Comparing Scanning Electron Microscope and Transmission Electron Microscope Grain Mapping Techniques Applied to Well-Defined and Highly Irregular Nanoparticles

Mariano, Ruperto G.; Yau, Allison; McKeown, Joseph T.; Kumar, Mukul; Kanan, Matthew W.

doi:10.1021/acsomega.9b03505

Title: Comparing Scanning Electron Microscope and Transmission Electron Microscope Grain Mapping Techniques Applied to Well-Defined and Highly Irregular Nanoparticles

Journal Article · Fri Feb 07 00:00:00 EST 2020 · ACS Omega

DOI:https://doi.org/10.1021/acsomega.9b03505· OSTI ID:1600045

^[1]; Yau, Allison ^[1]; McKeown, Joseph T. ^[2]; Kumar, Mukul ^[3];

^[1]

Department of Chemistry, Stanford University, Stanford, California 94305, United States
Materials Science Division, Lawrence Livermore National Laboratory, Livermore, California 94550, United States
Materials Engineering Division, Lawrence Livermore National Laboratory, Livermore, California 94550, United States

Investigating how grain structure affects the functional properties of nanoparticles requires a robust method for nanoscale grain mapping. In this study, we directly compare the grain mapping ability of transmission Kikuchi diffraction (TKD) in a scanning electron microscope to automated crystal orientation mapping (ACOM) in a transmission electron microscope across multiple nanoparticle materials. Analysis of well-defined Au, ZnO, and ZnSe nanoparticles showed that the grain orientations and GB geometries obtained by TKD are accurate and match those obtained by ACOM. For more complex polycrystalline Cu nanostructures, TKD provided an interpretable grain map whereas ACOM, with or without precession electron diffraction, yielded speckled, uninterpretable maps with orientation errors. Acquisition times for TKD were generally shorter than those for ACOM. Our results validate the use of TKD for characterizing grain orientation and grain boundary distributions in nanoparticles, providing a framework for the broader exploration of how microstructure influences nanoparticle properties.

View Journal Article

Cite

Export

Save

Research Organization:: Stanford Univ., CA (United States); Lawrence Livermore National Laboratory (LLNL), Livermore, CA (United States)

Sponsoring Organization:: USDOE Office of Science (SC), Basic Energy Sciences (BES); National Science Foundation (NSF); USDOE National Nuclear Security Administration (NNSA)

Grant/Contract Number:: AC52-07NA27344; CHE-1565945; ECCS-1542152

OSTI ID:: 1600045

Alternate ID(s):: OSTI ID: 1600656; OSTI ID: 1647448

Report Number(s):: LLNL-JRNL-752167

Journal Information:: ACS Omega, Journal Name: ACS Omega Vol. 5 Journal Issue: 6; ISSN 2470-1343

Publisher:: American Chemical Society (ACS)Copyright Statement

Country of Publication:: United States

Language:: English

Citation Metrics:

Cited by: 7 works

Citation information provided by
Web of Science

References (58)

