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Title: Characterizing crystalline defects in single nanoparticles from angular correlations of single-shot diffracted X-rays

Abstract

Characterizing and controlling the uniformity of nanoparticles is crucial for their application in science and technology because crystalline defects in the nanoparticles strongly affect their unique properties. Recently, ultra-short and ultra-bright X-ray pulses provided by X-ray free-electron lasers (XFELs) opened up the possibility of structure determination of nanometre-scale matter with Å spatial resolution. However, it is often difficult to reconstruct the 3D structural information from single-shot X-ray diffraction patterns owing to the random orientation of the particles. This report proposes an analysis approach for characterizing defects in nanoparticles using wide-angle X-ray scattering (WAXS) data from free-flying single nanoparticles. The analysis method is based on the concept of correlated X-ray scattering, in which correlations of scattered X-ray are used to recover detailed structural information. WAXS experiments of xenon nanoparticles, or clusters, were conducted at an XFEL facility in Japan by using the SPring-8 Ångstrom compact free-electron laser (SACLA). Bragg spots in the recorded single-shot X-ray diffraction patterns showed clear angular correlations, which offered significant structural information on the nanoparticles. The experimental angular correlations were reproduced by numerical simulation in which kinematical theory of diffraction was combined with geometric calculations. We also explain the diffuse scattering intensity as being due to themore » stacking faults in the xenon clusters.« less

Authors:
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Publication Date:
Research Org.:
Argonne National Lab. (ANL), Argonne, IL (United States)
Sponsoring Org.:
USDOE; USDOE Office of Science (SC), Basic Energy Sciences (BES). Chemical Sciences, Geosciences, & Biosciences Division; Ministry of Education, Culture, Sports, Science and Technology (MEXT) of Japan; Japan Society for the Promotion of Science (JSPS)
OSTI Identifier:
1617956
Alternate Identifier(s):
OSTI ID: 1763384
Grant/Contract Number:  
AC02-06CH11357; JP15K17487; JP16K05016; JP19J14969
Resource Type:
Published Article
Journal Name:
IUCrJ
Additional Journal Information:
Journal Name: IUCrJ Journal Volume: 7 Journal Issue: 2; Journal ID: ISSN 2052-2525
Publisher:
International Union of Crystallography (IUCr)
Country of Publication:
United Kingdom
Language:
English
Subject:
73 NUCLEAR PHYSICS AND RADIATION PHYSICS; XFELs; angular correlations; crystalline defects; single nanoparticles; single-shot diffraction; stacking faults; x-ray diffraction; x-ray scattering

