The paper of Prof. Etsuo Akiba (Principal Investigator, Hydrogen Storage Research Division, I2CNER) and Assoc. Prof. Li Hai-Wen (Hydrogen Storage Research Division, I2CNER) was published in "The Journal of Physical Chemistry C".
■ Outline
Metal dodecaborate, widely regarded as an obstacle of the rehydrogenation of high-density hydrogen storage materials metal borohydrides M(BH4)n, is generally synthesized using liquid-phase process followed by a careful dehydration process. In this study, we propose a new and facile solvent-free synthesis process of dodecaborates using B10H14 with a low melting point of 99.6 °C as a boron source. As a case study, our first challenge focused on the syntheses of anhydrous M2B12H12 (M = Li, Na, and K) by heat treatment of starting materials (a) 2MH + 1.2B10H14 or (b) 2MBH4 + B10H14 at 200–450 °C conditions, which have been proved to be successful for the first time by X-ray diffraction (XRD), Raman, and NMR analysis. Starting materials (b) 2MBH4 + B10H14 shows better reactivity than that of (a) 2MH + 1.2B10H14, which demonstrates that synthesis of anhydrous M2B12H12 by heat treatment of 2MBH4 + B10H14 is a feasible solvent-free process.
■ Paper
*Title: Facile Solvent-Free Synthesis of Anhydrous Alkali Metal Dodecaborate M2B12H12 (M = Li, Na, K)
*Authors: Liqing He, Hai-Wen Li, Son-Jong Hwang, and Etsuo Akiba
*DOI: 10.1021/jp500253k
*Publication Date (Web): February 28, 2014
