Facile Syntheses of pure Uranium(III) Halides: UF3, UCl3, UBr3, and UI3
Herein we describe a convenient lab scale synthesis for pure and solvent‐free binary uranium(III) halides UCl3, UBr3 and UI3. This is achieved by the reduction of the respective uranium(IV) halides with elemental silicon in borosilicate ampoules at moderate temperature. The silicon tetrahalides SiX4 formed as a side product are utilized for the removal of excess starting material via a chemical vapor transport reaction. The syntheses introduced here avoid the need for pure metallic uranium and are based on uranium(IV) halides synthesized from UO2 and the respective aluminium halides and purified by chemical vapor transport. These uranium(III) halides are obtained in single crystalline form. A similar reaction yields UF3 as a microcrystalline powder. However, no beneficial transport reaction occurs with this halide. Also, a higher temperature has to be applied and steel ampoules have to be used. The identities and purity of the products were checked by powder X‐ray diffraction as well as IR spectroscopy. The synthesis of UI3 enabled its crystal structure determination on single crystals for the first time. UI3 crystallizes in the PuBr3 structure type with space group type Cmcm and a = 4.3208(9), b = 13.923(3), c = 9.923(2) Å, V = 596.9(2) Å3, and Z = 4 at T = 100 K.
Stefan S Rudel, H. Lars Deubner, Benjamin Scheibe, Matthias Conrad, Florian Kraus
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