Direct Observation of Plasma-Stimulated Activation of Surface Species Using Multimodal In Situ/Operando Spectroscopy Combining Polarization-Modulation Infrared Reflection-Absorption Spectroscopy, Optical Emission Spectroscopy, and Mass Spectrometry

Lee, Garam; Go, David B.; O’Brien, Casey P.

doi:10.1021/acsami.1c18169

Direct Observation of Plasma-Stimulated Activation of Surface Species Using Multimodal In Situ/Operando Spectroscopy Combining Polarization-Modulation Infrared Reflection-Absorption Spectroscopy, Optical Emission Spectroscopy, and Mass Spectrometry

Journal Article · Wed Nov 17 00:00:00 EST 2021 · ACS Applied Materials and Interfaces

DOI:https://doi.org/10.1021/acsami.1c18169· OSTI ID:1902885

^[1]; ^[2]; ^[2]

Univ. of Notre Dame, IN (United States); University of Notre Dame
Univ. of Notre Dame, IN (United States)

Nonthermal plasmas (NTPs) produce reactive chemical environments, including electrons, ions, radicals, and vibrationally excited molecules, that can drive chemistry at temperatures at which such species are thermally inaccessible. There has been growing interest in the integration of conventional catalysis with reactive NTPs to promote novel chemical transformations. Unveiling the full potential of plasma-catalytic processes requires a comprehensive understanding of plasma-catalytic synergies, including characterization of plasma-catalytic surface interactions. In this work, we report on a newly designed multimodal spectroscopic instrument combining polarization-modulation infrared reflection-absorption spectroscopy (PM-IRAS), mass spectrometry, and optical emission spectroscopy (OES) for the investigation of plasma–surface interactions such as those found in plasma catalysis. In particular, this tool has been utilized to correlate plasma-phase chemistry with both surface chemistry and gas-phase products in situ (1) during the deposition of carbonaceous surface species via NTP-promoted nonoxidative coupling of methane and (2) during subsequent activation of surface deposits with an atmospheric pressure and temperature argon plasma jet on both nickel (Ni) and silicon dioxide (SiO₂) surfaces. For the first time, the activation of carbonaceous surface species by a NTP on Ni and SiO₂ surfaces to form hydrogen gas and C₂ hydrocarbons was directly observed, where both PM-IRAS and OES measurements suggest that they may form through different pathways. Furthermore, this unique tool for studying plasma–surface interactions could enable more rational design of plasma-stimulated catalytic processes.

View Accepted Manuscript (DOE)

Research Organization:: Univ. of Notre Dame, IN (United States)

Sponsoring Organization:: USDOE

Grant/Contract Number:: FE0031862

OSTI ID:: 1902885

Journal Information:: ACS Applied Materials and Interfaces, Journal Name: ACS Applied Materials and Interfaces Journal Issue: 47 Vol. 13; ISSN 1944-8244

Publisher:: American Chemical Society (ACS)Copyright Statement

Country of Publication:: United States

Language:: English

References (65)

