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Instruments / Technical Area	Publication Details	Published
B07-C-Versatile Soft X-ray beamline: Ambient Pressure XPS and NEXAFS	Paramagnetic states in oxygen-doped boron nitride extend light harvesting and photochemistry to the deep visible region Elan D. R. Mistry , Daphné Lubert-Perquel , Irena Nevjestic , Giuseppe Mallia , Pilar Ferrer , Kanak Roy , Georg Held , Tian Tian , Nicholas M. Harrison , Sandrine Heutz , Camille Petit Chemistry Of Materials 21 DOI: 10.1021/acs.chemmater.2c01646 Diamond Proposal Number(s): [26511] Open Access Show Abstract ▼ Abstract: A family of boron nitride (BN)-based photocatalysts for solar fuel syntheses have recently emerged. Studies have shown that oxygen doping, leading to boron oxynitride (BNO), can extend light absorption to the visible range. However, the fundamental question surrounding the origin of enhanced light harvesting and the role of specific chemical states of oxygen in BNO photochemistry remains unanswered. Here, using an integrated experimental and first-principles-based computational approach, we demonstrate that paramagnetic isolated OB3 states are paramount to inducing prominent red-shifted light absorption. Conversely, we highlight the diamagnetic nature of O–B–O states, which are shown to cause undesired larger band gaps and impaired photochemistry. This study elucidates the importance of paramagnetism in BNO semiconductors and provides fundamental insight into its photophysics. The work herein paves the way for tailoring of its optoelectronic and photochemical properties for solar fuel synthesis.	Feb 2023
B18-Core EXAFS	Cu-functionalised porous boron nitride derived from a metal–organic framework Tian Tian , Jiamin Xu , Ying Xiong , Nitya Ramanan , Mary Ryan , Fang Xie , Camille Petit Journal Of Materials Chemistry A 8 DOI: 10.1039/D2TA05515E Diamond Proposal Number(s): [27440] Open Access Show Abstract ▼ Abstract: Porous boron nitride (BN) displays promising properties for interfacial and bulk processes, e.g. molecular separation and storage, or (photo)catalysis. To maximise porous BN's potential in such applications, tuning and controlling its chemical and structural features is key. Functionalisation of porous BN with metal nanoparticle represents one possible route, albeit a hardly explored one. Metal–organic frameworks (MOFs) have been widely used as precursors to synthesise metal functionalised porous carbon-based materials, yet MOF-derived metal functionalised inorganic porous materials remain unexplored. Here, we hypothesise that MOFs could also serve as a platform to produce metal-functionalised porous BN. We have used a Cu-containing MOF, i.e. Cu/ZIF-8, as a precursor and successfully obtained porous BN functionalised with Cu nanoparticles (i.e. Cu/BN). While we have shown control of the Cu content, we have not yet demonstrated it for the nanoparticle size. The functionalisation has led to improved light harvesting and enhanced electron–hole separation, which have had a direct positive impact on the CO2 photoreduction activity (production formation rate 1.5 times higher than pristine BN and 12.5 times higher than g-C3N4). In addition, we have found that the metal in the MOF precursor impacts porous BN's purity. Unlike Cu/ZIF-8, a Co-containing ZIF-8 precursor led to porous C-BN (i.e. BN with a large amount of C in the structure). Overall, given the diversity of metals in MOFs, one could envision our approach as a method to produce a library of different metal functionalised porous BN samples.	Sep 2022
B07-C-Versatile Soft X-ray beamline: Ambient Pressure XPS and NEXAFS	Formation mechanism and porosity development in porous boron nitride Anouk L'Hermitte , Daniel M. Dawson , Pilar Ferrer , Kanak Roy , Georg Held , Tian Tian , Sharon E. Ashbrook , Camille Petit The Journal Of Physical Chemistry C 24 DOI: 10.1021/acs.jpcc.1c08565 Diamond Proposal Number(s): [26588] Show Abstract ▼ Abstract: Porous boron nitride (BN) has proven promising as a novel class of inorganic materials in the field of separations and particularly adsorption. Owing to its high surface area and thermal stability, porous BN has been researched for CO2 capture and water cleaning, for instance. However, research remains at the laboratory scale due to a lack of understanding of the formation mechanism of porous BN, which is largely a “black box” and prevents scale up. Partial reaction pathways have been unveiled, but they omit critical steps in the formation, including the porosity development, which is key to adsorption. To unlock the potential of porous BN at a larger scale, we have investigated its formation from the perspective of both chemical formation and porosity development. We have characterized reaction intermediates obtained at different temperatures with a range of analytical and spectroscopic tools. Using these analyses, we propose a mechanism highlighting the key stages of BN formation, including intermediates and gaseous species formed in the process. We identified the crucial formation of nonporous carbon nitride to form porous BN with release of porogens, such as CO2. This work paves the way for the use of porous BN at an industrial level for gas and liquid separations.	Dec 2021
I11-High Resolution Powder Diffraction	Role of crystal size on swing-effect and adsorption induced structure transition of ZIF-8 Tian Tian , Michael Wharmby , José B. Parra , Conchi O. Ania , David Fairen-Jimenez Dalton Transactions 45, 6893-6900 DOI: 10.1039/C6DT00565A Diamond Proposal Number(s): [9750] Open Access Show Abstract ▼ Abstract: The flexibility and structure transition behaviour of ZIF-8 in a series of samples with different particle size has been studied using a combination of high-resolution N2 gas adsorption isotherms and, for the first time, a broad in situ PXRD and Rietveld analysis. During the stepped adsorption process, large particles showed a narrow adsorption/desorption pressure range with a shorter equilibrium time due to lower kinetic hindrance, deriving from higher amount of active sites. In situ PXRD showed that both the rotation of imidazole ring and a bend in the methyl group led to the gate opening of ZIF-8	Feb 2016

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