In situ investigations of bimetallic potassium erbium borohydride

Heere, M. , GharibDoust, S.H.P. , Sørby, M.H. , Frommen, C. , Jensen, T.R. , Hauback, B.C.
International journal of hydrogen energy, Vol. 42, no. 35 (31 August 2017), 22468-22474
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Research on rare earth (RE) borohydrides is increasing due to their potential as possible hydrogen storage materials and as solid-state Li-ion conductors for battery applications. In this work, we report the formation of a new bimetallic RE borohydride, KEr(BH4)4, via mechanochemical reaction between KBH4 and Er(BH4)3 in a molar ratio of 1:1. Post-annealing of the ball-milled mixture at 175 °C for 12 h under 40 bar of hydrogen resulted in an almost phase pure material. KEr(BH4)4 is isostructural to NaSc(BH4)4 with lattice parameters of a = 8.4472(8) Å, b = 12.4292(11) Å, c = 9.6252(9) Å and space group Cmcm. An amorphization of the new bimetallic phase was observed at ∼170 °C under 1 bar argon via temperature programmed photographic analysis, which is in agreement with in situ synchrotron radiation powder X-ray diffraction (SR-PXD) as well as thermogravimetric and differential scanning calorimetry (TG-DSC). The in situ SR-PXD data did not show decomposition into the starting monometallic borohydrides.
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