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Instruments / Technical Area	Publication Details	Published
I19-Small Molecule Single Crystal Diffraction	Materials discovery and design limits in MDABCO perovskites Samuel D. Gale , Harry J. Lloyd , Louise Male , Mark R. Warren , Lucy K. Saunders , Paul A. Anderson , Hamish H.-M. Yeung Crystengcomm 91 DOI: 10.1039/D2CE00848C Diamond Proposal Number(s): [26118] Open Access Show Abstract ▼ Abstract: We report the structures of three new materials in the MDABCO-based perovskite family. Analysis of the Goldschmidt tolerance factor and octahedral factor enable us to propose compositional limits for pseudo-cubic perovskite phase formation and suggest directions for further materials discovery in this family of new ferroelectrics.	Aug 2022
I11-High Resolution Powder Diffraction	Synthesis and characterization of two new amide chloride compounds: Potential H2 storage materials Rosalind A. Davies , Paul A. Anderson International Journal Of Hydrogen Energy DOI: 10.1016/j.ijhydene.2014.12.044 Diamond Proposal Number(s): [3909] Open Access Show Abstract ▼ Abstract: Two new amide chloride phases, with approximate stoichiometries Li7(NH2)6Cl and Li6Mg0.5(NH2)6Cl, have been identified by powder X-ray diffraction, and their hydrogen storage properties studied. Both phases released hydrogen on reaction with LiH at a lower temperature than observed for lithium amide, and ammonia release was suppressed. The chloride ions were maintained within the structure after hydrogen desorption and rehydrogenation, raising the possibility that the materials might be cycled. The desorption properties of Li7(NH2)6Cl were found to be similar to the previously reported amide chloride Li4(NH2)3Cl but with a much reduced gravimetric penalty owing to chloride incorporation. Rehydrogenation of the imide products of reaction of both Li7(NH2)6Cl and Li6Mg0.5(NH2)6Cl with LiH occurred more readily at 90 bar and 300 °C than that of Li4(NH2)3Cl.	Jan 2015
I11-High Resolution Powder Diffraction	Enhancing ionic conductivity in lithium amide for improved energy storage materials Paul Anderson , D Hewitt , Rosalind Davies Advances In Natural Sciences: Nanoscience And Nanotechnology 6 (1) DOI: 10.1088/2043-6262/6/1/015005 Diamond Proposal Number(s): [3909] Open Access Show Abstract ▼ Abstract: Non-stoichiometry and bulk cation transport have been identified as key factors in the release and uptake of hydrogen in the Li–N–H system. Amide halide phases have been synthesized that have ionic conductivities several orders of magnitude greater than lithium amide, a faster rate of hydrogen release and elimination of the by-product, ammonia. Here we report the effect of both anion- and cation-doping on the hydrogen desorption properties of lithium amide, focusing in particular on how the presence of chloride anions and magnesium cations affects and controls the structure of the amide and imide compounds at the sub-nanometre level. Reducing the chloride content resulted in new low-chloride rhombohedral phases that contain around half of the chloride present in earlier amide chlorides, but maintained the enhancements seen in hydrogen desorption properties when compared to the halide-free system. These materials may also have potential in a range of other energy applications such as all solid state lithium ion batteries, supercapacitors, and CO2 capture and storage membranes.	Jan 2015
I11-High Resolution Powder Diffraction	Phase space investigation of the lithium amide halides Rosalind A. Davies , David R. Hewett , Emma Korkiakoski , Stephen P. Thompson , Paul A. Anderson Journal Of Alloys And Compounds DOI: 10.1016/j.jallcom.2014.12.130 Diamond Proposal Number(s): [3909] Show Abstract ▼ Abstract: An investigation has been carried out into the lower limits of halide incorporation in lithium amide (LiNH2). It was found that the lithium amide iodide Li3(NH2)2I was unable to accommodate any variation in stoichiometry. In contrast, some variation in stoichiometry was accommodated in Li7(NH2)6Br, as shown by a decrease in unit cell volume when the bromide content was reduced. The amide chloride Li4(NH2)3Cl was found to adopt either a rhombohedral or a cubic structure depending on the reaction conditions. Reduction in chloride content generally resulted in a mixture of phases, but a new rhombohedral phase with the stoichiometry Li7(NH2)6Cl was observed. In comparison to LiNH2, this new low-chloride phase exhibited similar improved hydrogen desorption properties as Li4(NH2)3Cl but with a much reduced weight penalty through addition of chloride. Attempts to dope lithium amide with fluoride ions have so far proved unsuccessful.	Dec 2014
I11-High Resolution Powder Diffraction	Chemical control of thermal expansion in cation-exchanged zeolite A Thomas Carey , Chiu C. Tang , Joe A. Hriljac , Paul A. Anderson Chemistry Of Materials 26 (4), 1561 - 1566 DOI: 10.1021/cm403312q Show Abstract ▼ Abstract: Variable-temperature powder X-ray diffraction studies have been used to monitor dramatic changes in the thermal expansion properties of zeolites with the LTA topology on changing the pore contents. Detailed structural analysis was performed on dehydrated Li-, Na-, K-, Rb-, and Cs-exchanged zeolite A and a comparison made with their purely siliceous analogue ITQ-29. Mean thermal expansion coefficients were also determined for the hydrated alkali-metal-exchanged forms. Thermal expansion behavior ranging from negative to positive was observed as different monovalent cations were included in the zeolite pores. Cation-induced strain to the zeolite framework has been shown to play a significant role in the thermal expansion mechanism of LTA-zeolites. Atomic-scale mechanisms behind the thermal expansion behavior have been deduced for ITQ-29, dehydrated Ag-A, and dehydrated Na-A systems.	Feb 2014
I11-High Resolution Powder Diffraction	The effect of extra framework species on the intrinsic negative thermal expansion property of zeolites with the LTA topology Thomas Carey , Avelino Corma , Fernando Rey , Chiu C. Tang , Joseph A. Hriljac , Paul A. Anderson Chemical Communications 48 (47), 5829-5831 DOI: 10.1039/c2cc30582h Show Abstract ▼ Abstract: X-Ray powder diffraction studies have been used to measure the thermal expansion properties of three zeolites with the LTA topology and provide details of the underlying structural changes. Siliceous ITQ-29 and dehydrated and hydrated silver zeolite A have large negative, moderate negative and positive thermal expansion coefficients, respectively.	Apr 2012

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