Development of a reaction cell for in-situ/operando studies of surface of a catalyst under a reaction condition and during catalysis

Luan Nguyen, Franklin (Feng) Tao

Research output: Contribution to journalArticlepeer-review

45 Scopus citations

Abstract

Tracking surface chemistry of a catalyst during catalysis is significant for fundamental understanding of catalytic performance of the catalyst since it allows for establishing an intrinsic correlation between surface chemistry of a catalyst at its working status and its corresponding catalytic performance. Ambient pressure X-ray photoelectron spectroscopy can be used for in-situ studies of surfaces of different materials or devices in a gas. To simulate the gaseous environment of a catalyst in a fixed-bed a flowing gaseous environment of reactants around the catalyst is necessary. Here, we report the development of a new flowing reaction cell for simulating in-situ study of a catalyst surface under a reaction condition in gas of one reactant or during catalysis in a mixture of reactants of a catalytic reaction. The homemade reaction cell is installed in a high vacuum (HV) or ultrahigh vacuum (UHV) environment of a chamber. The flowing gas in the reaction cell is separated from the HV or UHV environment through well sealings at three interfaces between the reaction cell and X-ray window, sample door and aperture of front cone of an energy analyzer. Catalyst in the cell is heated through infrared laser beam introduced through a fiber optics interfaced with the reaction cell through a homemade feedthrough. The highly localized heating on the sample holder and Au-passivated internal surface of the reaction cell effectively minimizes any unwanted reactions potentially catalyzed by the reaction cell. The incorporated laser heating allows a fast heating and a high thermal stability of the sample at a high temperature. With this cell, a catalyst at 800 °C in a flowing gas can be tracked readily.
Original languageEnglish (US)
Pages (from-to)064101
JournalReview of Scientific Instruments
Volume87
Issue number6
DOIs
StatePublished - Jun 7 2016
Externally publishedYes

Bibliographical note

KAUST Repository Item: Exported on 2022-06-01
Acknowledged KAUST grant number(s): OCRF-2014-CRG3-62140393
Acknowledgements: This cell was built at University of Notre Dame. The new energy analyzer and Al K alpha X-source of this system were purchased through NSF-CHE-1462121, DE-FG02-12ER1635, NSF-CBET-1264798 at Notre Dame and are now located in Tao group at University of Kansas. This work was supported by the Chemical Sciences, Geosciences and Biosciences Division, Office of Basic Energy Sciences, Office of Science, U.S. Department of Energy under Grant No. DE-SC0014561, Chemical Catalysis Program of Division of Chemistry of National Science Foundation (NSF Career Award) NSF-CHE-1462121, CBET Division of National Science Foundation NSF-CBET-1264798, King Abdullah University of Science and Technology (KAUST) Office of Sponsored Research (OSR) under Award No: OCRF-2014-CRG3-62140393, Energy Frontier Research Center (Integrated Mesoscale Architectures for Sustainable Catalysis at Harvard University) funded by the US Department of Energy, Office of Science, Basic Energy Sciences under Award No. DE- SC0012573, and ARPA-REBEL program of US Department of Energy under award number DE-AR0000502.
This publication acknowledges KAUST support, but has no KAUST affiliated authors.

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