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Title: Experimental setup combining in situ hard X-ray photoelectron spectroscopy and real-time surface X-ray diffraction for characterizing atomic and electronic structure evolution during complex oxide heterostructure growth

Abstract

We describe the next-generation system for in situ characterization of a complex oxide thin film and heterostructure growth by pulsed laser deposition (PLD) using synchrotron hard X-rays. The system consists of a PLD chamber mounted on a diffractometer allowing both real-time surface X-ray diffraction (SXRD) and in situ hard X-ray photoelectron spectroscopy (HAXPES). HAXPES is performed in the incident X-ray energy range from 4 to 12 keV using a Scienta EW4000 electron energy analyzer mounted on the PLD chamber fixed parallel with the surface normal. In addition to the standard application mode of HAXPES for disentangling surface from bulk properties, the increased penetration depth of high energy photoelectrons is used for investigation of the electronic structure changes through thin films grown deliberately as variable thickness capping layers. Such heterostructures represent model systems for investigating a variety of critical thickness and dead layer phenomena observed at complex oxide interfaces. In this new mode of operation, in situ HAXPES is used to determine the electronic structure associated with unique structural features identified by real-time SXRD during thin film growth. The system is configured for using both laboratory excitation sources off-line and on-line operation at beamline 33-ID-D at the Advanced Photon Source. Wemore » illustrate the performance of the system by preliminary scattering and spectroscopic data on oxygen vacancy ordering induced perovskite-to-brownmillerite reversible phase transformation in La 2/3Sr 1/3MnO 3 films capped with oxygen deficient SrTiO 3–δ (100) layers of varying thickness.« less

Authors:
ORCiD logo [1]; ORCiD logo [1]; ORCiD logo [1];  [2]; ORCiD logo [2]; ORCiD logo [1]; ORCiD logo [2]; ORCiD logo [2]
  1. Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)
  2. Argonne National Lab. (ANL), Lemont, IL (United States)
Publication Date:
Research Org.:
Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)
Sponsoring Org.:
USDOE Office of Science (SC), Basic Energy Sciences (BES) (SC-22). Materials Sciences & Engineering Division; USDOE Office of Science (SC), Basic Energy Sciences (BES) (SC-22)
OSTI Identifier:
1564192
Alternate Identifier(s):
OSTI ID: 1561333
Grant/Contract Number:  
AC05-00OR22725; ERKCS80
Resource Type:
Journal Article: Accepted Manuscript
Journal Name:
Review of Scientific Instruments
Additional Journal Information:
Journal Volume: 90; Journal Issue: 9; Journal ID: ISSN 0034-6748
Publisher:
American Institute of Physics (AIP)
Country of Publication:
United States
Language:
English
Subject:
47 OTHER INSTRUMENTATION

Citation Formats

Eres, Gyula, Rouleau, Christopher M., Lu, Qiyang, Zhang, Zhan, Benda, Erika, Lee, Ho Nyung, Tischler, Jon Z., and Fong, Dillon D. Experimental setup combining in situ hard X-ray photoelectron spectroscopy and real-time surface X-ray diffraction for characterizing atomic and electronic structure evolution during complex oxide heterostructure growth. United States: N. p., 2019. Web. doi:10.1063/1.5116135.
Eres, Gyula, Rouleau, Christopher M., Lu, Qiyang, Zhang, Zhan, Benda, Erika, Lee, Ho Nyung, Tischler, Jon Z., & Fong, Dillon D. Experimental setup combining in situ hard X-ray photoelectron spectroscopy and real-time surface X-ray diffraction for characterizing atomic and electronic structure evolution during complex oxide heterostructure growth. United States. doi:10.1063/1.5116135.
Eres, Gyula, Rouleau, Christopher M., Lu, Qiyang, Zhang, Zhan, Benda, Erika, Lee, Ho Nyung, Tischler, Jon Z., and Fong, Dillon D. Wed . "Experimental setup combining in situ hard X-ray photoelectron spectroscopy and real-time surface X-ray diffraction for characterizing atomic and electronic structure evolution during complex oxide heterostructure growth". United States. doi:10.1063/1.5116135. https://www.osti.gov/servlets/purl/1564192.
@article{osti_1564192,
title = {Experimental setup combining in situ hard X-ray photoelectron spectroscopy and real-time surface X-ray diffraction for characterizing atomic and electronic structure evolution during complex oxide heterostructure growth},
author = {Eres, Gyula and Rouleau, Christopher M. and Lu, Qiyang and Zhang, Zhan and Benda, Erika and Lee, Ho Nyung and Tischler, Jon Z. and Fong, Dillon D.},
abstractNote = {We describe the next-generation system for in situ characterization of a complex oxide thin film and heterostructure growth by pulsed laser deposition (PLD) using synchrotron hard X-rays. The system consists of a PLD chamber mounted on a diffractometer allowing both real-time surface X-ray diffraction (SXRD) and in situ hard X-ray photoelectron spectroscopy (HAXPES). HAXPES is performed in the incident X-ray energy range from 4 to 12 keV using a Scienta EW4000 electron energy analyzer mounted on the PLD chamber fixed parallel with the surface normal. In addition to the standard application mode of HAXPES for disentangling surface from bulk properties, the increased penetration depth of high energy photoelectrons is used for investigation of the electronic structure changes through thin films grown deliberately as variable thickness capping layers. Such heterostructures represent model systems for investigating a variety of critical thickness and dead layer phenomena observed at complex oxide interfaces. In this new mode of operation, in situ HAXPES is used to determine the electronic structure associated with unique structural features identified by real-time SXRD during thin film growth. The system is configured for using both laboratory excitation sources off-line and on-line operation at beamline 33-ID-D at the Advanced Photon Source. We illustrate the performance of the system by preliminary scattering and spectroscopic data on oxygen vacancy ordering induced perovskite-to-brownmillerite reversible phase transformation in La2/3Sr1/3MnO3 films capped with oxygen deficient SrTiO3–δ (100) layers of varying thickness.},
doi = {10.1063/1.5116135},
journal = {Review of Scientific Instruments},
issn = {0034-6748},
number = 9,
volume = 90,
place = {United States},
year = {2019},
month = {9}
}

Journal Article:
Free Publicly Available Full Text
Publisher's Version of Record

Figures / Tables:

FIG. 1 FIG. 1: Schematic diagram of the experimental apparatus for real-time SXRD and in situ HAXPES consisting of the PLD chamber mounted on the diffractometer with the S2D2 configuration, RHEED system, and electron energy analyzer for HAXPES.

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