Skip to main content
OSTI.GOVU.S. Department of Energy Office of Scientific and Technical Information
U.S. Department of Energy
Office of Scientific and Technical Information
 

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

Journal Article · · Review of Scientific Instruments
DOI:https://doi.org/10.1063/1.4946877· OSTI ID:1387868
 [1];  [1]
  1. Univ. of Notre Dame, IN (United States); Univ. of Kansas, Lawrence, KS (United States)
+ Show Author Affiliations
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.
Research Organization:
Energy Frontier Research Centers (EFRC) (United States). Integrated Mesoscale Architectures for Sustainable Catalysis (IMASC)
Sponsoring Organization:
USDOE Office of Science (SC), Basic Energy Sciences (BES) (SC-22)
Grant/Contract Number:
SC0012573
OSTI ID:
1387868
Alternate ID(s):
OSTI ID: 22597983
Journal Information:
Review of Scientific Instruments, Journal Name: Review of Scientific Instruments Journal Issue: 6 Vol. 87; ISSN 0034-6748
Publisher:
American Institute of Physics (AIP)Copyright Statement
Country of Publication:
United States
Language:
English

References (20)

X-ray photoelectron spectroscopy as a tool for in-situ study of the mechanisms of heterogeneous catalytic reactions journal February 2005
On the origin of core-level binding energy shifts journal December 1995
Surface of a catalyst in a gas phase journal May 2016
Ambient pressure photoelectron spectroscopy: A new tool for surface science and nanotechnology journal April 2008
Photoelectron Spectroscopy Study of Stoichiometric and Reduced Anatase TiO 2 (101) Surfaces: The Effect of Subsurface Defects on Water Adsorption at Near-Ambient Pressures journal June 2015
In-Situ Studies of Nanocatalysis journal April 2013
Atomic-Scale Observations of Catalyst Structures under Reaction Conditions and during Catalysis journal March 2016
Design and Performance Aspects of a Custom-Built Ambient Pressure Photoelectron Spectrometer toward Bridging the Pressure Gap: Oxidation of Cu, Ag, and Au Surfaces at 1 mbar O 2 Pressure journal February 2013
Electron Spectroscopy and Chemical Binding journal April 1966
Design of an in-house ambient pressure AP-XPS using a bench-top X-ray source and the surface chemistry of ceria under reaction conditions journal January 2012
Action of bimetallic nanocatalysts under reaction conditions and during catalysis: evolution of chemistry from high vacuum conditions to reaction conditions journal January 2012
A differentially pumped electrostatic lens system for photoemission studies in the millibar range journal November 2002
New setup for in situ x-ray photoelectron spectroscopy from ultrahigh vacuum to 1mbar journal January 2005
A new scanning tunneling microscope reactor used for high-pressure and high-temperature catalysis studies journal August 2008
Angle-resolved environmental X-ray photoelectron spectroscopy: A new laboratory setup for photoemission studies at pressures up to 0.4 Torr journal September 2012
Design of a new reactor-like high temperature near ambient pressure scanning tunneling microscope for catalysis studies journal March 2013
The ReactorSTM: Atomically resolved scanning tunneling microscopy under high-pressure, high-temperature catalytic reaction conditions journal August 2014
Electron Spectroscopy for Chemical Analysis (E.S.C.A.) journal November 1970
The new ambient-pressure X-ray photoelectron spectroscopy instrument at MAX-lab journal August 2012
In Situ Studies of Chemistry and Structure of Materials in Reactive Environments journal January 2011

Cited By (11)

Integrated In Situ Characterization of a Molten Salt Catalyst Surface: Evidence of Sodium Peroxide and Hydroxyl Radical Formation journal July 2017
Established and Emerging Concepts to Treat Imbalances of Iron Homeostasis in Inflammatory Diseases journal December 2018
Catalytic Intermediates of CO 2 Hydrogenation on Cu(111) Probed by In Operando Near-Ambient Pressure Technique journal October 2018
Tuning Pt-CeO2 interactions by high-temperature vapor-phase synthesis for improved reducibility of lattice oxygen journal March 2019
A robust fuel cell operated on nearly dry methane at 500 °C enabled by synergistic thermal catalysis and electrocatalysis journal October 2018
Operando chemistry of catalyst surfaces during catalysis journal January 2017
Transition of surface phase of cobalt oxide during CO oxidation journal January 2018
Interactions of gaseous molecules with X-ray photons and photoelectrons in AP-XPS study of solid surface in gas phase journal January 2018
A high-pressure x-ray photoelectron spectroscopy instrument for studies of industrially relevant catalytic reactions at pressures of several bars journal October 2019
A high-pressure x-ray photoelectron spectroscopy instrument for studies of industrially relevant catalytic reactions at pressures of several bars text January 2019
A high-pressure x-ray photoelectron spectroscopy instrument for studies of industrially relevant catalytic reactions at pressures of several bars text January 2019

Similar Records

Related Subjects

36 MATERIALS SCIENCE
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
catalysis (heterogeneous)
materials and chemistry by design
mesostructured materials
synthesis (novel materials)