Citation Formats

Niozu, Akinobu, Kumagai, Yoshiaki, Nishiyama, Toshiyuki, Fukuzawa, Hironobu, Motomura, Koji, Bucher, Maximilian, Asa, Kazuki, Sato, Yuhiro, Ito, Yuta, Takanashi, Tsukasa, You, Daehyun, Ono, Taishi, Li, Yiwen, Kukk, Edwin, Miron, Catalin, Neagu, Liviu, Callegari, Carlo, Di Fraia, Michele, Rossi, Giorgio, Galli, Davide E., Pincelli, Tommaso, Colombo, Alessandro, Owada, Shigeki, Tono, Kensuke, Kameshima, Takashi, Joti, Yasumasa, Katayama, Tetsuo, Togashi, Tadashi, Yabashi, Makina, Matsuda, Kazuhiro, Nagaya, Kiyonobu, Bostedt, Christoph, and Ueda, Kiyoshi. Characterizing crystalline defects in single nanoparticles from angular correlations of single-shot diffracted X-rays. United Kingdom: N. p., 2020. Web. doi:10.1107/S205225252000144X.
Niozu, Akinobu, Kumagai, Yoshiaki, Nishiyama, Toshiyuki, Fukuzawa, Hironobu, Motomura, Koji, Bucher, Maximilian, Asa, Kazuki, Sato, Yuhiro, Ito, Yuta, Takanashi, Tsukasa, You, Daehyun, Ono, Taishi, Li, Yiwen, Kukk, Edwin, Miron, Catalin, Neagu, Liviu, Callegari, Carlo, Di Fraia, Michele, Rossi, Giorgio, Galli, Davide E., Pincelli, Tommaso, Colombo, Alessandro, Owada, Shigeki, Tono, Kensuke, Kameshima, Takashi, Joti, Yasumasa, Katayama, Tetsuo, Togashi, Tadashi, Yabashi, Makina, Matsuda, Kazuhiro, Nagaya, Kiyonobu, Bostedt, Christoph, & Ueda, Kiyoshi. Characterizing crystalline defects in single nanoparticles from angular correlations of single-shot diffracted X-rays. United Kingdom. doi:https://doi.org/10.1107/S205225252000144X
Niozu, Akinobu, Kumagai, Yoshiaki, Nishiyama, Toshiyuki, Fukuzawa, Hironobu, Motomura, Koji, Bucher, Maximilian, Asa, Kazuki, Sato, Yuhiro, Ito, Yuta, Takanashi, Tsukasa, You, Daehyun, Ono, Taishi, Li, Yiwen, Kukk, Edwin, Miron, Catalin, Neagu, Liviu, Callegari, Carlo, Di Fraia, Michele, Rossi, Giorgio, Galli, Davide E., Pincelli, Tommaso, Colombo, Alessandro, Owada, Shigeki, Tono, Kensuke, Kameshima, Takashi, Joti, Yasumasa, Katayama, Tetsuo, Togashi, Tadashi, Yabashi, Makina, Matsuda, Kazuhiro, Nagaya, Kiyonobu, Bostedt, Christoph, and Ueda, Kiyoshi. Wed . "Characterizing crystalline defects in single nanoparticles from angular correlations of single-shot diffracted X-rays". United Kingdom. doi:https://doi.org/10.1107/S205225252000144X.
@article{osti_1617956,
title = {Characterizing crystalline defects in single nanoparticles from angular correlations of single-shot diffracted X-rays},
author = {Niozu, Akinobu and Kumagai, Yoshiaki and Nishiyama, Toshiyuki and Fukuzawa, Hironobu and Motomura, Koji and Bucher, Maximilian and Asa, Kazuki and Sato, Yuhiro and Ito, Yuta and Takanashi, Tsukasa and You, Daehyun and Ono, Taishi and Li, Yiwen and Kukk, Edwin and Miron, Catalin and Neagu, Liviu and Callegari, Carlo and Di Fraia, Michele and Rossi, Giorgio and Galli, Davide E. and Pincelli, Tommaso and Colombo, Alessandro and Owada, Shigeki and Tono, Kensuke and Kameshima, Takashi and Joti, Yasumasa and Katayama, Tetsuo and Togashi, Tadashi and Yabashi, Makina and Matsuda, Kazuhiro and Nagaya, Kiyonobu and Bostedt, Christoph and Ueda, Kiyoshi},
abstractNote = {Characterizing and controlling the uniformity of nanoparticles is crucial for their application in science and technology because crystalline defects in the nanoparticles strongly affect their unique properties. Recently, ultra-short and ultra-bright X-ray pulses provided by X-ray free-electron lasers (XFELs) opened up the possibility of structure determination of nanometre-scale matter with Å spatial resolution. However, it is often difficult to reconstruct the 3D structural information from single-shot X-ray diffraction patterns owing to the random orientation of the particles. This report proposes an analysis approach for characterizing defects in nanoparticles using wide-angle X-ray scattering (WAXS) data from free-flying single nanoparticles. The analysis method is based on the concept of correlated X-ray scattering, in which correlations of scattered X-ray are used to recover detailed structural information. WAXS experiments of xenon nanoparticles, or clusters, were conducted at an XFEL facility in Japan by using the SPring-8 Ångstrom compact free-electron laser (SACLA). Bragg spots in the recorded single-shot X-ray diffraction patterns showed clear angular correlations, which offered significant structural information on the nanoparticles. The experimental angular correlations were reproduced by numerical simulation in which kinematical theory of diffraction was combined with geometric calculations. We also explain the diffuse scattering intensity as being due to the stacking faults in the xenon clusters.},
doi = {10.1107/S205225252000144X},
journal = {IUCrJ},
number = 2,
volume = 7,
place = {United Kingdom},
year = {2020},
month = {2}
}

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Free Publicly Available Full Text
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DOI: https://doi.org/10.1107/S205225252000144X

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Works referenced in this record:

Single-shot three-dimensional structure determination of nanocrystals with femtosecond X-ray free-electron laser pulses
journal, June 2014

  • Xu, Rui; Jiang, Huaidong; Song, Changyong
  • Nature Communications, Vol. 5, Issue 1
  • DOI: 10.1038/ncomms5061

Single mimivirus particles intercepted and imaged with an X-ray laser
journal, February 2011

  • Seibert, M. Marvin; Ekeberg, Tomas; Maia, Filipe R. N. C.
  • Nature, Vol. 470, Issue 7332
  • DOI: 10.1038/nature09748

Development of an X-ray pixel detector with multi-port charge-coupled device for X-ray free-electron laser experiments
journal, March 2014