Effects of Crystal Phase Mixing on the Electrical Properties of InAs Nanowires Thelander, Claes; Caroff, Philippe; Plissard, Sébastien Nano Letters, Vol. 11, Issue 6 https://doi.org/10.1021/nl2008339	journal	June 2011
Retrieving overlapping crystals information from TEM nano-beam electron diffraction patterns: ACOM-TEM & OVERLAPPING CRYSTALS Valery, A.; Rauch, E. F.; ClÉMent, L. Journal of Microscopy, Vol. 268, Issue 2 https://doi.org/10.1111/jmi.12599	journal	July 2017
Spatial Control of Multiphoton Electron Excitations in InAs Nanowires by Varying Crystal Phase and Light Polarization Mårsell, Erik; Boström, Emil; Harth, Anne Nano Letters, Vol. 18, Issue 2 https://doi.org/10.1021/acs.nanolett.7b04267	journal	January 2018
Multiscale Phase Mapping of LiFePO ₄ -Based Electrodes by Transmission Electron Microscopy and Electron Forward Scattering Diffraction Robert, Donatien; Douillard, Thierry; Boulineau, Adrien ACS Nano, Vol. 7, Issue 12 https://doi.org/10.1021/nn4043964	journal	November 2013
In-Depth View of the Structure and Growth of SnO ₂ Nanowires and Nanobrushes Stuckert, Erin P.; Geiss, Roy H.; Miller, Christopher J. ACS Applied Materials & Interfaces, Vol. 8, Issue 34 https://doi.org/10.1021/acsami.6b06676	journal	August 2016
Dealing With Multiple Grains in TEM Lamellae Thickness for Microstructure Analysis Using Scanning Precession Electron Diffraction Valery, A.; Rauch, E. F.; Pofelski, A. Microscopy and Microanalysis, Vol. 21, Issue S3 https://doi.org/10.1017/S143192761500700X	journal	August 2015
Electroreduction of carbon monoxide to liquid fuel on oxide-derived nanocrystalline copper Li, Christina W.; Ciston, Jim; Kanan, Matthew W. Nature, Vol. 508, Issue 7497 https://doi.org/10.1038/nature13249	journal	April 2014
Li Electrochemical Tuning of Metal Oxide for Highly Selective CO ₂ Reduction Jiang, Kun; Wang, Han; Cai, Wen-Bin ACS Nano, Vol. 11, Issue 6 https://doi.org/10.1021/acsnano.7b03029	journal	May 2017
Nanoscale electrochemical movies and synchronous topographical mapping of electrocatalytic materials Bentley, Cameron L.; Unwin, Patrick R. Faraday Discussions, Vol. 210 https://doi.org/10.1039/C8FD00028J	journal	January 2018
Electron transport in indium arsenide nanowires Dayeh, Shadi A. Semiconductor Science and Technology, Vol. 25, Issue 2 https://doi.org/10.1088/0268-1242/25/2/024004	journal	January 2010
A stable multiply twinned decahedral gold nanoparticle with a barrel-like shape Santiago, Ulises; Velázquez-Salazar, J. Jesus; Sanchez, John Eder Surface Science, Vol. 644 https://doi.org/10.1016/j.susc.2015.09.015	journal	February 2016
Grain orientations and grain boundaries in tungsten nonotendril fuzz grown under divertor-like conditions Parish, Chad M.; Wang, Kun; Doerner, Russel P. Scripta Materialia, Vol. 127 https://doi.org/10.1016/j.scriptamat.2016.09.018	journal	January 2017
Catalyst-Directed Crystallographic Orientation Control of GaN Nanowire Growth Kuykendall, Tevye R.; Altoe, M. Virginia P.; Ogletree, D. Frank Nano Letters, Vol. 14, Issue 12 https://doi.org/10.1021/nl502079v	journal	November 2014
Specimen-thickness effects on transmission Kikuchi patterns in the scanning electron microscope: SPECIMEN-THICKNESS EFFECTS ON TRANSMISSION KIKUCHI PATTERNS IN SEM Rice, K. P.; Keller, R. R.; Stoykovich, M. P. Journal of Microscopy, Vol. 254, Issue 3 https://doi.org/10.1111/jmi.12124	journal	March 2014
Scanning precession electron tomography for three-dimensional nanoscale orientation imaging and crystallographic analysis Eggeman, Alexander S.; Krakow, Robert; Midgley, Paul A. Nature Communications, Vol. 6, Issue 1 https://doi.org/10.1038/ncomms8267	journal	June 2015
A systematic comparison of on-axis and off-axis transmission Kikuchi diffraction Niessen, F.; Burrows, A.; Fanta, A. Bastos da Silva Ultramicroscopy, Vol. 186 https://doi.org/10.1016/j.ultramic.2017.12.017	journal	March 2018
