Dual reactor for in situ/operando fluorescent mode XAS studies of sample containing low-concentration 3d or 5d metal elements

Nguyen, Luan; Tang, Yu; Li, Yuting; Zhang, Xiaoyan; Wang, Ding; Tao, Franklin Feng

doi:10.1063/1.5022738

Title: Dual reactor for in situ/operando fluorescent mode XAS studies of sample containing low-concentration 3d or 5d metal elements

Journal Article · Fri May 25 00:00:00 EDT 2018 · Review of Scientific Instruments

DOI:https://doi.org/10.1063/1.5022738· OSTI ID:1526016

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^[1]; Zhang, Xiaoyan ^[1]; Wang, Ding ^[1];

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Univ. of Kansas, Lawrence, KS (United States). Dept. of Chemical and Petroleum Engineering. Dept. of Chemistry

Transition metal elements are the most important elements of heterogeneous catalysts used for chemical and energy transformations. Many of these catalysts are active at a temperature higher than 400 °C. For a catalyst containing a 3d or 5d metal element with a low concentration, typically their released fluorescence upon the K-edge or L-edge adsorption of X-rays is collected for the analysis of chemical and coordination environments of these elements. However, it is challenging to perform in situ/operando X-ray absorption spectroscopy (XAS) studies of elements of low-energy absorption edges at a low concentration in a catalyst during catalysis at a temperature higher than about 450 °C. Here a unique reaction system consisting two reactors, called a dual reactor system, was designed for performing in situ or operando XAS studies of these elements of low-energy absorption edges in a catalyst at a low concentration during catalysis at a temperature higher than 450 °C in a fluorescent mode. This dual-reactor system contains a quartz reactor for preforming high-temperature catalysis up to 950 °C and a Kapton reactor remaining at a temperature up to 450 °C for collecting data in the same gas of catalysis. With this dual reactor, chemical and coordination environments of low-concentration metal elements with low-energy absorption edges such as the K-edge of 3d metals including Ti, V, Cr, Mn, Fe, Co, Ni, and Cu and L edge of 5d metals including W, Re, Os, Ir, Pt, and Au can be examined through first performing catalysis at a temperature higher than 450 °C in the quartz reactor and then immediately flipping the catalyst in the same gas flow to the Kapton reactor remained up to 450 °C to collect data. The capability of this dual reactor was demonstrated by tracking the Mn K-edge of the MnO_x/Na₂WO₄ catalyst during activation in the temperature range of 300-900 °C and catalysis at 850 °C.

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Research Organization:: Univ. of Kansas, Lawrence, KS (United States)

Sponsoring Organization:: USDOE Office of Science (SC), Basic Energy Sciences (BES); National Science Foundation (NSF)

Grant/Contract Number:: SC0014561; OIA-1539105

OSTI ID:: 1526016

Journal Information:: Review of Scientific Instruments, Vol. 89, Issue 5; ISSN 0034-6748

Publisher:: American Institute of Physics (AIP)Copyright Statement

Country of Publication:: United States

Language:: English

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Cited by: 8 works

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