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Facile Solvent-Free Synthesis of Anhydrous Alkali Metal Dodecaborate M_2B_(12)H_(12) (M = Li, Na, K)

He, Liqing and Li, Hai-Wen and Hwang, Son-Jong and Akiba, Etsuo (2014) Facile Solvent-Free Synthesis of Anhydrous Alkali Metal Dodecaborate M_2B_(12)H_(12) (M = Li, Na, K). Journal of Physical Chemistry C, 118 (12). pp. 6084-6089. ISSN 1932-7447. doi:10.1021/jp500253k.

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Metal dodecaborate, widely regarded as an obstacle of the rehydrogenation of high-density hydrogen storage materials metal borohydrides M(BH_4)_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 B_(10)H_(14) 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 M_2B_(12)H_(12) (M = Li, Na, and K) by heat treatment of starting materials (a) 2MH + 1.2B_(10)H_(14) or (b) 2MBH_4 + B_(10)H_(14) 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) 2MBH_4 + B_(10)H_(14) shows better reactivity than that of (a) 2MH + 1.2B_(10)H_(14), which demonstrates that synthesis of anhydrous M_2B_(12)H_(12) by heat treatment of 2MBH_4 + B_(10)H_(14) is a feasible solvent-free process.

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Hwang, Son-Jong0000-0002-3210-466X
Additional Information:© 2014 American Chemical Society. Publication Date (Web): February 28, 2014. Received: January 9, 2014. Revised: February 28, 2014. This study was partially supported by JSPS KAKENHI Grant Number 25709067, JSPS and CAS under the Japan - China Scientific Cooperation Program, and the International Institute for Carbon Neutral Energy Research (WPI-I2CNER), sponsored by the Japanese Ministry of Education, Culture, Sports, Science, and Technology. The NMR facility at Caltech was supported by the National Science Foundation (NSF) under Grant Number 9724240 and was partially supported by the MRSEC Program of the NSF under Award Number DMR-520565.
Funding AgencyGrant Number
Japan Society for the Promotion of Science (JSPS)25709067
Chinese Academy of SciencesUNSPECIFIED
Japan - China Scientific Cooperation ProgramUNSPECIFIED
International Institute for Carbon Neutral Energy Research (WPI-I2CNER)UNSPECIFIED
Ministry of Education, Culture, Sports, Science and Technology (MEXT)UNSPECIFIED
Issue or Number:12
Record Number:CaltechAUTHORS:20140505-094845453
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Official Citation:Facile Solvent-Free Synthesis of Anhydrous Alkali Metal Dodecaborate M2B12H12 (M = Li, Na, K) Liqing He, Hai-Wen Li, Son-Jong Hwang, and Etsuo Akiba The Journal of Physical Chemistry C 2014 118 (12), 6084-6089
Usage Policy:No commercial reproduction, distribution, display or performance rights in this work are provided.
ID Code:45489
Deposited By: Ruth Sustaita
Deposited On:05 May 2014 17:20
Last Modified:10 Nov 2021 17:04

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