Revealing inconsistencies in X-ray width methods for nanomaterials
Abstract
Since the landmark development of the Scherrer method a century ago, multiple generations of width methods for X-ray diffraction originated to non-invasively and rapidly characterize the property-controlling sizes of nanoparticles, nanowires, and nanocrystalline materials. Yet, the predictive power of this approach suffers from inconsistencies among numerous methods and from misinterpretations of the findings. Thus, we systematically evaluated twenty-two width methods on a representative nanomaterial subjected to thermal and mechanical loads. To bypass experimental complications and enable a 1:1 comparison between ground truths and the results of width methods, we produced virtual X-ray diffractograms from atomistic simulations. These simulations realistically captured the trends that we observed in experimental synchrotron diffraction. To comprehensively survey the width methods and to guide future investigations, we introduced a consistent, descriptive nomenclature. Surprisingly, our results demonstrated that popular width methods, especially the Williamson–Hall methods, can produce dramatically incorrect trends. We also showed that the simple Scherrer methods and the rare Energy methods can well characterize unloaded and loaded states, respectively. Overall, this work improved the utility of X-ray diffraction in experimentally evaluating a variety of nanomaterials by guiding the selection and interpretation of width methods.
- Publication Date:
- Research Org.:
- Sandia National Lab. (SNL-NM), Albuquerque, NM (United States)
- Sponsoring Org.:
- USDOE Office of Science (SC), Basic Energy Sciences (BES); USDOE National Nuclear Security Administration (NNSA)
- OSTI Identifier:
- 1574484
- Alternate Identifier(s):
- OSTI ID: 1576028
- Report Number(s):
- SAND-2019-13701J
Journal ID: ISSN 2040-3364; NANOHL; 681299; TRN: US2001391
- Grant/Contract Number:
- AC04-94AL85000; NA0003525
- Resource Type:
- Accepted Manuscript
- Journal Name:
- Nanoscale
- Additional Journal Information:
- Journal Volume: 11; Journal Issue: 46; Journal ID: ISSN 2040-3364
- Publisher:
- Royal Society of Chemistry
- Country of Publication:
- United States
- Language:
- English
- Subject:
- 36 MATERIALS SCIENCE
Citation Formats
Kunka, Cody, Boyce, Brad L., Foiles, Stephen M., and Dingreville, Rémi. Revealing inconsistencies in X-ray width methods for nanomaterials. United States: N. p., 2019.
Web. doi:10.1039/C9NR08268A.
Kunka, Cody, Boyce, Brad L., Foiles, Stephen M., & Dingreville, Rémi. Revealing inconsistencies in X-ray width methods for nanomaterials. United States. doi:10.1039/C9NR08268A.
Kunka, Cody, Boyce, Brad L., Foiles, Stephen M., and Dingreville, Rémi. Thu .
"Revealing inconsistencies in X-ray width methods for nanomaterials". United States. doi:10.1039/C9NR08268A. https://www.osti.gov/servlets/purl/1574484.
@article{osti_1574484,
title = {Revealing inconsistencies in X-ray width methods for nanomaterials},
author = {Kunka, Cody and Boyce, Brad L. and Foiles, Stephen M. and Dingreville, Rémi},
abstractNote = {Since the landmark development of the Scherrer method a century ago, multiple generations of width methods for X-ray diffraction originated to non-invasively and rapidly characterize the property-controlling sizes of nanoparticles, nanowires, and nanocrystalline materials. Yet, the predictive power of this approach suffers from inconsistencies among numerous methods and from misinterpretations of the findings. Thus, we systematically evaluated twenty-two width methods on a representative nanomaterial subjected to thermal and mechanical loads. To bypass experimental complications and enable a 1:1 comparison between ground truths and the results of width methods, we produced virtual X-ray diffractograms from atomistic simulations. These simulations realistically captured the trends that we observed in experimental synchrotron diffraction. To comprehensively survey the width methods and to guide future investigations, we introduced a consistent, descriptive nomenclature. Surprisingly, our results demonstrated that popular width methods, especially the Williamson–Hall methods, can produce dramatically incorrect trends. We also showed that the simple Scherrer methods and the rare Energy methods can well characterize unloaded and loaded states, respectively. Overall, this work improved the utility of X-ray diffraction in experimentally evaluating a variety of nanomaterials by guiding the selection and interpretation of width methods.},
doi = {10.1039/C9NR08268A},
journal = {Nanoscale},
number = 46,
volume = 11,
place = {United States},
year = {2019},
month = {11}
}
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Works referenced in this record:
X-Ray and Neutron Diffraction Measurements of Dislocation Density and Subgrain Size in a Friction-Stir-Welded Aluminum Alloy
journal, August 2009
- Woo, Wanchuck; Ungár, Tamás; Feng, Zhili
- Metallurgical and Materials Transactions A, Vol. 41, Issue 5
X-ray line broadening from filed aluminium and wolfram
journal, January 1953
- Williamson, G. K.; Hall, W. H.
