Recent Trends in Operando and
            <i>In Situ</i>
            Characterization: Techniques for Rational Design of Catalysts

Beale, Andrew M.; Hofmann, Jan P.; Sankar, Meenakshisundaram; Lantman, Evelien M. Schrojenstein; Weckhuysen, Bert M.

doi:10.1002/9783527658985.ch12

Cited by 5 publications

(2 citation statements)

References 155 publications

(213 reference statements)

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“…Instead, a more accurate interpretation of the action painting of a semiconductor can be established using in situ techniques with in-depth material characterization during irradiation, i.e., while the photocatalyst is in an excited state, and ideally under reaction ( in operando ) conditions. This approach is widely established in thermal catalysis (Newton and van Beek, 2010 ; O'Brien et al, 2011 ; Beale et al, 2013 , 2014 ; Liu et al, 2015 ) and is rapidly emerging in photocatalysis (Bora et al, 2013 , 2014 ; Dong and Vayssieres, 2018 ; Tan et al, 2019 ). A review on dedicated synchrotron X-ray microprobes and nanoprobes for in situ / operando material characterization has been reported recently (Mino et al, 2018 ).…”

Section: Qualitative Approaches For the Assessment Of Photocatalytic mentioning

confidence: 99%

Qualitative Approaches Towards Useful Photocatalytic Materials

Quesada-Cabrera

Parkin

2020

Front. Chem.

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The long-standing crusade searching for efficient photocatalytic materials has resulted in a vast landscape of promising photocatalysts, as reflected by the number of reviews reported in the last decade. Virtually all of these reviews have focused on quantitative approaches aiming at developing an understanding of the underlying mechanisms behind photocatalytic behavior and the parameters that influence structure-function correlation. Less attention has been paid, however, to qualitative measures around the development and assessment of photocatalysts. These measures will contribute toward narrowing the range of potential photocatalytic materials for widespread applications. The current report provides a critical perspective over some of the main factors affecting the assessment of photocatalytic materials as a code of good practice. A case of study is also provided, where this qualitative analysis is applied to one of the most prolific materials of the last-decade, disorder-engineered, black titanium dioxide (TiO 2).

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Section: Qualitative Approaches For the Assessment Of Photocatalytic mentioning

confidence: 99%

Qualitative Approaches Towards Useful Photocatalytic Materials

Quesada-Cabrera

Parkin

2020

Front. Chem.

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“…For these reasons, coupling of complementary operando spectroscopic techniques in the same experiment proved to be very helpful for deriving reliable reaction mechanisms in catalysis . This has been illustrated by impressive examples from both homogeneous and heterogeneous catalysis . The main advantage of using such techniques in a coupled setup is to get rid of such deviations, allowing results to be obtained under exactly the same conditions …”

Section: Introductionmentioning

confidence: 99%

Multivariate Analysis of Coupled Operando EPR/XANES/EXAFS/UV–Vis/ATR‐IR Spectroscopy: A New Dimension for Mechanistic Studies of Catalytic Gas‐Liquid Phase Reactions

Rabeah

Briois

Adomeit

et al. 2020

Chemistry A European J

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Operando EPR, XANES/EXAFS, UV‐Vis and ATR‐IR spectroscopic methods have been coupled for the first time in the same experimental setup for investigation of unclear mechanistic aspects of selective aerobic oxidation of benzyl alcohol by a Cu/TEMPO catalytic system (TEMPO=2,2,6,6‐tetramethylpiperidinyloxyl). By multivariate curve resolution with alternating least‐squares fitting (MCR‐ALS) of simultaneously recorded XAS and UV‐Vis data sets, it was found that an initially formed (bpy)(NMI)CuI‐ complex (bpy=2,2′‐bipyridine, NMI=N‐methylimidazole ) is converted to two different CuII species, a mononuclear (bpy)(NMI)(CH3CN)CuII‐OOH species detectable by EPR and ESI‐MS, and an EPR‐silent dinuclear (CH3CN)(bpy)(NMI)CuII(μ‐OH)2⋅CuII (bpy)(NMI) complex. The latter is cleaved in the further course of reaction into (bpy)(NMI)(HOO)CuII‐TEMPO monomers that are also EPR‐silent due to dipolar interaction with bound TEMPO. Both Cu monomers and the Cu dimer are catalytically active in the initial phase of the reaction, yet the dimer is definitely not a major active species nor a resting state since it is irreversibly cleaved in the course of the reaction while catalytic activity is maintained. Gradual formation of non‐reducible CuII leads to slight deactivation at extended reaction times.

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In Situ Spectroscopy for Mechanistic Studies in Semiconductor Photocatalysis

Hofmann

2021

Heterogeneous Photocatalysis

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Recent Trends in Operando and In Situ Characterization: Techniques for Rational Design of Catalysts

Cited by 5 publications

References 155 publications

Qualitative Approaches Towards Useful Photocatalytic Materials

Qualitative Approaches Towards Useful Photocatalytic Materials

Multivariate Analysis of Coupled Operando EPR/XANES/EXAFS/UV–Vis/ATR‐IR Spectroscopy: A New Dimension for Mechanistic Studies of Catalytic Gas‐Liquid Phase Reactions

In Situ Spectroscopy for Mechanistic Studies in Semiconductor Photocatalysis

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