Near total reflection x-ray photoelectron spectroscopy: quantifying chemistry at solid/liquid and solid/solid interfaces
Abstract
Near total reflection regime has been widely used in x-ray science, specifically in grazing incidence small angle x-ray scattering and in hard x-ray photoelectron spectroscopy (XPS). In this work, we introduce some practical aspects of using near total reflection (NTR) in ambient pressure XPS and apply this technique to study chemical concentration gradients in a substrate/photoresist system. Experimental data are accompanied by x-ray optical and photoemission simulations to quantitatively probe the photoresist and the interface with the depth accuracy of ~1 nm. Together, our calculations and experiments confirm that NTR XPS is a suitable method to extract information from buried interfaces with highest depth-resolution, which can help address open research questions regarding our understanding of concentration profiles, electrical gradients, and charge transfer phenomena at such interfaces. Furthermore, the presented methodology is especially attractive for solid/liquid interface studies, since it provides all the strengths of a Bragg-reflection standing-wave spectroscopy without the need of an artificial multilayer mirror serving as a standing wave generator, thus dramatically simplifying the sample synthesis.
- Authors:
-
- Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States); Carnegie Mellon Univ., Pittsburgh, PA (United States)
- Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States); Univ. of California, Davis, CA (United States)
- Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States)
- Univ. of California, Davis, CA (United States)
- Univ. of Twente (The Netherlands)
- Univ. of California, Davis, CA (United States); Forschungszentrum Juelich (Germany)
- Publication Date:
- Research Org.:
- Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States); Univ. of California, Davis, CA (United States)
- Sponsoring Org.:
- USDOE Office of Science (SC)
- OSTI Identifier:
- 1834590
- Alternate Identifier(s):
- OSTI ID: 1866267
- Grant/Contract Number:
- AC02-05CH11231; SC0014697
- Resource Type:
- Accepted Manuscript
- Journal Name:
- Journal of Physics. D, Applied Physics
- Additional Journal Information:
- Journal Volume: 54; Journal Issue: 46; Journal ID: ISSN 0022-3727
- Publisher:
- IOP Publishing
- Country of Publication:
- United States
- Language:
- English
- Subject:
- 37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY; X-ray photoelectron spectroscopy; near total reflection; solid/liquid interface; solid/solid interface; photoresist
Citation Formats
Martins, H. P., Conti, G., Cordova, I., Falling, L., Kersell, H., Salmassi, F., Gullikson, E., Vishik, I., Baeumer, C., Naulleau, P., Schneider, C. M., and Nemsak, S. Near total reflection x-ray photoelectron spectroscopy: quantifying chemistry at solid/liquid and solid/solid interfaces. United States: N. p., 2021.
Web. doi:10.1088/1361-6463/ac2067.
Martins, H. P., Conti, G., Cordova, I., Falling, L., Kersell, H., Salmassi, F., Gullikson, E., Vishik, I., Baeumer, C., Naulleau, P., Schneider, C. M., & Nemsak, S. Near total reflection x-ray photoelectron spectroscopy: quantifying chemistry at solid/liquid and solid/solid interfaces. United States. https://doi.org/10.1088/1361-6463/ac2067
Martins, H. P., Conti, G., Cordova, I., Falling, L., Kersell, H., Salmassi, F., Gullikson, E., Vishik, I., Baeumer, C., Naulleau, P., Schneider, C. M., and Nemsak, S. Wed .
"Near total reflection x-ray photoelectron spectroscopy: quantifying chemistry at solid/liquid and solid/solid interfaces". United States. https://doi.org/10.1088/1361-6463/ac2067. https://www.osti.gov/servlets/purl/1834590.