Infrared Spectroscopy: Fundamentals and Applications Stuart, Barbara H. Analytical Techniques in the Sciences https://doi.org/10.1002/0470011149	book	June 2004
Probing the Role of a Non-Thermal Plasma (NTP) in the Hybrid NTP Catalytic Oxidation of Methane Gibson, Emma K.; Stere, Cristina E.; Curran-McAteer, Bronagh Angewandte Chemie International Edition, Vol. 56, Issue 32 https://doi.org/10.1002/anie.201703550	journal	July 2017
Direct Coupling of Bromine-Mediated Methane Activation and Carbon-Deposit Gasification Osterwalder, Neil; Stark, Wendelin J. ChemPhysChem, Vol. 8, Issue 2 https://doi.org/10.1002/cphc.200600491	journal	February 2007
From Carbon Nanostructures to New Photoluminescence Sources: An Overview of New Perspectives and Emerging Applications of Low-Pressure PECVD Gordillo-Vázquez, F. J.; Herrero, V. J.; Tanarro, I. Chemical Vapor Deposition, Vol. 13, Issue 6-7 https://doi.org/10.1002/cvde.200604034	journal	July 2007
Methane Oligomerization in a Dielectric Barrier Discharge at Atmospheric Pressure Scarduelli, Giorgina; Guella, Graziano; Mancini, Ines Plasma Processes and Polymers, Vol. 6, Issue 1 https://doi.org/10.1002/ppap.200800096	journal	January 2009
Insights into the Mechanisms of Isopropanol Conversion on γ-Al2O3 by Dielectric Barrier Discharge Rivallan, Mickaël; Fourré, Elodie; Aiello, Sébastien Plasma Processes and Polymers, Vol. 9, Issue 9 https://doi.org/10.1002/ppap.201200021	journal	June 2012
The Identification of Molecular Spectra Pearse, R. W. B.; Gaydon, A. G. Journal of Physical Chemistry ABC, Vol. 55, Issue 5, P.758-759 https://doi.org/10.1007/978-94-009-5758-9	book	January 1976
Operando DRIFT Spectroscopy Characterization of Intermediate Species on Catalysts Surface in VOC Removal from Air by Non-thermal Plasma Assisted Catalysis Rodrigues, Anthony; Tatibouët, Jean-Michel; Fourré, Elodie Plasma Chemistry and Plasma Processing, Vol. 36, Issue 4 https://doi.org/10.1007/s11090-016-9718-1	journal	May 2016
Atomistic simulations of plasma catalytic processes Neyts, Erik C. Frontiers of Chemical Science and Engineering, Vol. 12, Issue 1 https://doi.org/10.1007/s11705-017-1674-7	journal	September 2017
Differential reflection spectroscopy of very thin surface films McIntyre, J. D. E.; Aspnes, D. E. Surface Science, Vol. 24, Issue 2 https://doi.org/10.1016/0039-6028(71)90272-X	journal	February 1971
Mechanisms of plasma polymerization of various silico-organic monomers Rau, Christiane; Kulisch, Wilhelm Thin Solid Films, Vol. 249, Issue 1 https://doi.org/10.1016/0040-6090(94)90081-7	journal	September 1994
Surface studies of supported model catalysts Henry, Claude R. Surface Science Reports, Vol. 31, Issue 7-8 https://doi.org/10.1016/S0167-5729(98)00002-8	journal	January 1998
IR spectroscopy in catalysis Ryczkowski, Janusz Catalysis Today, Vol. 68, Issue 4 https://doi.org/10.1016/S0920-5861(01)00334-0	journal	July 2001
Plasma-assisted methane conversion in an atmospheric pressure dielectric barrier discharge reactor Xu, Chao; Tu, Xin Journal of Energy Chemistry, Vol. 22, Issue 3 https://doi.org/10.1016/S2095-4956(13)60055-8	journal	May 2013
Combining non-thermal plasma with heterogeneous catalysis in waste gas treatment: A review Van Durme, Jim; Dewulf, Jo; Leys, Christophe Applied Catalysis B: Environmental, Vol. 78, Issue 3-4 https://doi.org/10.1016/j.apcatb.2007.09.035	journal	February 2008
