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Title: Deposition and characterization of α-Fe2O3/Pd thin films for neutron reflectometry studies

Abstract

We report deposition of hematite/Pd thin films on silicon wafers via radio frequency (RF) magnetron sputtering and subsequent characterization for future in situ neutron reflectometry studies. Following deposition, the hematite/Pd thin films were characterized as prepared and after annealing in air for 2h at 400, 500, and 600 °C, respectively. Raman spectroscopy, grazing incidence x-ray diffraction, and neutron reflectometry (NR) were used to characterize the structure and chemical compositions of the thin films. The results indicate that pure α-Fe2O3 (hematite) films were produced, free from other iron oxide phases and impurities. NR data reveal that one intermediate layer between the Pd layer and the hematite layer was formed during sputtering deposition processes. The fitted scattering length density (SLD) of the as-deposited hematite layer is 70% of the theoretical SLD value, indicating that the grains are loosely packed in the RF-deposited hematite films. After annealing at elevated temperatures, the hematite films show increased SLD values but remain comparable to that of preannealed.

Authors:
ORCiD logo [1]; ORCiD logo [1]; ORCiD logo [2];  [3]; ORCiD logo [2]; ORCiD logo [1];  [1]; ORCiD logo [4]; ORCiD logo [1]
  1. Oak Ridge National Laboratory (ORNL), Oak Ridge, TN (United States)
  2. Sandia National Laboratories (SNL-NM), Albuquerque, NM (United States). Center for Integrated Nanotechnologies (CINT)
  3. Oak Ridge National Laboratory (ORNL), Oak Ridge, TN (United States). Center for Nanophase Materials Sciences (CNMS)
  4. Univ. of Tennessee, Knoxville, TN (United States)
Publication Date:
Research Org.:
Oak Ridge National Laboratory (ORNL), Oak Ridge, TN (United States). Center for Nanophase Materials Sciences (CNMS); 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); USDOE Laboratory Directed Research and Development (LDRD) Program
OSTI Identifier:
1991731
Alternate Identifier(s):
OSTI ID: 2311362
Report Number(s):
SAND-2024-01339J
Journal ID: ISSN 0734-2101
Grant/Contract Number:  
AC05-00OR22725; NA0003525
Resource Type:
Accepted Manuscript
Journal Name:
Journal of Vacuum Science and Technology A
Additional Journal Information:
Journal Volume: 41; Journal Issue: 5; Journal ID: ISSN 0734-2101
Publisher:
American Vacuum Society / AIP
Country of Publication:
United States
Language:
English
Subject:
36 MATERIALS SCIENCE; Neutron reflectometry; Raman spectroscopy; Magnetron sputtering; Thin films; X-ray diffraction