@article{osti_1834590,
title = {Near total reflection x-ray photoelectron spectroscopy: quantifying chemistry at solid/liquid and solid/solid interfaces},
author = {Martins, H. P. and Conti, G. and Cordova, I. and Falling, L. and Kersell, H. and Salmassi, F. and Gullikson, E. and Vishik, I. and Baeumer, C. and Naulleau, P. and Schneider, C. M. and Nemsak, S.},
abstractNote = {Near total reflection regime has been widely used in x-ray science, specifically in grazing incidence small angle x-ray scattering and in hard x-ray photoelectron spectroscopy (XPS). In this work, we introduce some practical aspects of using near total reflection (NTR) in ambient pressure XPS and apply this technique to study chemical concentration gradients in a substrate/photoresist system. Experimental data are accompanied by x-ray optical and photoemission simulations to quantitatively probe the photoresist and the interface with the depth accuracy of ~1 nm. Together, our calculations and experiments confirm that NTR XPS is a suitable method to extract information from buried interfaces with highest depth-resolution, which can help address open research questions regarding our understanding of concentration profiles, electrical gradients, and charge transfer phenomena at such interfaces. Furthermore, the presented methodology is especially attractive for solid/liquid interface studies, since it provides all the strengths of a Bragg-reflection standing-wave spectroscopy without the need of an artificial multilayer mirror serving as a standing wave generator, thus dramatically simplifying the sample synthesis.},
doi = {10.1088/1361-6463/ac2067},
journal = {Journal of Physics. D, Applied Physics},
number = 46,
volume = 54,
place = {United States},
year = {Wed Sep 08 00:00:00 EDT 2021},
month = {Wed Sep 08 00:00:00 EDT 2021}
}
Works referenced in this record:
Fundamental understanding of chemical processes in extreme ultraviolet resist materials
journal, October 2018
- Kostko, Oleg; Xu, Bo; Ahmed, Musahid
- The Journal of Chemical Physics, Vol. 149, Issue 15
High Sensitivity Resists for EUV Lithography: A Review of Material Design Strategies and Performance Results
journal, August 2020
- Manouras, Theodore; Argitis, Panagiotis
- Nanomaterials, Vol. 10, Issue 8
Investigation of solid/vapor interfaces using ambient pressure X-ray photoelectron spectroscopy
journal, January 2013
- Starr, D. E.; Liu, Z.; Hävecker, M.
- Chemical Society Reviews, Vol. 42, Issue 13
Atomic subshell photoionization cross sections and asymmetry parameters: 1 ⩽ Z ⩽ 103
journal, January 1985
- Yeh, J. J.; Lindau, I.
- Atomic Data and Nuclear Data Tables, Vol. 32, Issue 1
Perspective—Outlook on Operando Photoelectron and Absorption Spectroscopy to Probe Catalysts at the Solid-Liquid Electrochemical Interface
journal, January 2020
- Carbonio, Emilia A.; Velasco-Velez, Juan-Jesus; Schlögl, Robert
- Journal of The Electrochemical Society, Vol. 167, Issue 5
X-ray diffraction from Si/Ge layers: Diffuse scattering in the region of total external reflection
journal, January 1995
- Schlomka, J. -P.; Tolan, M.; Schwalowsky, L.
- Physical Review B, Vol. 51, Issue 4
Present and new frontiers in materials research by ambient pressure x-ray photoelectron spectroscopy
journal, July 2020
- Schnadt, Joachim; Knudsen, Jan; Johansson, Niclas
- Journal of Physics: Condensed Matter, Vol. 32, Issue 41
Surface Studies of Solids by Total Reflection of X-Rays
journal, July 1954
- Parratt, L. G.
- Physical Review, Vol. 95, Issue 2
Operando characterization of interfacial charge transfer processes
journal, May 2021
- Baeumer, Christoph
- Journal of Applied Physics, Vol. 129, Issue 17
Aqueous solution/metal interfaces investigated in operando by photoelectron spectroscopy
journal, January 2015
- Karslıoğlu, O.; Nemšák, S.; Zegkinoglou, I.
- Faraday Discussions, Vol. 180
Interface Science Using Ambient Pressure Hard X-ray Photoelectron Spectroscopy
journal, January 2019
- Favaro, Marco; Abdi, Fatwa; Crumlin, Ethan
- Surfaces, Vol. 2, Issue 1
Making use of x-ray optical effects in photoelectron-, Auger electron-, and x-ray emission spectroscopies: Total reflection, standing-wave excitation, and resonant effects
journal, February 2013
- Yang, S. -H.; Gray, A. X.; Kaiser, A. M.
