Themed collection In situ and operando spectroscopy in catalysis

Operando XAS reveals that the copper catalysts undergo a remarkable reduction to the metallic state during CO₂RR.

A cross-disciplinary approach is employed to study working nanocomposite room temperature methanol sensors via a combination of operando and in situ spectroscopy techniques, paralleled by resistance measurements.

Two commercial Fe-zeolite catalysts used for N₂O abatement from nitric acid production plants are analysed before and after hydrothermal aging for their structure and activity towards N₂O conversion in complex feed.

In situ Mo K-edge X-ray absorption spectroscopy reveals different carburization pathways for unsupported and supported MoO₃ yielding Mo₂C and Mo₂C/SiO₂. Mo₂C/SiO₂ features higher resistance to oxidation under dry reforming of methane than Mo₂C.

Quantitative ³¹P operando FlowNMR spectroscopy allows chartering the unknown territory of catalyst speciation under process conditions.

Integrated CO₂ capture and conversion processes bring the promise of drastic abatement of CO₂ emission together with its valorisation to chemical building blocks such as CH₄ and CO.

Parahydrogen-induced polarization (PHIP) on Rh-containing silicalite-1 catalysts is studied using both liquid-state and in situ magic angle spinning NMR techniques and the catalyst structure effect is revealed.

Rh(OAc)₂/HPW/SiO₂ is an effective bifunctional catalyst for the halide-free carbonylation of methanol to methyl acetate and acetic acid.

Autonomous catalysis research requires elaborate integration of operando experiments into automated workflows. Suitable experimental data for analysis by artificial intelligence can be measured more readily according to standard operating procedures.

Iridium and rhodium complexes anchored on silica gel surface via NH₂–(CH₂)₃– and P(Ph)₂–(CH₂)₂– linker groups achieve high (∼9%) efficiency in pairwise addition of parahydrogen to unsaturated gaseous substrates in heterogeneous hydrogenation processes.

The weakened H_atop binding strength and increased H_atop coverage are universal phenomena on Pt, Ir, Rh, and Ru surfaces from acidic to alkaline media, which are important factors in the pH-dependent hydrogen reaction kinetics.

The in situ EXAFS experiments indicated that the Co–Ru moiety suppresses the formation of metallic Co under acidic conditions and dominates the catalytic activity of Ru_x@CoP electrocatalysts.

Reaction-time resolved IR spectroscopy highlights the role of CO and surface –OCH₃ in the MTO conversion catalysed by CoAPO-18 with maximised concentration of acidic sites.

Reflection absorption infrared spectroscopy (RAIRS) and first-principles density functional theory (DFT) combine to suggest a pathway for NO_x reduction on Cu{311} involving a flat-lying N₂O₂ intermediate.

Adsorbed SO₂ on Pt sites can be substituted by NO; adsorbed NO can be completely reduced to NH₄⁺ and removed in a reduction potential range.

Elucidating the role of Zn in bimetallic CuZn nanocatalysts for the electrocatalytic CO₂ reduction reaction (CO₂RR), where the greenhouse gas CO₂ is converted into valuable industrial chemicals using energy from renewable sources.

Both the structural change and mass change of adsorbates in heterogeneous surface reactions were simultaneously measured in situ using frequency-extended SERS spectroscopy.

To control diesel vehicle NO_x emissions, Cu-exchanged zeolites have been applied in the selective catalytic reduction of NO using NH₃ as reductant. In this work, the local structure of Cu²⁺ in zeolite ZSM-5 has been revealed by operando spectroscopies.

In situ synchrotron infrared microspectroscopy on single crystals of SAPO-34 reveals that a carbene insertion mechanism is responsible for the first carbon–carbon bond formation from surface methoxy groups.

The adsorption of H₂ and CO over Pt/Al₂O₃ was studied in gas and in liquid phase by FT-IR and ATR-IR spectroscopies under otherwise similar conditions. The solvent competes with hydrogen and CO for terrace and kink metal sites.

A correlation between the micro- and nano-scale coking behavior of SSZ-13 was discovered with in situ/operando spectroscopy and atom probe tomography (APT), which allows for spatial reconstruction and analysis of relations between framework elements and carbon atoms.

The hydrogenation of pyridine adsorbed on zeolite is dependent on the distance between acid and metal sites. Hydrogen species produced in the metal diffuse into pyridine and promote hydrogenation, suggesting a bifunctional mechanism is occurring.

Improving the stability of Ni-based dry reforming catalysts is a key challenge. ALD-grown Al₂O₃ overcoats deposited onto Ni/SiO₂ prevent the sintering of Ni, reduce deactivation by coke and inhibit the formation of inactive NiAl₂O₄ on time on stream.

This work reports a general and effective strategy of determining the intrinsic Stark tuning rate by removing the impact of the dynamical coupling of adsorbed CO on the Cu surface with surface enhanced infrared absorption spectroscopy (SEIRAS).

The interfacial coordination chemistry of water solvated single Cu²⁺ sites in ZSM-5 is assessed through pulsed EPR spectroscopy and selective ¹⁷O isotopic labelling.