  • Kameshima, Takashi; Ono, Shun; Kudo, Togo
  • Review of Scientific Instruments, Vol. 85, Issue 3
  • DOI: 10.1063/1.4867668

Ultrafast X-Ray Scattering of Xenon Nanoparticles: Imaging Transient States of Matter
journal, February 2012


Status of the SACLA Facility
journal, June 2017

  • Yabashi, Makina; Tanaka, Hitoshi; Tono, Kensuke
  • Applied Sciences, Vol. 7, Issue 6
  • DOI: 10.3390/app7060604

Operational properties of fluctuation X-ray scattering data
journal, March 2015


Fractal morphology, imaging and mass spectrometry of single aerosol particles in flight
journal, June 2012

  • Loh, N. D.; Hampton, C. Y.; Martin, A. V.
  • Nature, Vol. 486, Issue 7404
  • DOI: 10.1038/nature11222

Shapes and vorticities of superfluid helium nanodroplets
journal, August 2014


High-Resolution Protein Structure Determination by Serial Femtosecond Crystallography
journal, May 2012


X‐Ray Diffraction by Face‐Centered Cubic Crystals with Deformation Faults
journal, August 1952

  • Paterson, M. S.
  • Journal of Applied Physics, Vol. 23, Issue 8
  • DOI: 10.1063/1.1702312

Femtosecond X-ray protein nanocrystallography
journal, February 2011

  • Chapman, Henry N.; Fromme, Petra; Barty, Anton
  • Nature, Vol. 470, Issue 7332, p. 73-77
  • DOI: 10.1038/nature09750

Determination of the Pulse Duration of an X-Ray Free Electron Laser Using Highly Resolved Single-Shot Spectra
journal, October 2012


SwissFEL: The Swiss X-ray Free Electron Laser
journal, July 2017

  • Milne, Christopher; Schietinger, Thomas; Aiba, Masamitsu
  • Applied Sciences, Vol. 7, Issue 7
  • DOI: 10.3390/app7070720

Single-particle imaging without symmetry constraints at an X-ray free-electron laser
journal, September 2018


Correlations in Scattered X-Ray Laser Pulses Reveal Nanoscale Structural Features of Viruses
journal, October 2017

  • Kurta, Ruslan P.; Donatelli, Jeffrey J.; Yoon, Chun Hong
  • Physical Review Letters, Vol. 119, Issue 15, Article No. 158102
  • DOI: 10.1103/PhysRevLett.119.158102

Serial time-resolved crystallography of photosystem II using a femtosecond X-ray laser
journal, July 2014

  • Kupitz, Christopher; Basu, Shibom; Grotjohann, Ingo
  • Nature, Vol. 513, Issue 7517
  • DOI: 10.1038/nature13453

Transient lattice contraction in the solid-to-plasma transition
journal, January 2016

  • Ferguson, Ken R.; Bucher, Maximilian; Gorkhover, Tais
  • Science Advances, Vol. 2, Issue 1
  • DOI: 10.1126/sciadv.1500837

The Quantum Mechanics of Larger Semiconductor Clusters ("Quantum Dots")
journal, October 1990


Three-dimensional single-particle imaging using angular correlations from X-ray laser data
journal, May 2013

  • Liu, Haiguang; Poon, Billy K.; Saldin, Dilano K.
  • Acta Crystallographica Section A Foundations of Crystallography, Vol. 69, Issue 4
  • DOI: 10.1107/S0108767313006016

Fluctuation x-ray scattering from biological particles in frozen solution by using synchrotron radiation.
journal, June 1981

  • Kam, Z.; Koch, M. H.; Bordas, J.
  • Proceedings of the National Academy of Sciences, Vol. 78, Issue 6
  • DOI: 10.1073/pnas.78.6.3559

Angular X-ray Cross-Correlation Analysis (AXCCA): Basic Concepts and Recent Applications to Soft Matter and Nanomaterials
journal, October 2019

  • Zaluzhnyy, Ivan; Kurta, Ruslan; Scheele, Marcus
  • Materials, Vol. 12, Issue 21
  • DOI: 10.3390/ma12213464

Clusters in intense FLASH pulses: ultrafast ionization dynamics and electron emission studied with spectroscopic and scattering techniques
journal, September 2010

  • Bostedt, C.; Adolph, M.; Eremina, E.
  • Journal of Physics B: Atomic, Molecular and Optical Physics, Vol. 43, Issue 19
  • DOI: 10.1088/0953-4075/43/19/194011

The 3D-architecture of individual free silver nanoparticles captured by X-ray scattering
journal, February 2015

