Paper Title:

Release of Tetrahydrofuran, Structural Phase Transitions and Dynamic Relaxation Processes in Ca (BH4)2

Periodical Solid State Phenomena (Volume 184)
Main Theme Internal Friction and Mechanical Spectroscopy
Edited by Robert Schaller and D. Mari
Pages 24-32
DOI 10.4028/www.scientific.net/SSP.184.24
Citation Annalisa Paolone et al., 2012, Solid State Phenomena, 184, 24
Online since January, 2012
Authors Annalisa Paolone, O. Palumbo, P. Rispoli, R. Cantelli, E. Rönnebro, A. Luedtke, D. Chandra
Keywords Adduct Release, Calcium Borohydride, Hydrogen Storage Materials, Relaxation Processes, Structural Phase Transitions
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Abstract

Various calcium borohydride samples were investigated by means of combined measurements of thermogravimetry and mass spectrometry, and anelastic spectroscopy. On heating, the release of 2-5% tetrahydrofuran (THF) is detected in all the samples at temperatures below ~480 K, even in those which were previously thermally treated, according to procedures known from the literature, in order to remove the solvent. Dehydrogenation takes place above 480 K. Above room temperature the temperature dependence of the Young modulus of Ca (BH4)2 clearly monitors the release of THF and two irreversible structural phase transitions: from the α to the α’ phase around 460 K and from the α’ to the β phase, nearly completely evolved around 590 K. Moreover, the coefficient of elastic energy dissipation presents two dynamic processes below room temperature; a peak around 120 K characterized by an activation energy of 0.20 eV and a pre-exponential factor typical of atom-cluster relaxations, that we attributed to the dynamics of THF molecules retained in the borohydride lattice, and a peak around 200 K, possibly due to the relaxation of H vacancies.