Kinetically Controlled Growth of Gold Nanoplates and Nanorods via a One-Step Seed-Mediated Method Hong, Soonchang; Acapulco, Jesus A. I. Jr.; Jang, Hee-Jeong Bulletin of the Korean Chemical Society, Vol. 35, Issue 6 https://doi.org/10.5012/bkcs.2014.35.6.1737	journal	June 2014
Conductivity of ZnO Nanowires, Nanoparticles, and Thin Films Using Time-Resolved Terahertz Spectroscopy ^† Baxter, Jason B.; Schmuttenmaer, Charles A. The Journal of Physical Chemistry B, Vol. 110, Issue 50 https://doi.org/10.1021/jp064399a	journal	December 2006
Identifying and mapping the polytypes and orientation relationships in ZnO/CdSe core–shell nanowire arrays Consonni, Vincent; Rapenne, Laetitia; Renou, Gilles Nanotechnology, Vol. 27, Issue 44 https://doi.org/10.1088/0957-4484/27/44/445712	journal	September 2016
Orientation mapping of nanostructured materials using transmission Kikuchi diffraction in the scanning electron microscope Trimby, Patrick W. Ultramicroscopy, Vol. 120 https://doi.org/10.1016/j.ultramic.2012.06.004	journal	September 2012
Symmetry-Broken Atom Configurations at Grain Boundaries and Oxygen Evolution Electrocatalysis in Perovskite Oxides Heo, Yoon; Choi, Seungkyu; Bak, Jumi Advanced Energy Materials, Vol. 8, Issue 34 https://doi.org/10.1002/aenm.201802481	journal	October 2018
Oriented epitaxial TiO ₂ nanowires for water splitting Hou, Wenting; Cortez, Pablo; Wuhrer, Richard Nanotechnology, Vol. 28, Issue 26 https://doi.org/10.1088/1361-6528/aa7356	journal	June 2017
On the influence of the metal loading on the structure of carbon-supported PtRu catalysts and their electrocatalytic activities in CO and methanol electrooxidation Gavrilov, Alexei N.; Savinova, Elena R.; Simonov, Pavel A. Physical Chemistry Chemical Physics, Vol. 9, Issue 40 https://doi.org/10.1039/b707598g	journal	January 2007
Ultraflat Transparent Gold Nanoplates-Ideal Substrates for Tip-Enhanced Raman Scattering Experiments Deckert-Gaudig, Tanja; Deckert, Volker Small, Vol. 5, Issue 4 https://doi.org/10.1002/smll.200801237	journal	February 2009
Spontaneous Polarization-Induced Nanohelixes, Nanosprings, and Nanorings of Piezoelectric Nanobelts Kong, Xiang Yang; Wang, Zhong Lin Nano Letters, Vol. 3, Issue 12 https://doi.org/10.1021/nl034463p	journal	December 2003
Deformation Microstructures in Individual Cold Sprayed Al-Cu Alloy Particles Studied via Precession Electron Diffraction and Transmission Kikuchi Diffraction Liu, Tian; Leazer, Jeremy D.; Brewer, Luke N. Microscopy and Microanalysis, Vol. 24, Issue S1 https://doi.org/10.1017/S1431927618011388	journal	August 2018
Orientation precision of TEM-based orientation mapping techniques Morawiec, A.; Bouzy, E.; Paul, H. Ultramicroscopy, Vol. 136 https://doi.org/10.1016/j.ultramic.2013.08.008	journal	January 2014
Transmission EBSD from 10 nm domains in a scanning electron microscope: TRANSMISSION EBSD IN THE SEM Keller, R. R.; Geiss, R. H. Journal of Microscopy, Vol. 245, Issue 3 https://doi.org/10.1111/j.1365-2818.2011.03566.x	journal	November 2011
Nanoscale Structure Dynamics within Electrocatalytic Materials Bentley, Cameron L.; Kang, Minkyung; Unwin, Patrick R. Journal of the American Chemical Society, Vol. 139, Issue 46 https://doi.org/10.1021/jacs.7b09355	journal	October 2017
Automated crystal orientation and phase mapping in TEM Rauch, E. F.; Véron, M. Materials Characterization, Vol. 98 https://doi.org/10.1016/j.matchar.2014.08.010	journal	December 2014
Morphologies of tungsten nanotendrils grown under helium exposure Wang, Kun; Doerner, R. P.; Baldwin, M. J. Scientific Reports, Vol. 7, Issue 1 https://doi.org/10.1038/srep42315	journal	February 2017
