P. Campone et al., HYDROGEN DESORPTION FROM CRYSTALLINE QUARTZ AND SOME RELATED DIFFERENTIAL-SCANNING CALORIMETRY AND CONDUCTIVITY PHENOMENA, Solid state communications, 98(10), 1996, pp. 917-922
Temperature-programmed desorption (TPD) and differential-scanning calo
rimetry (DSC) analyses were performed on synthetic crystalline quartz,
both ''as received'' and ''hydrogen swept'', from 200 to 600 degrees
C. The TPD measurements allowed us to establish that interstitial hydr
ogen ions, present as charge compensators near trivalent aluminium ion
s substitutional for silicon, are removed from the crystal in the cons
idered temperature range, mostly in the form of H-2 molecules. In 2 th
e hydrogen-swept samples, release of small amounts of other molecular
groups, namely SiH4 and NaOH, was also observed. The DSC studies revea
led the existence of a weak exothermic peak (enthalpy change similar o
r equal to 0.90 J g(-1)) in the temperature range from 350 to 400 degr
ees C. The exothermic process, only observable in hydrogen-swept sampl
es, may tentatively be attributed to the total-energy variation involv
ed in processes leading to H-2 formation and to SiO4 tetrahedra relaxa
tion after H-2 release. The above results have been compared with the
intensity variations, following annealing treatments, of near-infrared
OH stretching vibrations and with time-transient effects observed in
ionic conductivity measurements. The analysis contributes to a deeper
understanding of the hydrogen-impurity dynamics in crystalline quartz.
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