  • Barke, Ingo; Hartmann, Hannes; Rupp, Daniela
  • Nature Communications, Vol. 6, Issue 1
  • DOI: 10.1038/ncomms7187

Ultrafast Structural Dynamics of Nanoparticles in Intense Laser Fields
journal, September 2019


Nucleation and growth of clusters in expanding nozzle flows
journal, May 1981


The reconstruction of structure from electron micrographs of randomly oriented particles
journal, January 1980


High-throughput imaging of heterogeneous cell organelles with an X-ray laser
journal, November 2014


A compact X-ray free-electron laser emitting in the sub-ångström region
journal, June 2012


First lasing and operation of an ångstrom-wavelength free-electron laser
journal, August 2010


X-ray optics for advanced ultrafast pump–probe X-ray experiments at SACLA
journal, February 2019

  • Katayama, Tetsuo; Hirano, Takashi; Morioka, Yuki
  • Journal of Synchrotron Radiation, Vol. 26, Issue 2
  • DOI: 10.1107/S1600577518018362

Three-Dimensional Reconstruction of the Giant Mimivirus Particle with an X-Ray Free-Electron Laser
journal, March 2015


Single-particle structure determination by correlations of snapshot X-ray diffraction patterns
journal, January 2012

  • Starodub, D.; Aquila, A.; Bajt, S.
  • Nature Communications, Vol. 3, Issue 1
  • DOI: 10.1038/ncomms2288

Photon Beam Transport and Scientific Instruments at the European XFEL
journal, June 2017

  • Tschentscher, Thomas; Bressler, Christian; Grünert, Jan
  • Applied Sciences, Vol. 7, Issue 6
  • DOI: 10.3390/app7060592

Electron diffraction study of the structural transformations in free argon clusters
journal, February 2004

  • Danylchenko, O. G.; Kovalenko, S. I.; Samovarov, V. N.
  • Low Temperature Physics, Vol. 30, Issue 2
  • DOI: 10.1063/1.1645170

Construction and Commissioning of PAL-XFEL Facility
journal, May 2017

  • Ko, In; Kang, Heung-Sik; Heo, Hoon
  • Applied Sciences, Vol. 7, Issue 5
  • DOI: 10.3390/app7050479

Structure of large argon clusters ArN,103
journal, November 2000


Chemistry and Properties of Nanocrystals of Different Shapes
journal, April 2005

  • Burda, Clemens; Chen, Xiaobo; Narayanan, Radha
  • Chemical Reviews, Vol. 105, Issue 4
  • DOI: 10.1021/cr030063a

Ultrafast Three-Dimensional Imaging of Lattice Dynamics in Individual Gold Nanocrystals
journal, May 2013


Quantum size effects in metal particles
journal, July 1986


The linac coherent light source single particle imaging road map
journal, July 2015

  • Aquila, A.; Barty, A.; Bostedt, C.
  • Structural Dynamics, Vol. 2, Issue 4
  • DOI: 10.1063/1.4918726

Noncrystalline structure of argon clusters. I. Polyicosahedral structure of Ar N clusters, 20< N <50
journal, April 1983

  • Farges, J.; de Feraudy, M. F.; Raoult, B.
  • The Journal of Chemical Physics, Vol. 78, Issue 8
  • DOI: 10.1063/1.445375

Observation of correlated X-ray scattering at atomic resolution
journal, July 2014

  • Mendez, Derek; Lane, Thomas J.; Sung, Jongmin
  • Philosophical Transactions of the Royal Society B: Biological Sciences, Vol. 369, Issue 1647
  • DOI: 10.1098/rstb.2013.0315

Angular correlations of photons from solution diffraction at a free-electron laser encode molecular structure
journal, September 2016


Semiconductor Clusters, Nanocrystals, and Quantum Dots
journal, February 1996


Coherent Diffraction Imaging Analysis of Shape-Controlled Nanoparticles with Focused Hard X-ray Free-Electron Laser Pulses
journal, November 2013

  • Takahashi, Yukio; Suzuki, Akihiro; Zettsu, Nobuyuki
  • Nano Letters, Vol. 13, Issue 12
  • DOI: 10.1021/nl403247x

Structure determination of Pt-coated Au dumbbells via fluctuation X-ray scattering
journal, July 2012

  • Chen, Gang; Modestino, Miguel A.; Poon, Billy K.
  • Journal of Synchrotron Radiation, Vol. 19, Issue 5
  • DOI: 10.1107/S0909049512023801

Determination of Macromolecular Structure in Solution by Spatial Correlation of Scattering Fluctuations
journal, September 1977


Natively Inhibited Trypanosoma brucei Cathepsin B Structure Determined by Using an X-ray Laser
journal, November 2012