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Instruments / Technical Area	Publication Details	Published
B18-Core EXAFS	Pt nanoparticles on beta zeolites for catalytic toluene oxidation: effect of the hydroxyl groups of beta zeolite Run Zou , Sarayute Chansai , Shaojun Xu , Bing An , Shima Zainal , Yangtao Zhou , Ruojia Xin , Pan Gao , Guangjin Hou , Carmine D’agostino , Stuart M. Holmes , Christopher Hardacre , Yilai Jiao , Xiaolei Fan Chemcatchem DOI: 10.1002/cctc.202300811 Diamond Proposal Number(s): [29271] Show Abstract ▼ Abstract: Stabilisation of metal species using hydroxyl-rich dealuminated zeolites is a promising method for catalysis. However, insights into the interactions between the hydroxyl groups in zeolite and noble metals and their effects on catalysis are not yet fully understood. Herein, comparative studies were conducted using Pt catalysts supported on hydroxyl-rich dealuminated Beta (deAl-Beta) and the pristine proton-form Beta (H-Beta) for catalytic oxidation of toluene. The findings suggest that during impregnation the Pt precursor (i.e., Pt(NH3)4(NO3)2) interacted with different sites on deAl-Beta and H-Beta, leading to the formation of supported Pt nanoparticles with different physicochemical properties. The resulting Pt/deAl-Beta exhibited improved activity and anti-coking ability than Pt/H-Beta in catalytic toluene oxidation. According to toluene-TPD, 1H NMR relaxation and in situ DRIFTS characterisation, the enhanced performance of Pt/deAl-Beta could be ascribed to (i) the active Pt-O sites stabilised by hydroxyl groups, which interact with toluene easily for conversion, and (ii) the acid-free feature of the deAl-Beta support, which avoids the formation of coke precursors (such as benzoate species) on the catalyst surface. Findings of the work can serve as the design guidelines for making effective supported metal catalysts using zeolitic carriers.	Sep 2023
I20-EDE-Energy Dispersive EXAFS (EDE)	Bimetallic aluminum- and niobium-doped MCM-41 for efficient conversion of biomass-derived 2-methyltetrahydrofuran to pentadienes Mengtian Fan , Shaojun Xu , Bing An , Alena M. Sheveleva , Alexander Betts , Joseph Hurd , Zhaodong Zhu , Meng He , Dinu Iuga , Longfei Lin , Xinchen Kang , Christopher M. A. Parlett , Floriana Tuna , Eric J. L. Mcinnes , Luke L. Keenan , Daniel Lee , Martin P. Attfield , Sihai Yang Angewandte Chemie International Edition DOI: 10.1002/anie.202212164 Diamond Proposal Number(s): [28575] Show Abstract ▼ Abstract: The production of conjugated C4-C5 dienes from biomass can enable the sustainable synthesis of many important polymers and liquid fuels. Here, we report the first example of bimetallic (Nb, Al)-atomically doped mesoporous silica, denoted as AlNb-MCM-41, which affords quantitative conversion of 2-methyltetrahydrofuran (2-MTHF) to pentadienes with a high selectivity of 91%. The incorporation of Al(III) and Nb(V) sites into the framework of AlNb-MCM-41 has effectively tuned the nature and distribution of Lewis and Brønsted acid sites within the structure. Operando X-ray absorption, diffuse reflectance infrared and solid-state NMR spectroscopy collectively reveal the molecular mechanism of the conversion of adsorbed 2-MTHF over AlNb-MCM-41. Specifically, the atomically-dispersed Nb(V) sites play an important role in binding 2-MTHF to drive the conversion. Overall, this study highlights the potential of hetero-atomic mesoporous solids for the manufacture of renewable materials.	Oct 2022
B22-Multimode InfraRed imaging And Microspectroscopy I11-High Resolution Powder Diffraction	Highly efficient proton conduction in the metal–organic framework material MFM-300(Cr)·SO4(H3O)2 Jin Chen , Qingqing Mei , Yinlin Chen , Christopher Marsh , Bing An , Xue Han , Ian P. Silverwood , Ming Li , Yongqiang Cheng , Meng He , Xi Chen , Weiyao Li , Meredydd Kippax-Jones , Danielle Crawshaw , Mark D. Frogley , Sarah J. Day , Victoria García-Sakai , Pascal Manuel , Anibal J. Ramirez-Cuesta , Sihai Yang , Martin Schroeder Journal Of The American Chemical Society DOI: 10.1021/jacs.2c04900 Diamond Proposal Number(s): [29649] Open Access Show Abstract ▼ Abstract: The development of materials showing rapid proton conduction with a low activation energy and stable performance over a wide temperature range is an important and challenging line of research. Here, we report confinement of sulfuric acid within porous MFM-300(Cr) to give MFM-300(Cr)·SO4(H3O)2, which exhibits a record-low activation energy of 0.04 eV, resulting in stable proton conductivity between 25 and 80 °C of >10–2 S cm–1. In situ synchrotron X-ray powder diffraction (SXPD), neutron powder diffraction (NPD), quasielastic neutron scattering (QENS), and molecular dynamics (MD) simulation reveal the pathways of proton transport and the molecular mechanism of proton diffusion within the pores. Confined sulfuric acid species together with adsorbed water molecules play a critical role in promoting the proton transfer through this robust network to afford a material in which proton conductivity is almost temperature-independent.	Jul 2022
B22-Multimode InfraRed imaging And Microspectroscopy	Direct photo-oxidation of methane to methanol over a mono-iron hydroxyl site Bing An , Zhe Li , Zi Wang , Xiangdi Zeng , Xue Han , Yongqiang Chen , Alena M. Sheveleva , Zhongyue Zhang , Floriana Tuna , Eric J. L. Mcinnes , Mark D. Frogley , Anibal J. Ramirez-Cuesta , Louise S. Natrajan , Cheng Wang , Wenbin Li , Sihai Yang , Martin Schroeder Nature Materials 338 DOI: 10.1038/s41563-022-01279-1 Diamond Proposal Number(s): [23782] Show Abstract ▼ Abstract: Natural gas, consisting mainly of methane (CH4), has a relatively low energy density at ambient conditions (~36 kJ l−1). Partial oxidation of CH4 to methanol (CH3OH) lifts the energy density to ~17 MJ l−1 and drives the production of numerous chemicals. In nature, this is achieved by methane monooxygenase with di-iron sites, which is extremely challenging to mimic in artificial systems due to the high dissociation energy of the C–H bond in CH4 (439 kJ mol−1) and facile over-oxidation of CH3OH to CO and CO2. Here we report the direct photo-oxidation of CH4 over mono-iron hydroxyl sites immobilized within a metal–organic framework, PMOF-RuFe(OH). Under ambient and flow conditions in the presence of H2O and O2, CH4 is converted to CH3OH with 100% selectivity and a time yield of 8.81 ± 0.34 mmol gcat−1 h−1 (versus 5.05 mmol gcat−1 h−1 for methane monooxygenase). By using operando spectroscopic and modelling techniques, we find that confined mono-iron hydroxyl sites bind CH4 by forming an [Fe–OH···CH4] intermediate, thus lowering the barrier for C–H bond activation. The confinement of mono-iron hydroxyl sites in a porous matrix demonstrates a strategy for C–H bond activation in CH4 to drive the direct photosynthesis of CH3OH.	Jun 2022

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