Review of plasma catalysis on hydrocarbon reforming for hydrogen production—Interaction, integration, and prospects Chen, H.; Lee, H.; Chen, S. Applied Catalysis B: Environmental, Vol. 85, Issue 1-2 https://doi.org/10.1016/j.apcatb.2008.06.021	journal	December 2008
Fabrication of vertically aligned single-walled carbon nanotubes in atmospheric pressure non-thermal plasma CVD Nozaki, Tomohiro; Ohnishi, Kuma; Okazaki, Ken Carbon, Vol. 45, Issue 2 https://doi.org/10.1016/j.carbon.2006.09.009	journal	February 2007
Growth of graphene on Cu by plasma enhanced chemical vapor deposition Terasawa, Tomo-o; Saiki, Koichiro Carbon, Vol. 50, Issue 3 https://doi.org/10.1016/j.carbon.2011.09.047	journal	March 2012
Diagnosis of atmospheric pressure low temperature plasma and application to high efficient methane conversion Kado, Shigeru; Sekine, Yasushi; Nozaki, Tomohiro Catalysis Today, Vol. 89, Issue 1-2 https://doi.org/10.1016/j.cattod.2003.11.036	journal	February 2004
Non-thermal plasma catalysis of methane: Principles, energy efficiency, and applications Nozaki, Tomohiro; Okazaki, Ken Catalysis Today, Vol. 211 https://doi.org/10.1016/j.cattod.2013.04.002	journal	August 2013
Plasma N2-fixation: 1900–2014 Patil, B. S.; Wang, Q.; Hessel, V. Catalysis Today, Vol. 256 https://doi.org/10.1016/j.cattod.2015.05.005	journal	November 2015
Advances in methane conversion processes Wang, Bingwen; Albarracín-Suazo, Sandra; Pagán-Torres, Yomaira Catalysis Today, Vol. 285 https://doi.org/10.1016/j.cattod.2017.01.023	journal	May 2017
Catalyst-assisted DBD plasma for coupling of methane: Minimizing carbon-deposits by structured reactors García-Moncada, Nuria; van Rooij, Gerard; Cents, Toine Catalysis Today, Vol. 369 https://doi.org/10.1016/j.cattod.2020.04.028	journal	June 2021
The panorama of plasma-assisted non-oxidative methane reforming Scapinello, Marco; Delikonstantis, Evangelos; Stefanidis, Georgios D. Chemical Engineering and Processing: Process Intensification, Vol. 117 https://doi.org/10.1016/j.cep.2017.03.024	journal	July 2017
Methane conversion to H2 and higher hydrocarbons using non-thermal plasma dielectric barrier discharge reactor Saleem, Faisal; Kennedy, Jonathan; Dahiru, Usman H. Chemical Engineering and Processing - Process Intensification, Vol. 142 https://doi.org/10.1016/j.cep.2019.107557	journal	August 2019
Recent advances in high-growth rate single-crystal CVD diamond Liang, Qi; Yan, Chih-shiue; Meng, Yufei Diamond and Related Materials, Vol. 18, Issue 5-8 https://doi.org/10.1016/j.diamond.2008.12.002	journal	May 2009
Microporous organosilica membranes for gas separation prepared via PECVD using different O/Si ratio precursors Nagasawa, Hiroki; Minamizawa, Toshihiro; Kanezashi, Masakoto Journal of Membrane Science, Vol. 489 https://doi.org/10.1016/j.memsci.2015.04.011	journal	September 2015
Plasma Catalysis: Synergistic Effects at the Nanoscale Neyts, Erik C.; Ostrikov, Kostya (Ken); Sunkara, Mahendra K. Chemical Reviews, Vol. 115, Issue 24 https://doi.org/10.1021/acs.chemrev.5b00362	journal	November 2015
Plasma-Based CH ₄ Conversion into Higher Hydrocarbons and H ₂ : Modeling to Reveal the Reaction Mechanisms of Different Plasma Sources Heijkers, Stijn; Aghaei, Maryam; Bogaerts, Annemie The Journal of Physical Chemistry C, Vol. 124, Issue 13 https://doi.org/10.1021/acs.jpcc.0c00082	journal	March 2020
