Facile synthesis of anhydrous Li2B12H12 with high purity by solvent-free method

He, Liqing; Shao, Huaiyu; Felderhoff, Michael; Li, Hai-Wen; Li, Xiangnan; Zhu, Qing; Zhang, Dehui; Wu, Dong; Fu, Yanda; Deng, Yonghong; Lu, Zhouguang

doi:10.1016/j.ica.2017.05.025

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Facile synthesis of anhydrous Li₂B₁₂H₁₂ with high purity by solvent-free method

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Felderhoff, Michael
Research Department Schüth, Max-Planck-Institut für Kohlenforschung, Max Planck Society;

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Citation

He, L., Shao, H., Felderhoff, M., Li, H.-W., Li, X., Zhu, Q., et al. (2017). Facile synthesis of anhydrous Li₂B₁₂H₁₂ with high purity by solvent-free method. Inorganica Chimica Acta, 464, 147-151. doi:10.1016/j.ica.2017.05.025.

Cite as: https://hdl.handle.net/21.11116/0000-0000-C161-8

Abstract

This work is aimed to synthesize anhydrous Li₂B₁₂H₁₂ with high purity via solvent-free reaction between solid state reagents LiBH₄ and B₁₀H₁₄. The reaction is conducted respectively in open system and sealed system for comparison. It is observed to experience three thermodynamic steps: (1) melting of B₁₀H₁₄ at 103°C, (2) phase transition of LiBH₄ at 118°C and (3) Li₂B₁₂H₁₂ formation at 135°C. With appropriate heat treatment at 180°C for 2h, Li₂B₁₂H₁₂ with purity high as 93% is obtained in open system of 2 LiBH₄ +1.4 B₁₀H₁₄ with excess B₁₀H₁₄. Sealed system reacting at approximate even optimized conditions is unavailable to produce such high purity of Li₂B₁₂H₁₂. Chemical equilibrium confines the sufficient interaction between LiBH₄ and B₁₀H₁₄ in sealed system but it does not do in open system.