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Applying X-ray Imaging Crystal Spectroscopy for Use as a High Temperature Plasma Diagnostic

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High-throughput operando-ready X-ray absorption spectroscopy flow reactor cell for powder samples.

James D Kammert¹, Gordon Brezicki¹, Raul Acevedo-Esteves²

¹Department of Chemical Engineering, University of Virginia, 102 Engineer's Way, P.O. Box 400741, Charlottesville, Virginia 22904-4741, USA.

The Review of Scientific Instruments

|February 5, 2020

Summary

A new X-ray absorption spectroscopy cell enables high-throughput catalytic reaction studies under various conditions. This operando-ready system simplifies in-situ analysis for advanced materials research.

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Area of Science:

Materials Science
Chemical Engineering
Spectroscopy

Background:

In-situ characterization is crucial for understanding catalytic mechanisms.
Existing methods often lack the throughput or operational flexibility needed for complex reactions.
Operando X-ray absorption spectroscopy (XAS) provides detailed electronic and structural information.

Purpose of the Study:

To design and demonstrate a high-throughput, operando-ready X-ray absorption spectroscopy (XAS) catalytic reaction cell.
To enable simultaneous collection of XAS spectra from multiple parallel reactors under diverse reaction conditions.
To facilitate straightforward use in synchrotron-based experiments.

Main Methods:

A novel catalytic reaction cell with 4 parallel reactors was engineered.
The cell supports temperatures up to 773 K and pressures up to 2 MPa.
Operando XAS (X-ray absorption near edge structure and extended fine structure) data were collected under reaction conditions.

Main Results:

The cell successfully collected operando XAS spectra from four parallel reactors simultaneously.
The system demonstrated robust performance across a range of temperatures, pressures, and gas environments.
Mechanical simplicity and programmable operation at beamline 8-ID (NSLS-II) were confirmed.

Conclusions:

The developed XAS reaction cell significantly enhances throughput for in-situ catalytic studies.
This versatile tool simplifies the investigation of reaction mechanisms under industrially relevant conditions.
The design offers a practical solution for advanced materials and catalysis research.