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Guide to Water Free Lithium Bis(oxalate) Borate (LiBOB)

The use of LiBOB is limited due to slight instability
issues under ambient conditions that might require extra purification steps and
might result in poorer performances in real systems. Here, we address some of
these issues and report the high purity water free LiBOB synthesized with fewer
processing steps employing lithium carbonate, oxalic acid, and boric acid as
low-cost starting materials, and via ceramic processing methods under
protective atmosphere. The physical and chemical characterizations of both
anhydrous and monohydrate phases are performed with X-ray powder diffraction
(XRPD), Fourier-transform infra-red spectroscopy (FTIR), Raman spectroscopy and
scanning electron microscopy (SEM) analyses to determine the degree of the
purity and the formation of impurities like LiBOB.H2O, HBO2 and
Li2C2O4 as a result of the aging
investigations performed. Differential thermal analysis (DTA) is applied to
determine the optimum synthesis conditions for anhydrous LiBOB and to analyze
the water loss and the decomposition of LiBOB.H2O. Aging experiments
with the water free LiBOB are carried out to evaluate the effect of humidity in
the phase changes and resulting impurities under various conditions. The
detrimental effect of even slightest humidity conditions is shown, and
protective measures during and after the synthesis of LiBOB are discussed.