Identifying Surface Reaction Intermediates in Plasma Catalytic Ammonia Synthesis Winter, Lea R.; Ashford, Bryony; Hong, Jungmi ACS Catalysis, Vol. 10, Issue 24 https://doi.org/10.1021/acscatal.0c03166	journal	December 2020
Toward Benchmarking in Catalysis Science: Best Practices, Challenges, and Opportunities Bligaard, Thomas; Bullock, R. Morris; Campbell, Charles T. ACS Catalysis, Vol. 6, Issue 4 https://doi.org/10.1021/acscatal.6b00183	journal	March 2016
Inelastic Neutron Scattering Observation of Plasma-Promoted Nitrogen Reduction Intermediates on Ni/γ-Al ₂ O ₃ Barboun, Patrick M.; Daemen, Luke L.; Waitt, Craig ACS Energy Letters, Vol. 6, Issue 6 https://doi.org/10.1021/acsenergylett.1c00643	journal	May 2021
Enhancing C–H Bond Activation of Methane via Temperature-Controlled, Catalyst–Plasma Interactions Kim, Jongsik; Abbott, Marshall S.; Go, David B. ACS Energy Letters, Vol. 1, Issue 1 https://doi.org/10.1021/acsenergylett.6b00051	journal	May 2016
Catalysis Enabled by Plasma Activation of Strong Chemical Bonds: A Review Mehta, Prateek; Barboun, Patrick; Go, David B. ACS Energy Letters, Vol. 4, Issue 5 https://doi.org/10.1021/acsenergylett.9b00263	journal	April 2019
Predicted Influence of Plasma Activation on Nonoxidative Coupling of Methane on Transition Metal Catalysts Engelmann, Yannick; Mehta, Prateek; Neyts, Erik C. ACS Sustainable Chemistry & Engineering, Vol. 8, Issue 15 https://doi.org/10.1021/acssuschemeng.0c00906	journal	March 2020
Distinguishing Plasma Contributions to Catalyst Performance in Plasma-Assisted Ammonia Synthesis Barboun, Patrick; Mehta, Prateek; Herrera, Francisco A. ACS Sustainable Chemistry & Engineering, Vol. 7, Issue 9 https://doi.org/10.1021/acssuschemeng.9b00406	journal	March 2019
Vibrationally Excited Activation of N ₂ in Plasma-Enhanced Catalytic Ammonia Synthesis: A Kinetic Analysis Rouwenhorst, Kevin H. R.; Kim, Hyun-Ha; Lefferts, Leon ACS Sustainable Chemistry & Engineering, Vol. 7, Issue 20 https://doi.org/10.1021/acssuschemeng.9b04997	journal	September 2019
Probing a Non-Thermal Plasma Activated Heterogeneously Catalyzed Reaction Using in Situ DRIFTS-MS Stere, C. E.; Adress, W.; Burch, R. ACS Catalysis, Vol. 5, Issue 2 https://doi.org/10.1021/cs5019265	journal	January 2015
Catalytic Nonthermal Plasma Reactor for Dry Reforming of Methane Mahammadunnisa, Sk.; Manoj Kumar Reddy, P.; Ramaraju, B. Energy & Fuels, Vol. 27, Issue 8 https://doi.org/10.1021/ef302193e	journal	March 2013
Infrared reflection-absorption spectroscopy of surface species: a comparison of Fourier transform and dispersion methods Golden, William G.; Saperstein, David D.; Severson, Mark W. The Journal of Physical Chemistry, Vol. 88, Issue 3 https://doi.org/10.1021/j150647a049	journal	February 1984
Chemical Reaction Studies in CH ₄ /Ar and CH ₄ /N ₂ Gas Mixtures of a Dielectric Barrier Discharge Majumdar, Abhijit; Behnke, Jürgen F.; Hippler, Rainer The Journal of Physical Chemistry A, Vol. 109, Issue 41 https://doi.org/10.1021/jp053588a	journal	September 2005
Overcoming ammonia synthesis scaling relations with plasma-enabled catalysis Mehta, Prateek; Barboun, Patrick; Herrera, Francisco A. Nature Catalysis, Vol. 1, Issue 4 https://doi.org/10.1038/s41929-018-0045-1	journal	April 2018
