Mechanochemical pretreatment of ammonia borane: A new procedure for sodium amidoborane synthesis

• DOI: 10.1016/j.ijhydene.2019.06.042
• Publication Date: 2019-07-09T12:10:15Z
• Authors: Igor Milanović; Nikola Biliškov
• Keywords: amidoboranes; XRD; Hydrides; Amidoboranes; 02 engineering and technology; Hydrogen storage; 01 natural sciences; hydrogen storage; 0104 chemical sciences; IR spectroscopy; Ammonia borane; ball milling; mechanochemistry; 0210 nano-technology; Ammonia borane ; amidoboranes ; ball milling ; mechanochemistry ; XRD ; IR spectroscopy ; Hydrides ; hydrogen storage; Mechanochemistry

The present work reports a new procedure for solid state synthesis of sodium amidoborane (NaAB) by mechanochemical (MC) reaction between as-received NaH and MC pretreated AB. Ball milling (BM) method was used for this purpose. Firstly, pretreated AB was obtained by BM of as-received AB for 4.5 min. Secondly, powder of pretreated AB was mixed with as-received NaH and conducted to BM. Milling times were from 0 to 200 min: 5, 10, 30, 50, 100 and 200 min, respectively. By fixing the parameters of the milling conditions, only the influence of milling time on NaAB formation was followed. FTIR and XRD methods are used for analysis of powders after milling. We proved, by MC modification of pure AB, that the reaction rate between AB and NaH could be restricted to the interface between newly formed larger AB and small NaH particles. On such a way we obtained much better control of the reaction system with very accurate determination of reaction steps. Depending on the milling times, reaction process can be separated in three parts: i) 0–30 min part - reactant and product are present ; ii) 50–100 min part - formed NaAB is almost without other phases ; iii) 200 min part - NaAB is totally decomposed. By that synthesis procedure we produced, for the first time, pure NaAB almost without any impurity.