DOE PAGES title logo U.S. Department of Energy
Office of Scientific and Technical Information

Title: Instrument for in situ hard x-ray nanobeam characterization during epitaxial crystallization and materials transformations

Abstract

Solid-phase epitaxy (SPE) and other three-dimensional epitaxial crystallization processes pose challenging structural and chemical characterization problems. The concentration of defects, the spatial distribution of elastic strain, and the chemical state of ions each vary with nanoscale characteristic length scales and depend sensitively on the gas environment and elastic boundary conditions during growth. The lateral or three-dimensional propagation of crystalline interfaces in SPE has nanoscale or submicrometer characteristic distances during typical crystallization times. Here, an in situ synchrotron hard x-ray instrument allows these features to be studied during deposition and crystallization using diffraction, resonant scattering, nanobeam and coherent diffraction imaging, and reflectivity. The instrument incorporates a compact deposition system allowing the use of short-working-distance x-ray focusing optics. Layers are deposited using radio-frequency magnetron sputtering and evaporation sources. The deposition system provides control of the gas atmosphere and sample temperature. The sample is positioned using a stable mechanical design to minimize vibration and drift and employs precise translation stages to enable nanobeam experiments. Results of in situ x-ray characterization of the amorphous thin film deposition process for a SrTiO3/BaTiO3 multilayer illustrate implementation of this instrument.

Authors:
ORCiD logo [1]; ORCiD logo [1]; ORCiD logo [1]; ORCiD logo [2]; ORCiD logo [2]; ORCiD logo [1]; ORCiD logo [2]; ORCiD logo [1]
  1. Univ. of Wisconsin, Madison, WI (United States)
  2. Argonne National Lab. (ANL), Argonne, IL (United States)
Publication Date:
Research Org.:
Argonne National Laboratory (ANL), Argonne, IL (United States)
Sponsoring Org.:
USDOE Office of Science (SC), Basic Energy Sciences (BES). Materials Sciences & Engineering Division; National Science Foundation (NSF); USDOE
OSTI Identifier:
1774161
Alternate Identifier(s):
OSTI ID: 1765926
Grant/Contract Number:  
AC02-06CH11357; DMR-1720415
Resource Type:
Accepted Manuscript
Journal Name:
Review of Scientific Instruments
Additional Journal Information:
Journal Volume: 92; Journal Issue: 2; Journal ID: ISSN 0034-6748
Publisher:
American Institute of Physics (AIP)
Country of Publication:
United States
Language:
English
Subject:
47 OTHER INSTRUMENTATION; x-ray instruments; crystallization; coherence imaging; x-ray microscopy; thin film deposition; synchrotrons; epitaxy; materials analysis; hard x-rays; magnetron sputtering

Citation Formats

Marks, Samuel D., Quan, Peiyu, Liu, Rui, Highland, Matthew J., Zhou, Hua, Kuech, Thomas F., Stephenson, G. Brian, and Evans, Paul G. Instrument for in situ hard x-ray nanobeam characterization during epitaxial crystallization and materials transformations. United States: N. p., 2021. Web. doi:10.1063/5.0039196.
Marks, Samuel D., Quan, Peiyu, Liu, Rui, Highland, Matthew J., Zhou, Hua, Kuech, Thomas F., Stephenson, G. Brian, & Evans, Paul G. Instrument for in situ hard x-ray nanobeam characterization during epitaxial crystallization and materials transformations. United States. https://doi.org/10.1063/5.0039196
Marks, Samuel D., Quan, Peiyu, Liu, Rui, Highland, Matthew J., Zhou, Hua, Kuech, Thomas F., Stephenson, G. Brian, and Evans, Paul G. Mon . "Instrument for in situ hard x-ray nanobeam characterization during epitaxial crystallization and materials transformations". United States. https://doi.org/10.1063/5.0039196. https://www.osti.gov/servlets/purl/1774161.
@article{osti_1774161,
title = {Instrument for in situ hard x-ray nanobeam characterization during epitaxial crystallization and materials transformations},
author = {Marks, Samuel D. and Quan, Peiyu and Liu, Rui and Highland, Matthew J. and Zhou, Hua and Kuech, Thomas F. and Stephenson, G. Brian and Evans, Paul G.},
abstractNote = {Solid-phase epitaxy (SPE) and other three-dimensional epitaxial crystallization processes pose challenging structural and chemical characterization problems. The concentration of defects, the spatial distribution of elastic strain, and the chemical state of ions each vary with nanoscale characteristic length scales and depend sensitively on the gas environment and elastic boundary conditions during growth. The lateral or three-dimensional propagation of crystalline interfaces in SPE has nanoscale or submicrometer characteristic distances during typical crystallization times. Here, an in situ synchrotron hard x-ray instrument allows these features to be studied during deposition and crystallization using diffraction, resonant scattering, nanobeam and coherent diffraction imaging, and reflectivity. The instrument incorporates a compact deposition system allowing the use of short-working-distance x-ray focusing optics. Layers are deposited using radio-frequency magnetron sputtering and evaporation sources. The deposition system provides control of the gas atmosphere and sample temperature. The sample is positioned using a stable mechanical design to minimize vibration and drift and employs precise translation stages to enable nanobeam experiments. Results of in situ x-ray characterization of the amorphous thin film deposition process for a SrTiO3/BaTiO3 multilayer illustrate implementation of this instrument.},
doi = {10.1063/5.0039196},
journal = {Review of Scientific Instruments},
number = 2,
volume = 92,
place = {United States},
year = {Mon Feb 01 00:00:00 EST 2021},
month = {Mon Feb 01 00:00:00 EST 2021}
}

