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Instruments / Technical Area	Publication Details	Published	Actions
E02-JEM ARM 300CF	Droplet-based millifluidic synthesis of a proton-conducting sulfonate metal–organic framework Chao Sun , Matthew Barton , Christopher M. Pask , Mohamed Edokali , Lina Yang , Andrew J. Britton , Stuart Micklethwaite , Francesco Iacoviello , Ali Hassanpour , Maximilian Besenhard , Rik Drummond-Brydson , Ke-Jun Wu , Sean M. Collins Chemical Engineering Journal 707 DOI: 10.1016/j.cej.2023.145892 Diamond Proposal Number(s): [26822, 30160] Open Access Show Abstract ▼ Abstract: Metal–organic frameworks (MOFs) have emerged as promising candidate materials for proton exchange membranes (PEMs), due to the control of proton transport enabled by functional groups and the structural order within the MOFs. In this work, we report a millifluidic approach for the synthesis of a MOF incorporating both sulfonate and amine groups, termed Cu-SAT, which exhibits a high proton conductivity. The fouling-free multiphase flow reactor synthesis was operated for more than 5 h with no reduction in yield or change in the particle size distribution, demonstrating a sustained space–time yield up to 131.7 kg m−3 day−1 with consistent particle quality. Reaction yield and particle size were controllably tuned by the adjustment of reaction parameters, such as residence/reaction time, temperature, and reagent concentration. The reaction yields from the flow reactor were 10–20% higher than those of corresponding batch syntheses, indicating improved mass and heat transfer in flow. A systematic exploration of synthetic parameters using a factorial design of experiments approach revealed the key correlations between the process parameters and yields and particle size distributions. The proton conductivity of the synthesized Cu-SAT MOF was evaluated in a mixed matrix membrane model PEM with polyvinylpyrrolidone and polyvinylidene fluoride polymers, exhibiting a promising composite conductivity of 1.34 ± 0.05 mS cm−1 at 353 K and 95% relative humidity (RH).	Sep 2023
E02-JEM ARM 300CF	Mapping nanocrystalline disorder within an amorphous metal–organic framework Adam F. Sapnik , Chao Sun , Joonatan E. M. Laulainen , Duncan N. Johnstone , Rik Brydson , Timothy Johnson , Paul A. Midgley , Thomas D. Bennett , Sean M. Collins Communications Chemistry 6 DOI: 10.1038/s42004-023-00891-9 Diamond Proposal Number(s): [20198] Open Access Show Abstract ▼ Abstract: Intentionally disordered metal–organic frameworks (MOFs) display rich functional behaviour. However, the characterisation of their atomic structures remains incredibly challenging. X-ray pair distribution function techniques have been pivotal in determining their average local structure but are largely insensitive to spatial variations in the structure. Fe-BTC (BTC = 1,3,5-benzenetricarboxylate) is a nanocomposite MOF, known for its catalytic properties, comprising crystalline nanoparticles and an amorphous matrix. Here, we use scanning electron diffraction to first map the crystalline and amorphous components to evaluate domain size and then to carry out electron pair distribution function analysis to probe the spatially separated atomic structure of the amorphous matrix. Further Bragg scattering analysis reveals systematic orientational disorder within Fe-BTC’s nanocrystallites, showing over 10° of continuous lattice rotation across single particles. Finally, we identify candidate unit cells for the crystalline component. These independent structural analyses quantify disorder in Fe-BTC at the critical length scale for engineering composite MOF materials.	May 2023

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