A Direct Grain-Boundary-Activity Correlation for CO Electroreduction on Cu Nanoparticles Feng, Xiaofeng; Jiang, Kaili; Fan, Shoushan ACS Central Science, Vol. 2, Issue 3 https://doi.org/10.1021/acscentsci.6b00022	journal	March 2016
Oxidation of etched Zn foil for the formation of ZnO nanostructure Tan, W. K.; Razak, K. Abdul; Ibrahim, K. Journal of Alloys and Compounds, Vol. 509, Issue 24 https://doi.org/10.1016/j.jallcom.2011.03.055	journal	June 2011
Correlation of Electron Diffraction between t-EBSD in the SEM, CBED in the TEM and ACOM using ASTAR in the TEM using GaN Nanowires Geiss, Roy H. Microscopy and Microanalysis, Vol. 21, Issue S3 https://doi.org/10.1017/S1431927615007035	journal	August 2015
Grain boundary mediated hydriding phase transformations in individual polycrystalline metal nanoparticles Alekseeva, Svetlana; Fanta, Alice Bastos da Silva; Iandolo, Beniamino Nature Communications, Vol. 8, Issue 1 https://doi.org/10.1038/s41467-017-00879-9	journal	October 2017
ZnSe Heterocrystalline Junctions Based on Zinc Blende−Wurtzite Polytypism Jin, Lei; Wang, Jianbo; Jia, Shuangfeng The Journal of Physical Chemistry C, Vol. 114, Issue 3 https://doi.org/10.1021/jp909182e	journal	January 2010
Selective increase in CO ₂ electroreduction activity at grain-boundary surface terminations Mariano, Ruperto G.; McKelvey, Kim; White, Henry S. Science, Vol. 358, Issue 6367 https://doi.org/10.1126/science.aao3691	journal	November 2017
Nonradiative Step Facets in Semiconductor Nanowires Sanchez, Ana M.; Zhang, Yunyan; Tait, Edward W. Nano Letters, Vol. 17, Issue 4 https://doi.org/10.1021/acs.nanolett.7b00123	journal	March 2017
Artifacts induced in metallic glasses during TEM sample preparation Sun, B. B.; Wang, Y. B.; Wen, J. Scripta Materialia, Vol. 53, Issue 7 https://doi.org/10.1016/j.scriptamat.2005.06.007	journal	October 2005
Grain-Boundary-Dependent CO ₂ Electroreduction Activity Feng, Xiaofeng; Jiang, Kaili; Fan, Shoushan Journal of the American Chemical Society, Vol. 137, Issue 14 https://doi.org/10.1021/ja5130513	journal	April 2015
The structure of high-angle grain boundaries Brandon, D. G. Acta Metallurgica, Vol. 14, Issue 11 https://doi.org/10.1016/0001-6160(66)90168-4	journal	November 1966
Transmission EBSD in the Scanning Electron Microscope Geiss, Roy H.; Rice, Katherine P.; Keller, Robert R. Microscopy Today, Vol. 21, Issue 3 https://doi.org/10.1017/S1551929513000503	journal	May 2013
Characterization of the inner structure of porous TiO 2 nanoparticle films in dye sensitive solar cells (DSSC) by focused ion beam (FIB) tomography and transmission Kikuchi diffraction (TKD) in the scanning electron microscope (SEM) Wollschläger, Nicole; Palasse, Laurie; Häusler, Ines Materials Characterization, Vol. 131 https://doi.org/10.1016/j.matchar.2017.06.030	journal	September 2017
Characterization of the near-surface nanocrystalline microstructure of ultrasonically treated Ti-6Al-4V using ASTAR™/precession electron diffraction technique Ghamarian, I.; Samimi, P.; Telang, A. Materials Science and Engineering: A, Vol. 688 https://doi.org/10.1016/j.msea.2017.02.029	journal	March 2017
Grain boundary engineering in electrospun ZnO nanostructures as promising photocatalysts Senthamizhan, Anitha; Balusamy, Brabu; Aytac, Zeynep CrystEngComm, Vol. 18, Issue 34 https://doi.org/10.1039/C6CE00693K	journal	January 2016
A new titanium alloy with a combination of high strength, high strain hardening and improved ductility Sun, F.; Zhang, J. Y.; Marteleur, M. Scripta Materialia, Vol. 94 https://doi.org/10.1016/j.scriptamat.2014.09.005	journal	January 2015
Orientation and phase mapping in the transmission electron microscope using precession-assisted diffraction spot recognition: state-of-the-art results: REVIEW OF PACOM (ASTAR) APPLICATION Viladot, D.; VÉRon, M.; Gemmi, M. Journal of Microscopy, Vol. 252, Issue 1 https://doi.org/10.1111/jmi.12065	journal	July 2013