Works referenced in this record:

A two magnetron sputter deposition chamber for in situ observation of thin film growth by synchrotron radiation scattering
journal, August 2001

  • Matz, W.; Schell, N.; Neumann, W.
  • Review of Scientific Instruments, Vol. 72, Issue 8
  • DOI: 10.1063/1.1384432

Scanning x-ray diffraction with 200nm spatial resolution
journal, May 2008

  • Hanke, M.; Dubslaff, M.; Schmidbauer, M.
  • Applied Physics Letters, Vol. 92, Issue 19
  • DOI: 10.1063/1.2929374

Nanomembrane-based materials for Group IV semiconductor quantum electronics
journal, February 2014

  • Paskiewicz, D. M.; Savage, D. E.; Holt, M. V.
  • Scientific Reports, Vol. 4, Issue 1
  • DOI: 10.1038/srep04218

Fast nonthermal processes in pulsed laser deposition
journal, June 2020


Lateral solid phase epitaxy of amorphous Si films on Si substrates with SiO 2 patterns
journal, December 1983

  • Ishiwara, Hiroshi; Yamamoto, Hiroshi; Furukawa, Seijiro
  • Applied Physics Letters, Vol. 43, Issue 11
  • DOI: 10.1063/1.94217

In situ x-ray and electron scattering studies of oxide molecular beam epitaxial growth
journal, October 2020

  • Yan, Xi; Wrobel, Friederike; Li, Yan
  • APL Materials, Vol. 8, Issue 10
  • DOI: 10.1063/5.0025849

Accessing a growth window for SrVO3 thin films
journal, October 2015

  • Brahlek, Matthew; Zhang, Lei; Eaton, Craig
  • Applied Physics Letters, Vol. 107, Issue 14
  • DOI: 10.1063/1.4932198

Crystallization of amorphous complex oxides: New geometries and new compositions via solid phase epitaxy
journal, December 2018

  • Evans, Paul G.; Chen, Yajin; Tilka, Jack A.
  • Current Opinion in Solid State and Materials Science, Vol. 22, Issue 6
  • DOI: 10.1016/j.cossms.2018.09.001

In situ X-ray diffraction and the evolution of polarization during the growth of ferroelectric superlattices
journal, December 2015

  • Bein, Benjamin; Hsing, Hsiang-Chun; Callori, Sara J.
  • Nature Communications, Vol. 6, Issue 1
  • DOI: 10.1038/ncomms10136

Lateral Solid-Phase Epitaxy of Oxide Thin Films on Glass Substrate Seeded with Oxide Nanosheets
journal, May 2014

  • Taira, Kenji; Hirose, Yasushi; Nakao, Shoichiro
  • ACS Nano, Vol. 8, Issue 6
  • DOI: 10.1021/nn501563j

Characterization of the X-ray coherence properties of an undulator beamline at the Advanced Photon Source
journal, June 2018

  • Ju, Guangxu; Highland, Matthew J.; Thompson, Carol
  • Journal of Synchrotron Radiation, Vol. 25, Issue 4
  • DOI: 10.1107/s1600577518006501