Mind the gap Esposita, David Nature Catalysis, Vol. 1, Issue 11, p. 807-808 https://doi.org/10.1038/s41929-018-0188-0	journal	November 2018
Methane activation: the past and future Tang, Pei; Zhu, Qingjun; Wu, Zhaoxuan Energy Environ. Sci., Vol. 7, Issue 8 https://doi.org/10.1039/C4EE00604F	journal	January 2014
Synergistic effects of plasma–catalyst interactions for CH ₄ activation Kim, Jongsik; Go, David B.; Hicks, Jason C. Physical Chemistry Chemical Physics, Vol. 19, Issue 20 https://doi.org/10.1039/C7CP01322A	journal	January 2017
A design of a fixed bed plasma DRIFTS cell for studying the NTP-assisted heterogeneously catalysed reactions Stere, Cristina; Chansai, Sarayute; Gholami, Rahman Catalysis Science & Technology, Vol. 10, Issue 5 https://doi.org/10.1039/D0CY00036A	journal	January 2020
Helium atmospheric pressure plasma jets touching dielectric and metal surfaces Norberg, Seth A.; Johnsen, Eric; Kushner, Mark J. Journal of Applied Physics, Vol. 118, Issue 1 https://doi.org/10.1063/1.4923345	journal	July 2015
Plasma medicine—current state of research and medical application Weltmann, K-D; von Woedtke, Th Plasma Physics and Controlled Fusion, Vol. 59, Issue 1 https://doi.org/10.1088/0741-3335/59/1/014031	journal	November 2016
Interfacial reactions between DBD and porous catalyst in dry methane reforming Kameshima, Seigo; Mizukami, Ryo; Yamazaki, Takumi Journal of Physics D: Applied Physics, Vol. 51, Issue 11 https://doi.org/10.1088/1361-6463/aaad7d	journal	February 2018
The impact of transition metal catalysts on macroscopic dielectric barrier discharge (DBD) characteristics in an ammonia synthesis plasma catalysis reactor Herrera, Francisco A.; Brown, Gabriel H.; Barboun, Patrick Journal of Physics D: Applied Physics, Vol. 52, Issue 22 https://doi.org/10.1088/1361-6463/ab0c58	journal	March 2019
Mechanistic aspects of plasma-enhanced catalytic methane decomposition by time-resolved operando diffuse reflectance infrared Fourier transform spectroscopy Zhang, S.; Li, Y.; Knoll, A. Journal of Physics D: Applied Physics, Vol. 53, Issue 21 https://doi.org/10.1088/1361-6463/ab795b	journal	March 2020
Development of a small-scale helical surface dielectric barrier discharge for characterizing plasma–surface interfaces Turan, Nazli; Barboun, Patrick M.; Nayak, Pritam K. Journal of Physics D: Applied Physics, Vol. 53, Issue 27 https://doi.org/10.1088/1361-6463/ab8320	journal	May 2020
The 2020 plasma catalysis roadmap Bogaerts, Annemie; Tu, Xin; Whitehead, J. Christopher Journal of Physics D: Applied Physics, Vol. 53, Issue 44 https://doi.org/10.1088/1361-6463/ab9048	journal	August 2020
Investigation of plasma dynamics and spatially varying O and OH concentrations in atmospheric pressure plasma jets impinging on glass, water and metal substrates Yue, Yuanfu; Pei, Xuekai; Gidon, Dogan Plasma Sources Science and Technology, Vol. 27, Issue 6 https://doi.org/10.1088/1361-6595/aac618	journal	June 2018
Plasma bullet propagation and reflection from metallic and dielectric targets Babaeva, Natalia Yu; Naidis, George V.; Panov, Vladislav A. Plasma Sources Science and Technology, Vol. 28, Issue 9 https://doi.org/10.1088/1361-6595/ab36d3	journal	September 2019
Rapid contamination during storage of carbonaceous chondrites prepared for micro FTIR measurements Kebukawa, Yoko; Nakashima, Satoru; Otsuka, Takahiro Meteoritics & Planetary Science, Vol. 44, Issue 4 https://doi.org/10.1111/j.1945-5100.2009.tb00750.x	journal	April 2009