On the depth resolution of transmission Kikuchi diffraction (TKD) analysis Liu, Junliang; Lozano-Perez, Sergio; Wilkinson, Angus J. Ultramicroscopy, Vol. 205 https://doi.org/10.1016/j.ultramic.2019.06.003	journal	October 2019
Coupled microstructural observations and local texture measurements with an automated crystallographic orientation mapping tool attached to a tem Rauch, E. F.; Veron, M. Materialwissenschaft und Werkstofftechnik, Vol. 36, Issue 10, p. 552-556 https://doi.org/10.1002/mawe.200500923	journal	October 2005
New structure in refractory high-entropy alloys Lilensten, L.; Couzinié, J. P.; Perrière, L. Materials Letters, Vol. 132 https://doi.org/10.1016/j.matlet.2014.06.064	journal	October 2014
{113} Twinned ZnSe Bicrystal Nanobelts Filled with <111> Twinnings Jin, Lei; Wang, Jianbo; Cao, Guangyi The Journal of Physical Chemistry C, Vol. 112, Issue 13 https://doi.org/10.1021/jp710800w	journal	March 2008
Electrocatalytic Activity and Interconnectivity of Pt Nanoparticles on Multiwalled Carbon Nanotubes for Fuel Cells Wang, Shuangyin; Jiang, San Ping; White, T. J. The Journal of Physical Chemistry C, Vol. 113, Issue 43 https://doi.org/10.1021/jp906923z	journal	October 2009
Planar defects and phase transformation in ZnSe nanosaws Wang, Y. Q.; Philipose, U.; Ruda, H. Journal of Materials Science: Materials in Electronics, Vol. 17, Issue 12 https://doi.org/10.1007/s10854-006-9006-6	journal	August 2006
Application of Transmitted Kikuchi Diffraction in Studying Nano-oxide and Ultrafine Metallic Grains Abbasi, Majid; Kim, Dong-Ik; Guim, Hwan-Uk ACS Nano, Vol. 9, Issue 11 https://doi.org/10.1021/acsnano.5b04296	journal	October 2015
High-performance nanostructured thermoelectric materials Li, Jing-Feng; Liu, Wei-Shu; Zhao, Li-Dong NPG Asia Materials, Vol. 2, Issue 4 https://doi.org/10.1038/asiamat.2010.138	journal	October 2010
The synthesis of high yield Au nanoplate and optimized optical properties Ni, Yuan; Kan, Caixia; Xu, Juan Superlattices and Microstructures, Vol. 114 https://doi.org/10.1016/j.spmi.2017.12.021	journal	February 2018
Exploring transmission Kikuchi diffraction using a Timepix detector Vespucci, S.; Winkelmann, A.; Mingard, K. Journal of Instrumentation, Vol. 12, Issue 02 https://doi.org/10.1088/1748-0221/12/02/C02075	journal	February 2017
Density and Energy Distribution of Interface States in the Grain Boundaries of Polysilicon Nanowire Amit, Iddo; Englander, Danny; Horvitz, Dror Nano Letters, Vol. 14, Issue 11 https://doi.org/10.1021/nl5024468	journal	October 2014

Similar Records

Elevated temperature transmission Kikuchi diffraction in the SEM

Journal Article · Tue May 15 00:00:00 EDT 2018 · Materials Characterization · OSTI ID:1600045

Todeschini, Matteo; Burrows, Andrew; Jansen, Henri; +1 more

High throughput crystal structure and composition mapping of crystalline nanoprecipitates in alloys by transmission Kikuchi diffraction and analytical electron microscopy

Journal Article · Thu Mar 28 00:00:00 EDT 2019 · Ultramicroscopy · OSTI ID:1600045

Bhattacharya, Arunodaya; Parish, Chad M.; Henry, Jean; +1 more

Transmission Kikuchi diffraction and transmission electron forescatter imaging of electropolished and FIB manufactured TEM specimens

Journal Article · Mon Jun 15 00:00:00 EDT 2015 · Materials Characterization · OSTI ID:1600045

Płociński, T.; Kurzydłowski, K. J.

Related Subjects

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
Grain
nanowires
nanoparticles
transmission electron microscopy
nanoplates

Title: Comparing Scanning Electron Microscope and Transmission Electron Microscope Grain Mapping Techniques Applied to Well-Defined and Highly Irregular Nanoparticles

Citation Formats

References (58)

Similar Records

Related Subjects