Stand-alone polarization-modulation infrared reflection absorption spectroscopy instrument optimized for the study of catalytic processes at elevated pressures
Abstract
This article describes the design and construction of a compact, “user-friendly” polarization-modulation infrared reflection absorption spectroscopy (PM-IRRAS) instrument at the Center for Functional Nanomaterials (CFN) of Brookhaven National Laboratory, which allows studying surfaces at pressures ranging from ultra-high vacuum to 100 Torr. Surface infrared spectroscopy is ideally suited for studying these processes as the vibrational frequencies of the IR chromophores are sensitive to the nature of the bonding environment on the surface. Relying on the surface selection rules, by modulating the polarization of incident light, it is possible to separate the contributions from the isotropic gas or solution phase, from the surface bound species. A spectral frequency range between 1000 cm-1 and 4000 cm-1 can be acquired. While typical spectra with a good signal to noise ratio can be obtained at elevated pressures of gases in ~2 min at 4 cm-1 resolution, we have also acquired higher resolution spectra at 0.25 cm-1 with longer acquisition times. By way of verification, CO uptake on a heavily oxidized Ru(0001) sample was studied. As part of this test study, the presence of CO adsorbed on Ru bridge sites was confirmed, in agreement with previous ambient pressure X ray photoelectron spectroscopy studies. In termsmore »
- Authors:
-
- Brookhaven National Lab. (BNL), Upton, NY (United States). Center for Functional Nanomaterials (CFN)
- Brookhaven National Lab. (BNL), Upton, NY (United States). Chemistry Dept.; King Abdullah Univ. of Science and Technology, Thuwal (Saudi Arabia). Saudi Basic Industries Corporation (SABIC) and Controlled Release and Delivery Lab. (CRD)
- Publication Date:
- Research Org.:
- Brookhaven National Laboratory (BNL), Upton, NY (United States)
- Sponsoring Org.:
- USDOE Office of Science (SC), Basic Energy Sciences (BES)
- OSTI Identifier:
- 1430855
- Alternate Identifier(s):
- OSTI ID: 1399286
- Report Number(s):
- BNL-203375-2018-JAAM
Journal ID: ISSN 0034-6748; TRN: US1802923
- Grant/Contract Number:
- SC0012704
- Resource Type:
- Accepted Manuscript
- Journal Name:
- Review of Scientific Instruments
- Additional Journal Information:
- Journal Volume: 88; Journal Issue: 10; Journal ID: ISSN 0034-6748
- Publisher:
- American Institute of Physics (AIP)
- Country of Publication:
- United States
- Language:
- English
- Subject:
- 77 NANOSCIENCE AND NANOTECHNOLOGY; 46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND TECHNOLOGY; 47 OTHER INSTRUMENTATION; 36 MATERIALS SCIENCE; 37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY; Materials; Metals; Spectroscopy; Metallurgy; Chemical analysis; Transition metals; Optical metrology; Thin film deposition; Materials analysis; Spectra
Citation Formats
Kestell, John D., Mudiyanselage, Kumudu, Ye, Xinyi, Nam, Chang-Yong, Stacchiola, Dario, Sadowski, Jerzy, and Boscoboinik, J. Anibal. Stand-alone polarization-modulation infrared reflection absorption spectroscopy instrument optimized for the study of catalytic processes at elevated pressures. United States: N. p., 2017.
Web. doi:10.1063/1.5007024.
Kestell, John D., Mudiyanselage, Kumudu, Ye, Xinyi, Nam, Chang-Yong, Stacchiola, Dario, Sadowski, Jerzy, & Boscoboinik, J. Anibal. Stand-alone polarization-modulation infrared reflection absorption spectroscopy instrument optimized for the study of catalytic processes at elevated pressures. United States. https://doi.org/10.1063/1.5007024
Kestell, John D., Mudiyanselage, Kumudu, Ye, Xinyi, Nam, Chang-Yong, Stacchiola, Dario, Sadowski, Jerzy, and Boscoboinik, J. Anibal. Sun .
"Stand-alone polarization-modulation infrared reflection absorption spectroscopy instrument optimized for the study of catalytic processes at elevated pressures". United States. https://doi.org/10.1063/1.5007024. https://www.osti.gov/servlets/purl/1430855.
