Silicon microfabricated reactor for operando XAS/DRIFTS studies of heterogeneous catalytic reactions

Abstract

A novel microreactor for operando XAS and DRIFTS studies of catalytic reactions is reported, exhibiting plug-flow, isothermal behaviour and absence of mass transfer resistances and dead volume, enabling time- and spatially-resolved experiments.

Applications of X-ray Absorption Fine Structure Spectroscopy in the Photocatalytic Conversion of Small Molecules

“…Furthermore, the exploration of structural characterizations at the bulk and surfaces of catalysts is difficult to perform using only a single technique. With the continuous efforts made by researchers, the XAFS technique can be combined with other measurement results to present full-scale details, such as XAFS-XRD, − XAFS/DRIFTS/MS (DRIFT, diffuse reflectance infrared Fourier transform spectroscopy; MS, mass spectrometry) − and the SAXS/XRD/XAFS combined technique . As shown in Figure , the signals of synchrotron radiation-based combined techniques can be obtained simultaneously.…”

“…Synchrotron radiation-based combined techniques: XAFS-XRD, XAFS-DRIFTS, and XAFS-DRIFTS-MS . Reproduced with permission from refs , , and . Copyright 2022 Springer Nature.…”

Tracking the in situ generation of hetero-metal–metal bonds in phosphide electrocatalysts for electrocatalytic hydrogen evolution

“…[26][27][28][29] To resolve this dilemma, advanced in situ characterization methods have provided many new perspectives to realize the real-time catalytic behavior, including the information of atomic configuration and electronic structure of the real active sites during catalysis. [30][31][32][33][34][35][36][37] In the present study, through a controllable phosphatizing reaction on carbon paper, we demonstrate a Ru x @CoP (x = 0.6, 1.2, 1.8, and 2.4) structure with high electrocatalytic performance toward the HER under acidic conditions. We adopted the in situ X-ray absorption spectroscopy (XAS) method to track the atomic-scale structure under electrochemical conditions, from which we revealed a newlyformed Co-Ru moiety around Co sites during the HER.…”

“…26–29 To resolve this dilemma, advanced in situ characterization methods have provided many new perspectives to realize the real-time catalytic behavior, including the information of atomic configuration and electronic structure of the real active sites during catalysis. 30–37…”

Correction: Temperature control in DRIFT cells used for in situ and operando studies: where do we stand today?

“…After the revision of the proofs of this paper, DOI: 10.1039/d0cp04352d, the author became aware of a recently-accepted study by Venezia et al, 1 which is closely related to this perspective on temperature control in DRIFT cells. Venezia et al 1 report a silicon micro-fabricated reactor cell for XAS/DRIFT studies whose dimensions, fabrication, assembly and experimental conditions are provided. Interestingly, the cell contains -perpendicular to the catalyst container -seven thermocouples by which the temperature can be monitored in the axial direction.…”