Citation Formats

Wang, Hanyu, Self, Ethan C., Addamane, Sadhvikas J., Rouleau, Christopher M., Wixom, Ryan R., Browning, Katie L., Veith, Gabriel M., Liang, Liyuan, and Browning, James F. Deposition and characterization of α-Fe2O3/Pd thin films for neutron reflectometry studies. United States: N. p., 2023. Web. doi:10.1116/6.0002717.
Wang, Hanyu, Self, Ethan C., Addamane, Sadhvikas J., Rouleau, Christopher M., Wixom, Ryan R., Browning, Katie L., Veith, Gabriel M., Liang, Liyuan, & Browning, James F. Deposition and characterization of α-Fe2O3/Pd thin films for neutron reflectometry studies. United States. https://doi.org/10.1116/6.0002717
Wang, Hanyu, Self, Ethan C., Addamane, Sadhvikas J., Rouleau, Christopher M., Wixom, Ryan R., Browning, Katie L., Veith, Gabriel M., Liang, Liyuan, and Browning, James F. Fri . "Deposition and characterization of α-Fe2O3/Pd thin films for neutron reflectometry studies". United States. https://doi.org/10.1116/6.0002717.
@article{osti_1991731,
title = {Deposition and characterization of α-Fe2O3/Pd thin films for neutron reflectometry studies},
author = {Wang, Hanyu and Self, Ethan C. and Addamane, Sadhvikas J. and Rouleau, Christopher M. and Wixom, Ryan R. and Browning, Katie L. and Veith, Gabriel M. and Liang, Liyuan and Browning, James F.},
abstractNote = {We report deposition of hematite/Pd thin films on silicon wafers via radio frequency (RF) magnetron sputtering and subsequent characterization for future in situ neutron reflectometry studies. Following deposition, the hematite/Pd thin films were characterized as prepared and after annealing in air for 2h at 400, 500, and 600 °C, respectively. Raman spectroscopy, grazing incidence x-ray diffraction, and neutron reflectometry (NR) were used to characterize the structure and chemical compositions of the thin films. The results indicate that pure α-Fe2O3 (hematite) films were produced, free from other iron oxide phases and impurities. NR data reveal that one intermediate layer between the Pd layer and the hematite layer was formed during sputtering deposition processes. The fitted scattering length density (SLD) of the as-deposited hematite layer is 70% of the theoretical SLD value, indicating that the grains are loosely packed in the RF-deposited hematite films. After annealing at elevated temperatures, the hematite films show increased SLD values but remain comparable to that of preannealed.},
doi = {10.1116/6.0002717},
journal = {Journal of Vacuum Science and Technology A},
number = 5,
volume = 41,
place = {United States},
year = {Fri Jul 14 00:00:00 EDT 2023},
month = {Fri Jul 14 00:00:00 EDT 2023}
}

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Works referenced in this record:

Ultrahigh vacuum dc magnetron sputter-deposition of epitaxial Pd(111)/Al2O3(0001) thin films
journal, March 2018

  • Aleman, Angel; Li, Chao; Zaid, Hicham
  • Journal of Vacuum Science & Technology A: Vacuum, Surfaces, and Films, Vol. 36, Issue 3
  • DOI: 10.1116/1.5021609

Synergies of co-doping in ultra-thin hematite photoanodes for solar water oxidation: In and Ti as representative case
journal, January 2020

  • Singh, Aadesh P.; Tossi, Camilla; Tittonen, Ilkka
  • RSC Advances, Vol. 10, Issue 55
  • DOI: 10.1039/D0RA04576D

Mechanism of PdO thin film formation during the oxidation of Pd(111)
journal, September 2009


Effects of soluble flavin on heterogeneous electron transfer between surface-exposed bacterial cytochromes and iron oxides
journal, August 2015


Motofit – integrating neutron reflectometry acquisition, reduction and analysis into one, easy to use, package
journal, November 2010


Growth without Postannealing of Monoclinic VO2 Thin Film by Atomic Layer Deposition Using VCl4 as Precursor
journal, November 2018


Exploring the Efficacy of Platinum and Palladium Nanostructures for Organic Molecule Detection via Raman Spectroscopy
journal, January 2018

  • Tran, Minh; Whale, Alison; Padalkar, Sonal
  • Sensors, Vol. 18, Issue 2
  • DOI: 10.3390/s18010147

Redox-linked conformation change and electron transfer between monoheme c-type cytochromes and oxides
journal, September 2006

  • Khare, Nidhi; Lovelace, David M.; Eggleston, Carrick M.
  • Geochimica et Cosmochimica Acta, Vol. 70, Issue 17
  • DOI: 10.1016/j.gca.2006.06.1561

Nanostructured hematite: synthesis, characterization, charge carrier dynamics, and photoelectrochemical properties
journal, January 2012

  • Wheeler, Damon A.; Wang, Gongming; Ling, Yichuan
  • Energy & Environmental Science, Vol. 5, Issue 5
  • DOI: 10.1039/c2ee00001f

Reaction of hydroquinone with hematite
journal, June 2004

  • Stack, Andrew G.; Rosso, Kevin M.; Smith, Dayle M. A.
  • Journal of Colloid and Interface Science, Vol. 274, Issue 2
  • DOI: 10.1016/j.jcis.2004.01.001

