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In-Situ and Real-time Monitoring of Mechanochemical Preparation of Li2 Mg(NH2 BH3 )4 and Na2 Mg(NH2 BH3 )4 and Their Thermal Dehydrogenation

Biliškov, Nikola; Borgschulte, Andreas; Užarević, Krunoslav; Halasz, Ivan; Lukin, Stipe; Milošević, Sanja; Milanović, Igor; Novaković, Jasmina Grbović (2017) In-Situ and Real-time Monitoring of Mechanochemical Preparation of Li2 Mg(NH2 BH3 )4 and Na2 Mg(NH2 BH3 )4 and Their Thermal Dehydrogenation. Chemistry - A European Journal, 23 (64). pp. 16274-16282. ISSN 0947-6539

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Abstract

For the first time, in-situ monitoring of uninterrupted mechanochemical synthesis of two bimetallic amidoboranes, M2Mg(NH2BH3)4 (M = Li, Na), by means of Raman spectroscopy has been applied. This approach allowed real-time observation of key intermediate phases and a straightforward follow-up of the reaction course. Detailed analysis of time-dependent spectra revealed a two-step mechanism through MNH2BH3.NH3BH3 adducts as key intermediate phases which further reacted with MgH2, giving M2Mg(NH2BH3)4 as final products. The intermediates partially take a competitive pathway toward the oligomeric M(BH3NH2BH2NH2BH3) phases. The crystal structure of the novel bimetallic amidoborane Li2Mg(NH2BH3)4 was solved from high-resolution powder diffraction data and showed an analogous metal coordination as in Na2Mg(NH2BH3)4, but a significantly different crystal packing. Li2Mg(NH2BH3)4 thermally dehydrogenates releasing highly pure H2 in the amount of 7 wt% and at a lower temperature then its sodium analogue making it significantly more viable for practical applications.

Item Type: Article
Uncontrolled Keywords: hydrogen storage; amidoborane; Raman spectroscopy; ammonia borane; mechanochemistry
Subjects: NATURAL SCIENCES
NATURAL SCIENCES > Chemistry
NATURAL SCIENCES > Chemistry > Inorganic Chemistry
Divisions: Division of Materials Chemistry
Projects:
Project titleProject leaderProject codeProject type
New Materials for Energy StorageIvan HalaszPKP-2016-06-4480HRZZ
Depositing User: Nikola Biliškov
Date Deposited: 19 Dec 2017 11:06
Last Modified: 20 Dec 2017 08:14
URI: http://fulir.irb.hr/id/eprint/3798
DOI: 10.1002/chem.201702665

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