Inorganic halides such as GaX<sub>n</sub> and TiX<sub>n</sub> are important precursors for the preparation of organometallics and inorganic coatings. Work on the synthesis of these compounds from the elements has remained relatively stagnant with the traditional “shake and bake” synthesis dominating their preparation.  While appropriate for laboratory scale experiments, even small increases in scale drastically increase the size of apparatus needed as well as the probability for catastrophic failure.  Through implementation of mechanochemical approaches these halides can be produced at scales from a few to dozens of grams in a small laboratory reactor. Syntheses can be safely implemented despite the potential for significant reaction exotherms.  Importantly control of the oxidation state is much simpler than with tradition methods with species such as Ga(I) and Ti(III) easily prepared.  Moderately malleable metals and halides with good solubilities can be simply prepared with excellent yields. Difficulties arise with highly malleable or covalently bound precursors.  Malleability can be mitigated through the addition of inorganic salts.  We have found the covalent precursors such as boron do not readily react with halides due to the strong bonding within the solid. Researchers have recently bulk quantities of a new form of boron has been prepared a new form of boron can be produced that consists of sheets of boron terminated with hydrogen.  This structural change increases the reactivity of the solid and allows rapid production of boron halides suitable for inorganic synthesis. This represents a safer and scalable approach to realizing heavy halide boron compounds.

Structure influence on the mechanochemical synthesis of inorganic halides

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