- Acta Metallurgica, Vol. 1, Issue 1
VI. Lorentz-Faktor und Intensitätsverteilung in Debye-Scherrer-Ringen
journal, January 1926
- Laue, Μ. v.
- Zeitschrift für Kristallographie - Crystalline Materials, Vol. 64, Issue 1-6
Virtual diffraction analysis of Ni [0 1 0] symmetric tilt grain boundaries
journal, June 2013
- Coleman, S. P.; Spearot, D. E.; Capolungo, L.
- Modelling and Simulation in Materials Science and Engineering, Vol. 21, Issue 5
X-ray diffraction line broadening analysis of nanostructured nickel powder
journal, September 2017
- Bahramyan, M.; Hossein Nedjad, S.
- Physics of Metals and Metallography, Vol. 118, Issue 9
X-ray analysis of ZnO nanoparticles by Williamson–Hall and size–strain plot methods
journal, January 2011
- Khorsand Zak, A.; Abd. Majid, W. H.; Abrishami, M. E.
- Solid State Sciences, Vol. 13, Issue 1
Microstructural evaluation of CoAl 2 O 4 nanoparticles by Williamson–Hall and size–strain plot methods
journal, January 2018
- Irfan, H.; Racik K., Mohamed; Anand, S.
- Journal of Asian Ceramic Societies, Vol. 6, Issue 1
Pitfalls in the characterization of nanoporous and nanosized materials
journal, January 2011
- Weidenthaler, Claudia
- Nanoscale, Vol. 3, Issue 3
Validating grain size analysis from X-ray line broadening: A virtual experiment
journal, July 2008
- Markmann, J.; Yamakov, V.; Weissmüller, J.
- Scripta Materialia, Vol. 59, Issue 1
The Separation of Cold‐Work Distortion and Particle Size Broadening in X‐Ray Patterns
journal, April 1952
- Warren, B. E.; Averbach, B. L.
- Journal of Applied Physics, Vol. 23, Issue 4
The role of copper twin boundaries in cryogenic indentation-induced grain growth
journal, January 2014
- Brons, J. G.; Hardwick, J. A.; Padilla, H. A.
- Materials Science and Engineering: A, Vol. 592
X-ray diffraction line broadening: modeling and applications to high-Tc superconductors
journal, May 1993
- Balzar, D.
- Journal of Research of the National Institute of Standards and Technology, Vol. 98, Issue 3
Fast Parallel Algorithms for Short-Range Molecular Dynamics
journal, March 1995
- Plimpton, Steve
- Journal of Computational Physics, Vol. 117, Issue 1
Tutorial on Powder X-ray Diffraction for Characterizing Nanoscale Materials
journal, July 2019
- Holder, Cameron F.; Schaak, Raymond E.
- ACS Nano, Vol. 13, Issue 7
Detecting rare, abnormally large grains by x-ray diffraction
journal, July 2015
- Boyce, B. L.; Furnish, T. A.; Padilla, H. A.
- Journal of Materials Science, Vol. 50, Issue 20
Mechanical properties of stabilized nanocrystalline FCC metals
journal, September 2019
- Spearot, Douglas E.; Tucker, Garritt J.; Gupta, Ankit
- Journal of Applied Physics, Vol. 126, Issue 11
Dislocations and grain size in ball-milled iron powder
journal, September 1996
- Révész, Á.; Ungár, T.; Borbély, A.
- Nanostructured Materials, Vol. 7, Issue 7
Dislocation Characterization by the Direct-fitting/modified Williamson–Hall (DF/mWH) Method in Cold Worked Ferritic Steel
journal, January 2019
- Takaki, Setsuo; Masumura, Takuro; Tsuchiyama, Toshihiro
- ISIJ International, Vol. 59, Issue 3
The effect of dislocation contrast on x‐ray line broadening: A new approach to line profile analysis
journal, November 1996
- Ungár, T.; Borbély, A.
