Issue: 4; Journal ID: ISSN 1600-5767

Publisher:: International Union of Crystallography

Country of Publication:: United States

Language:: English

Subject:: 36 MATERIALS SCIENCE; Diffraction; nanoparticle; Lorenz factor; X-rays, statistics

Citation Formats


                    Öztürk, Hande, Yan, Hanfei, Hill, John P., and Noyan, I. Cevdet. Correlating sampling and intensity statistics in nanoparticle diffraction experiments.  United States: N. p., 2015. 
Web.  doi:10.1107/S1600576715011747.

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                    Öztürk, Hande, Yan, Hanfei, Hill, John P., & Noyan, I. Cevdet. Correlating sampling and intensity statistics in nanoparticle diffraction experiments.  United States.  https://doi.org/10.1107/S1600576715011747

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                    Öztürk, Hande, Yan, Hanfei, Hill, John P., and Noyan, I. Cevdet. Tue .  
"Correlating sampling and intensity statistics in nanoparticle diffraction experiments".  United States.  https://doi.org/10.1107/S1600576715011747.  https://www.osti.gov/servlets/purl/1239776.

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@article{osti_1239776,

  title        = {Correlating sampling and intensity statistics in nanoparticle diffraction experiments},

  author       = {Öztürk, Hande and Yan, Hanfei and Hill, John P. and Noyan, I. Cevdet},

  abstractNote = {It is shown in a previous article [Öztürk, Yan, Hill & Noyan (2014).J. Appl. Cryst.47, 1016–1025] that the sampling statistics of diffracting particle populations within a polycrystalline ensemble depended on the size of the constituent crystallites: broad X-ray peak breadths enabled some nano-sized particles to contribute more than one diffraction spot to Debye–Scherrer rings. Here it is shown that the equations proposed by Alexander, Klug & Kummer [J. Appl. Phys.(1948),19, 742–753] (AKK) to link diffracting particle and diffracted intensity statistics are not applicable if the constituent crystallites of the powder are below 10 nm. In this size range, (i) the one-to-one correspondence between diffracting particles and Laue spots assumed in the AKK analysis is not satisfied, and (ii) the crystallographic correlation between Laue spots originating from the same grain invalidates the assumption that all diffracting plane normals are randomly oriented and uncorrelated. Such correlation produces unexpected results in the selection of diffracting grains. For example, three or more Laue spots from a given grain for a particular reflection can only be observed at certain wavelengths. In addition, correcting the diffracted intensity values by the traditional Lorentz term, 1/cos θ, to compensate for the variation of particles sampled within a reflection band does not maintain fidelity to the number of poles contributing to the diffracted signal. A new term, cos θB/cos θ, corrects this problem.},

  doi          = {10.1107/S1600576715011747},

  journal      = {Journal of Applied Crystallography (Online)},

  number       = 4,

  volume       = 48,

  place        = {United States},

  year         = {Tue Jul 28 00:00:00 EDT 2015},

  month        = {Tue Jul 28 00:00:00 EDT 2015}

}

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