Plasma deposition of optical films and coatings: A review Martinu, Ludvik; Poitras, Daniel Journal of Vacuum Science & Technology A: Vacuum, Surfaces, and Films, Vol. 18, Issue 6 https://doi.org/10.1116/1.1314395	journal	November 2000
Plasma etching: Yesterday, today, and tomorrow Donnelly, Vincent M.; Kornblit, Avinoam Journal of Vacuum Science & Technology A: Vacuum, Surfaces, and Films, Vol. 31, Issue 5 https://doi.org/10.1116/1.4819316	journal	September 2013
Influence of the Plasma Condition on the Morphology of Vertically Aligned Carbon Nanotube Films Grown by RF Plasma Chemical Vapor Deposition Ikuno, Takashi; Takahashi, Syunji; Kamada, Kazunori Surface Review and Letters, Vol. 10, Issue 04 https://doi.org/10.1142/S0218625X03005505	journal	August 2003
A Selection of Recent Advances in C1 Chemistry Mesters, Carl Annual Review of Chemical and Biomolecular Engineering, Vol. 7, Issue 1 https://doi.org/10.1146/annurev-chembioeng-080615-034616	journal	June 2016
Unconventional Catalytic Approaches to Ammonia Synthesis Barboun, Patrick M.; Hicks, Jason C. Annual Review of Chemical and Biomolecular Engineering, Vol. 11, Issue 1 https://doi.org/10.1146/annurev-chembioeng-092319-080240	journal	June 2020
The “Refractor”: A Refractive Grazing Incidence Specular Reflection Attachment Harrick, N. J.; Milosevic, Milan Applied Spectroscopy, Vol. 44, Issue 3 https://doi.org/10.1366/0003702904086281	journal	March 1990
Polarization Modulation FT-IR Spectroscopy of Surfaces and Ultra-Thin Films: Experimental Procedure and Quantitative Analysis Buffeteau, T.; Desbat, B.; Turlet, J. M. Applied Spectroscopy, Vol. 45, Issue 3 https://doi.org/10.1366/0003702914337308	journal	March 1991
Computational chemistry applied to vibrational spectroscopy: A tool for characterization of nucleic acid bases and some of their 5-substituted derivatives Palafox, M. Alcolea Physical Sciences Reviews, Vol. 2, Issue 8 https://doi.org/10.1515/psr-2016-0132	journal	August 2017
Modulation Excitation PM-IRRAS: A New Possibility for Simultaneous Monitoring of Surface and Gas Species and Surface Properties Urakawa, Atsushi; Bürgi, Thomas; Baiker, Alfons CHIMIA International Journal for Chemistry, Vol. 60, Issue 4 https://doi.org/10.2533/000942906777674949	journal	April 2006

Similar Records

Nonthermal Plasma-Stimulated C–N Coupling from CH₄ and N₂ Depends on the Presence of Surface CH_x and Plasma-Phase CN Species

Journal Article · Sun May 19 20:00:00 EDT 2024 · ACS Applied Materials and Interfaces · OSTI ID:2564870

Observation and Characterization of Vibrationally Active Surface Species Accessed with Nonthermal Nitrogen Plasmas

Journal Article · Thu Jan 18 19:00:00 EST 2024 · ACS Applied Materials and Interfaces · OSTI ID:2297420

Related Subjects

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
MS
OES
PM-IRAS
carbon deposits
deposition
hydrocarbons
methane coupling
multimodal spectroscopy
nonthermal plasma
plasma
spectroscopy
surface chemistry

Direct Observation of Plasma-Stimulated Activation of Surface Species Using Multimodal In Situ/Operando Spectroscopy Combining Polarization-Modulation Infrared Reflection-Absorption Spectroscopy, Optical Emission Spectroscopy, and Mass Spectrometry

Citation Formats

References (65)

Similar Records

Related Subjects