- Journal of Applied Physics, Vol. 113, Issue 7
Concentration and chemical-state profiles at heterogeneous interfaces with sub-nm accuracy from standing-wave ambient-pressure photoemission
journal, November 2014
- Nemšák, Slavomír; Shavorskiy, Andrey; Karslioglu, Osman
- Nature Communications, Vol. 5, Issue 1
Interface properties of magnetic tunnel junction superlattices studied by standing-wave excited photoemission spectroscopy
journal, November 2010
- Gray, A. X.; Papp, C.; Balke, B.
- Physical Review B, Vol. 82, Issue 20
Depth Profiling Charge Accumulation from a Ferroelectric into a Doped Mott Insulator
journal, March 2015
- Marinova, Maya; Rault, Julien E.; Gloter, Alexandre
- Nano Letters, Vol. 15, Issue 4
An Efficient Algorithm for Automatic Structure Optimization in X-ray Standing-Wave Experiments
journal, January 2019
- Karslıoğlu, Osman; Gehlmann, Mathias; Müller, Juliane
- Journal of Electron Spectroscopy and Related Phenomena, Vol. 230
Some future perspectives in soft- and hard- X-ray photoemission
journal, August 2014
- Fadley, Charles S.; Nemšák, Slavomir
- Journal of Electron Spectroscopy and Related Phenomena, Vol. 195
Core level photoelectron spectroscopy of heterogeneous reactions at liquid–vapor interfaces: Current status, challenges, and prospects
journal, February 2021
- Dupuy, Rémi; Richter, Clemens; Winter, Bernd
- The Journal of Chemical Physics, Vol. 154, Issue 6
Calibrated binding energies of some core levels in the energy range between 1.5–4 keV
journal, January 1988
- Huschka, W.; Ross, D.; Maier, M.
- Journal of Electron Spectroscopy and Related Phenomena, Vol. 46, Issue 2
Three-dimensional coherent X-ray surface scattering imaging near total external reflection
journal, August 2012
- Sun, Tao; Jiang, Zhang; Strzalka, Joseph
- Nature Photonics, Vol. 6, Issue 9
A theoritical study on spin coating technique
journal, December 2013
- Tyona, M. D.
- Advances in materials Research, Vol. 2, Issue 4
Energetic, spatial, and momentum character of the electronic structure at a buried interface: The two-dimensional electron gas between two metal oxides
journal, June 2016
- Nemšák, S.; Conti, G.; Gray, A. X.
- Physical Review B, Vol. 93, Issue 24
Waveguide-enhanced grazing-incidence small-angle x-ray scattering of buried nanostructures in thin films
journal, August 2011
- Jiang, Zhang; Lee, Dong Ryeol; Narayanan, Suresh
- Physical Review B, Vol. 84, Issue 7
X-Ray Evanescent-Wave Absorption and Emission
journal, January 1983
- Becker, R. S.; Golovchenko, J. A.; Patel, J. R.
- Physical Review Letters, Vol. 50, Issue 3
Ultrasoft-X-Ray Reflection, Refraction, and Production of Photoelectrons (100-1000-eV Region)
journal, July 1972
- Henke, Burton L.
- Physical Review A, Vol. 6, Issue 1
Combining theory and experiment in electrocatalysis: Insights into materials design
journal, January 2017
- Seh, Zhi Wei; Kibsgaard, Jakob; Dickens, Colin F.
- Science, Vol. 355, Issue 6321
Electron escape depth in silicon
journal, January 1974
- Klasson, M.; Berndtsson, A.; Hedman, J.
- Journal of Electron Spectroscopy and Related Phenomena, Vol. 3, Issue 6
Photoelectron spectroscopy of liquid water and aqueous solution: Electron effective attenuation lengths and emission-angle anisotropy
journal, March 2010
- Ottosson, Niklas; Faubel, Manfred; Bradforth, Stephen E.
- Journal of Electron Spectroscopy and Related Phenomena, Vol. 177, Issue 2-3
Determination of effective attenuation length of slow electrons in polymer films
journal, June 2020
- Ma, J. H.; Naulleau, P.; Ahmed, M.
- Journal of Applied Physics, Vol. 127, Issue 24
Calculations of electron inelastic mean free paths. V. Data for 14 organic compounds over the 50-2000 eV range
journal, March 1994
- Tanuma, S.; Powell, C. J.; Penn, D. R.
- Surface and Interface Analysis, Vol. 21, Issue 3