@article{osti_1430855,
title = {Stand-alone polarization-modulation infrared reflection absorption spectroscopy instrument optimized for the study of catalytic processes at elevated pressures},
author = {Kestell, John D. and Mudiyanselage, Kumudu and Ye, Xinyi and Nam, Chang-Yong and Stacchiola, Dario and Sadowski, Jerzy and Boscoboinik, J. Anibal},
abstractNote = {This article describes the design and construction of a compact, “user-friendly” polarization-modulation infrared reflection absorption spectroscopy (PM-IRRAS) instrument at the Center for Functional Nanomaterials (CFN) of Brookhaven National Laboratory, which allows studying surfaces at pressures ranging from ultra-high vacuum to 100 Torr. Surface infrared spectroscopy is ideally suited for studying these processes as the vibrational frequencies of the IR chromophores are sensitive to the nature of the bonding environment on the surface. Relying on the surface selection rules, by modulating the polarization of incident light, it is possible to separate the contributions from the isotropic gas or solution phase, from the surface bound species. A spectral frequency range between 1000 cm-1 and 4000 cm-1 can be acquired. While typical spectra with a good signal to noise ratio can be obtained at elevated pressures of gases in ~2 min at 4 cm-1 resolution, we have also acquired higher resolution spectra at 0.25 cm-1 with longer acquisition times. By way of verification, CO uptake on a heavily oxidized Ru(0001) sample was studied. As part of this test study, the presence of CO adsorbed on Ru bridge sites was confirmed, in agreement with previous ambient pressure X ray photoelectron spectroscopy studies. In terms of instrument performance, it was also determined that the gas phase contribution from CO could be completely removed even up to pressures close to 100 Torr. A second test study demonstrated the use of the technique for studying morphological properties of a spin coated polymer on a conductive surface. Note that this is a novel application of this technique. In this experiment, the polarization of incident light was modulated manually (vs. through a photoelastic modulator). It was demonstrated, in good agreement with the literature, that the polymer chains preferentially lie parallel with the surface. This PM-IRRAS system is small, modular, and easily reconfigurable. It also features a “vacuum suitcase” that allows for the integration of the PM-IRRAS system with the rest of the suite of instrumentation at our laboratory available to external users through the CFN user proposal system.},
doi = {10.1063/1.5007024},
journal = {Review of Scientific Instruments},
number = 10,
volume = 88,
place = {United States},
year = {Sun Oct 01 00:00:00 EDT 2017},
month = {Sun Oct 01 00:00:00 EDT 2017}
}
Web of Science
Works referenced in this record:
Bridging the gap between insightful simplicity and successful complexity: From fundamental studies on model systems to technical catalysts
journal, August 2015
- Prieto, Gonzalo; Schüth, Ferdi
- Journal of Catalysis, Vol. 328
A New Method for Performing Polarization Modulation Infrared Reflection-Adsorption Spectroscopy of Surfaces
journal, March 2009
- Schennach, Robert; Hirschmugl, Carol; Gilli, Eduard
- Applied Spectroscopy, Vol. 63, Issue 3
CO oxidation over ruthenium: identification of the catalytically active phases at near-atmospheric pressures
journal, January 2012
- Gao, Feng; Goodman, D. Wayne
- Physical Chemistry Chemical Physics, Vol. 14, Issue 19
Real‐time sampling electronics for double modulation experiments with Fourier transform infrared spectrometers
journal, June 1991
- Green, Michael J.; Barner, Barbara J.; Corn, Robert M.
- Review of Scientific Instruments, Vol. 62, Issue 6
Simultaneous Monitoring of Surface and Gas Phase Species during Hydrogenation of Acetylene over Pt(111) by Polarization-Dependent Infrared Spectroscopy
journal, July 2015
- Krooswyk, Joel D.; Waluyo, Iradwikanari; Trenary, Michael
- ACS Catalysis, Vol. 5, Issue 8
Design of a reflection–absorption experiment for studying the ir spectrum of molecules adsorbed on a metal surface
journal, November 1975
- Greenler, Robert G.
- Journal of Vacuum Science and Technology, Vol. 12, Issue 6
Mechanical Behavior and Anisotropy of Spin-Coated SU-8 Thin Films for MEMS
journal, February 2014
- Robin, C. J.; Vishnoi, Aakansha; Jonnalagadda, Krishna N.
- Journal of Microelectromechanical Systems, Vol. 23, Issue 1
Model Studies in Heterogeneous Catalysis
journal, July 2010
- Freund, H. -J.
- Chemistry - A European Journal, Vol. 16, Issue 31
CO adsorption on the reduced RuO2(110) surface
journal, December 2003
- Paulus, U. A.; Wang, Y.; Jacobi, K.
- Surface Science, Vol. 547, Issue 3
An experimental set-up to apply polarization modulation to infrared reflection absorption spectroscopy for improved in situ studies of atmospheric corrosion processes
journal, June 2014
- Wiesinger, R.; Schade, U.; Kleber, Ch.
- Review of Scientific Instruments, Vol. 85, Issue 6
Catalysis and Surface Science
journal, January 1999
- Ertl, Gerhard; Freund, Hans‐Joachim
- Physics Today, Vol. 52, Issue 1
Bridging the pressure and materials gaps between catalysis and surface science: clean and modified oxide surfaces
journal, June 2001
- Freund, H. -J.; Kuhlenbeck, H.; Libuda, J.
- Topics in Catalysis, Vol. 15, Issue 2/4, p. 201-209
Adsorption and reaction of CO on RuO2(110) surfaces
journal, June 2001
- Wang, J.; Fan, C. Y.; Jacobi, K.
- Surface Science, Vol. 481, Issue 1-3
CO adsorption and dissociation on Ru(0001) at elevated pressures
journal, February 2013
- Starr, David E.; Bluhm, Hendrik
- Surface Science, Vol. 608
Effects of Residual Solvent Molecules Facilitating the Infiltration Synthesis of ZnO in a Nonreactive Polymer
journal, May 2017
- Ye, Xinyi; Kestell, John; Kisslinger, Kim
- Chemistry of Materials, Vol. 29, Issue 10
Infrared Spectra of Monolayers on Metal Mirrors
journal, January 1959
- Francis, S. A.; Ellison, A. H.
- Journal of the Optical Society of America, Vol. 49, Issue 2
In Situ PM-IRRAS Study of Liquid-Phase Benzyl Alcohol Oxidation on Palladium
journal, November 2009
- Meier, Daniel M.; Urakawa, Atsushi; Baiker, Alfons
- The Journal of Physical Chemistry C, Vol. 113, Issue 52
Infrared Study of Adsorbed Molecules on Metal Surfaces by Reflection Techniques
journal, January 1966
- Greenler, Robert G.
- The Journal of Chemical Physics, Vol. 44, Issue 1
Works referencing / citing this record:
Ionization‐Facilitated Formation of 2D (Alumino)Silicate–Noble Gas Clathrate Compounds
journal, March 2019
- Zhong, Jian‐Qiang; Wang, Mengen; Akter, Nusnin
- Advanced Functional Materials, Vol. 29, Issue 20