- Applied Physics Letters, Vol. 69, Issue 21
Formation of annealing twins in f.c.c. crystals
journal, June 1997
- Mahajan, S.
- Acta Materialia, Vol. 45, Issue 6
Line broadening analysis using integral breadth methods: a critical review
journal, May 2004
- Scardi, P.; Leoni, M.; Delhez, R.
- Journal of Applied Crystallography, Vol. 37, Issue 3
The embedded-atom method: a review of theory and applications
journal, March 1993
- Daw, Murray S.; Foiles, Stephen M.; Baskes, Michael I.
- Materials Science Reports, Vol. 9, Issue 7-8
The diffraction of X rays by distorted crystal aggregates - I
journal, May 1944
- Stokes, A. R.; Wilson, A. J. C.
- Proceedings of the Physical Society, Vol. 56, Issue 3
Influence of dislocations and grain boundaries on diffraction line profiles of nano-crystalline materials: A numerical study
journal, January 2020
- Naveen Kumar, N.; Mani Krishna, K. V.; Chandra, Sagar
- Computational Materials Science, Vol. 171
Williamson-Hall analysis in estimation of lattice strain in nanometer-sized ZnO particles
journal, January 2012
- Mote, Vd; Purushotham, Y.; Dole, Bn
- Journal of Theoretical and Applied Physics, Vol. 6, Issue 1
Scherrer after sixty years: A survey and some new results in the determination of crystallite size
journal, April 1978
- Langford, J. I.; Wilson, A. J. C.
- Journal of Applied Crystallography, Vol. 11, Issue 2
Nanomechanics of Hall–Petch relationship in nanocrystalline materials
journal, August 2009
- Pande, C. S.; Cooper, K. P.
- Progress in Materials Science, Vol. 54, Issue 6
Metrological characterization of X-ray diffraction methods at different acquisition geometries for determination of crystallite size in nano-scale materials
journal, November 2013
- Uvarov, Vladimir; Popov, Inna
- Materials Characterization, Vol. 85
Estimating grain-size distributions in nanocrystalline materials from X-ray diffraction profile analysis
journal, March 1998
- Kril, C. E.; Birringer, R.
- Philosophical Magazine A, Vol. 77, Issue 3
Probing the limits of metal plasticity with molecular dynamics simulations
journal, September 2017
- Zepeda-Ruiz, Luis A.; Stukowski, Alexander; Oppelstrup, Tomas
- Nature, Vol. 550, Issue 7677
The contrast factors of dislocations in cubic crystals: the dislocation model of strain anisotropy in practice
journal, October 1999
- Ungár, T.; Dragomir, I.; Révész, Á.
- Journal of Applied Crystallography, Vol. 32, Issue 5
The Scherrer equation versus the 'Debye-Scherrer equation'
journal, August 2011
- Holzwarth, Uwe; Gibson, Neil
- Nature Nanotechnology, Vol. 6, Issue 9
Reliability of the Simplified Integral-Breadth Methods in Diffraction Line-Broadening Analysis
journal, February 1996
- Balzar, D.; Popović, S.
- Journal of Applied Crystallography, Vol. 29, Issue 1
Nanoscale Hard X-Ray Microscopy Methods for Materials Studies
journal, July 2013
- Holt, Martin; Harder, Ross; Winarski, Robert
- Annual Review of Materials Research, Vol. 43, Issue 1
Dislocations and Grain Size in Electrodeposited Nanocrystalline Ni Determined by the Modified Williamson–Hall and Warren–Averbach Procedures
journal, August 1998
- Ungár, T.; Révész, Á ;.; Borbély, A.
- Journal of Applied Crystallography, Vol. 31, Issue 4
Correlating deformation mechanisms with X-ray diffraction phenomena in nanocrystalline metals using atomistic simulations
journal, November 2018
- Foley, Daniel J.; Coleman, Shawn P.; Tschopp, Mark A.
- Computational Materials Science, Vol. 154
Development of physically based atomistic microstructures: The effect on the mechanical response of polycrystals
journal, February 2017
- Gruber, Jacob; Lim, Hojun; Abdeljawad, Fadi
- Computational Materials Science, Vol. 128
Structural changes in iron powder during ball milling
journal, September 2010
- Khatirkar, R. K.; Murty, B. S.