Photoelectrochemistry: Applications to Solar Energy Conversion
journal, October 1978


Transformation mechanism of magnetite nanoparticles
journal, June 2015


Cytochrome c interaction with hematite (α-Fe2O3) surfaces
journal, February 2006

  • Eggleston, Carrick M.; Khare, Nidhi; Lovelace, David M.
  • Journal of Electron Spectroscopy and Related Phenomena, Vol. 150, Issue 2-3
  • DOI: 10.1016/j.elspec.2005.06.006

The SNS Liquids Reflectometer
journal, July 2008


Reductive dissolution of goethite and hematite by reduced flavins
journal, November 2013


Photoenhanced Electrochemical Interaction between Shewanella and a Hematite Nanowire Photoanode
journal, June 2014

  • Qian, Fang; Wang, Hanyu; Ling, Yichuan
  • Nano Letters, Vol. 14, Issue 6
  • DOI: 10.1021/nl501664n

Review of Sn-Doped Hematite Nanostructures for Photoelectrochemical Water Splitting
journal, July 2014

  • Ling, Yichuan; Li, Yat
  • Particle & Particle Systems Characterization, Vol. 31, Issue 11
  • DOI: 10.1002/ppsc.201400051

Phonon Anharmonicity of PdO Studied by Raman Spectrometry
journal, September 2015

  • Zhao, Zhouying; Elwood, Jacqueline; Carpenter, Michael A.
  • The Journal of Physical Chemistry C, Vol. 119, Issue 40
  • DOI: 10.1021/acs.jpcc.5b07652

Electrochemical interaction of Shewanella oneidensis MR-1 and its outer membrane cytochromes OmcA and MtrC with hematite electrodes
journal, September 2009

  • Meitl, Leisa A.; Eggleston, Carrick M.; Colberg, Patricia J. S.
  • Geochimica et Cosmochimica Acta, Vol. 73, Issue 18
  • DOI: 10.1016/j.gca.2009.06.021

Structural, optical and electrical properties of undoped polycrystalline hematite thin films produced using filtered arc deposition
journal, February 2008


The role of the substrate on the mechanical and thermal stability of Pd thin films during hydrogen (de)sorption
journal, January 2021


Polarized Raman spectra of hematite and assignment of external modes
journal, January 2020

  • Marshall, Craig P.; Dufresne, William J. B.; Rufledt, Carson J.
  • Journal of Raman Spectroscopy, Vol. 51, Issue 9
  • DOI: 10.1002/jrs.5824

Influence of apparatus geometry and deposition conditions on the structure and topography of thick sputtered coatings
journal, July 1974

  • Thornton, John A.
  • Journal of Vacuum Science and Technology, Vol. 11, Issue 4
  • DOI: 10.1116/1.1312732

Electrochemistry of Sputtered Hematite Photoanodes: A Comparison of Metallic DC versus Reactive RF Sputtering
journal, May 2019


Electrochemical properties of the interaction between cytochrome c and a hematite nanowire array electrode
journal, October 2019


Vibrational Spectroscopic Characterization of Hematite, Maghemite, and Magnetite Thin Films Produced by Vapor Deposition
journal, September 2010

  • Jubb, Aaron M.; Allen, Heather C.
  • ACS Applied Materials & Interfaces, Vol. 2, Issue 10
  • DOI: 10.1021/am1004943

Raman spectroscopy of Fe-Ti-Cr-oxides, case study: Martian meteorite EETA79001
journal, May 2004

  • Wang, Alian; Kuebler, Karla E.; Jolliff, Bradley L.
  • American Mineralogist, Vol. 89, Issue 5-6
  • DOI: 10.2138/am-2004-5-601

Textures of Au, Pt and Pd/PdO nanoparticles thermally dewetted from thin metal layers on fused silica
journal, January 2014

  • Kracker, Michael; Wisniewski, Wolfgang; Rüssel, Christian
  • RSC Adv., Vol. 4, Issue 89
  • DOI: 10.1039/C4RA07296K