Observation of Columnar Microstructure in Step-Graded Si 1 x Ge x / Si Films Using High-Resolution X-Ray Microdiffraction
journal, March 2002


Incorporation of air-cavity into sapphire substrate and its effect on GaN growth and optical properties
journal, November 2015


High-Resolution Scanning X-ray Diffraction Microscopy
journal, July 2008


Hard x‐ray phase zone plate fabricated by lithographic techniques
journal, October 1992

  • Lai, B.; Yun, W. B.; Legnini, D.
  • Applied Physics Letters, Vol. 61, Issue 16
  • DOI: 10.1063/1.108400

Elements of Modern X-ray Physics
book, March 2011


In-Situ X-ray Diffraction Study of the Crystallization Kinetics of Mesoporous Titania Films
journal, August 2004

  • Kirsch, Bradley L.; Richman, Erik K.; Riley, Andrew E.
  • The Journal of Physical Chemistry B, Vol. 108, Issue 34
  • DOI: 10.1021/jp036442p

Functional links between stability and reactivity of strontium ruthenate single crystals during oxygen evolution
journal, June 2014

  • Chang, Seo Hyoung; Danilovic, Nemanja; Chang, Kee-Chul
  • Nature Communications, Vol. 5, Issue 1
  • DOI: 10.1038/ncomms5191

Nanometer focusing of hard x rays by phase zone plates
journal, May 1999

  • Yun, W.; Lai, B.; Cai, Z.
  • Review of Scientific Instruments, Vol. 70, Issue 5
  • DOI: 10.1063/1.1149744

Measurements of Surface Diffusivity and Coarsening during Pulsed Laser Deposition
journal, December 2009


High-resolution three-dimensional structural microscopy by single-angle Bragg ptychography
journal, November 2016

  • Hruszkewycz, S. O.; Allain, M.; Holt, M. V.
  • Nature Materials, Vol. 16, Issue 2
  • DOI: 10.1038/nmat4798

Structure and strain relaxation mechanisms of ultrathin epitaxial Pr2O3 films on Si(111)
journal, April 2005

  • Schroeder, T.; Lee, T. -L.; Libralesso, L.
  • Journal of Applied Physics, Vol. 97, Issue 7
  • DOI: 10.1063/1.1883304

Germanium hut nanostressors on freestanding thin silicon membranes
journal, August 2005

  • Evans, P. G.; Tinberg, D. S.; Roberts, M. M.
  • Applied Physics Letters, Vol. 87, Issue 7
  • DOI: 10.1063/1.2031941

An instrument for in situ coherent x-ray studies of metal-organic vapor phase epitaxy of III-nitrides
journal, March 2017

  • Ju, Guangxu; Highland, Matthew J.; Yanguas-Gil, Angel
  • Review of Scientific Instruments, Vol. 88, Issue 3
  • DOI: 10.1063/1.4978656

A compact UHV deposition system for in situ study of ultrathin films via hard x-ray scattering and spectroscopy
journal, January 2008

  • Couet, Sebastien; Diederich, Thomas; Schlage, Kai
  • Review of Scientific Instruments, Vol. 79, Issue 9
  • DOI: 10.1063/1.2982059

In-situ X-ray Diffraction study of Metal Induced Crystallization of amorphous silicon
journal, June 2008


Role of ferroelectric polarization during growth of highly strained ferroelectric materials
journal, May 2020


Spontaneous Hall effect enhanced by local Ir moments in epitaxial P r 2 I r 2 O 7 thin films
journal, March 2020


Modular instrument mounting system for variable environment in operando X-ray experiments
journal, February 2013

  • Folkman, C. M.; Highland, M. J.; Perret, E.
  • Review of Scientific Instruments, Vol. 84, Issue 2
  • DOI: 10.1063/1.4791799

Reduction of Interface Reactions in the Low-Temperature Solid-Phase Epitaxy of ScAlMgO 4 on Al 2 O 3 (0001)
journal, July 2020


Molecular dynamics simulations of the solid phase epitaxy of Si: Growth mechanism and orientation effects
journal, September 2009

  • Lampin, E.; Krzeminski, C.
  • Journal of Applied Physics, Vol. 106, Issue 6
  • DOI: 10.1063/1.3211972