- Materials Chemistry and Physics, Vol. 123, Issue 1
Fatigue-driven acceleration of abnormal grain growth in nanocrystalline wires
journal, January 2019
- Foiles, Stephen M.; Abdeljawad, Fadi; Moore, Alexander
- Modelling and Simulation in Materials Science and Engineering, Vol. 27, Issue 2
Modified Scherrer Equation to Estimate More Accurately Nano-Crystallite Size Using XRD
journal, January 2012
- Monshi, Ahmad; Foroughi, Mohammad Reza; Monshi, Mohammad Reza
- World Journal of Nano Science and Engineering, Vol. 02, Issue 03
Extended pseudo-Voigt function for approximating the Voigt profile
journal, December 2000
- Ida, T.; Ando, M.; Toraya, H.
- Journal of Applied Crystallography, Vol. 33, Issue 6
A Computational Algorithm to Produce Virtual X-ray and Electron Diffraction Patterns from Atomistic Simulations
journal, January 2014
- Coleman, Shawn P.; Sichani, Mehrdad M.; Spearot, Douglas E.
- JOM, Vol. 66, Issue 3
Untangling dislocation and grain boundary mediated plasticity in nanocrystalline nickel
journal, February 2014
- Lohmiller, Jochen; Grewer, Manuel; Braun, Christian
- Acta Materialia, Vol. 65
Small Angle X-ray Scattering for Nanoparticle Research
journal, April 2016
- Li, Tao; Senesi, Andrew J.; Lee, Byeongdu
- Chemical Reviews, Vol. 116, Issue 18
Visualization and analysis of atomistic simulation data with OVITO–the Open Visualization Tool
journal, December 2009
- Stukowski, Alexander
- Modelling and Simulation in Materials Science and Engineering, Vol. 18, Issue 1
The determination of density and distribution of dislocations in deformed single crystals from broadened X-ray diffraction profiles
journal, June 1970
- Wilkens, M.
- Physica Status Solidi (a), Vol. 2, Issue 2
Catastrophic vs Gradual Collapse of Thin-Walled Nanocrystalline Ni Hollow Cylinders As Building Blocks of Microlattice Structures
journal, October 2011
- Lian, Jie; Jang, Dongchan; Valdevit, Lorenzo
- Nano Letters, Vol. 11, Issue 10
Size effect on the ferroelectric phase transition in SrBi2Ta2O9 nanoparticles
journal, July 2003
- Yu, T.; Shen, Z. X.; Toh, W. S.
- Journal of Applied Physics, Vol. 94, Issue 1
Calculation of x-ray spectra for nanocrystalline materials
journal, January 2005
- Derlet, P. M.; Van Petegem, S.; Van Swygenhoven, H.
- Physical Review B, Vol. 71, Issue 2
Structural transformations of bioactive glass 45S5 with thermal treatments
journal, June 2007
- Lefebvre, L.; Chevalier, J.; Gremillard, L.
- Acta Materialia, Vol. 55, Issue 10
A new facile synthesis of ultra fine magnesium oxide nanowires and optical properties
journal, October 2012
- Al-Ghamdi, Ahmed A.; Al-Hazmi, Faten; Alnowaiser, Fowzia
- Journal of Electroceramics, Vol. 29, Issue 3
Estimation of lattice strain in nanocrystalline RuO 2 by Williamson–Hall and size–strain plot methods
journal, January 2016
- Sivakami, R.; Dhanuskodi, S.; Karvembu, R.
- Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy, Vol. 152
Combining Atomistic Simulation and X-ray Diffraction for the Characterization of Nanostructures: A Case Study on Fivefold Twinned Nanowires
journal, January 2014
- Niekiel, Florian; Bitzek, Erik; Spiecker, Erdmann
- ACS Nano, Vol. 8, Issue 2
Atomistic origin of microstrain broadening in diffraction data of nanocrystalline solids
journal, March 2009
- Stukowski, A.; Markmann, J.; Weissmüller, J.
- Acta Materialia, Vol. 57, Issue 5
Separation of particle size and lattice strain in integral breadth measurements
journal, February 1966
- Halder, N. C.; Wagner, C. N. J.
- Acta Crystallographica, Vol. 20, Issue 2