The fictive temperature of vitreous silica containing approximately 900wtppm of hydroxyl groups was monitored with small angle x-ray scattering. The measurements were carried out during annealing and while scanning the temperature, with annealing temperatures ranging between 930 and 1330K. Fitting the data to the Adam-Gibbs-Fulcher equation by using the Tool-Narayanaswamy method yields a particularly simple thermorheological behavior for type-III vitreous silica. Unlike the general case for glass kinetics, including vitreous silica with low hydroxyl content, the relaxation time constant is nearly decoupled from the fictive temperature. This high degree of decoupling of the state of the glass and the relaxation rate agrees with the results of viscosity measurements. By improving the data analysis procedure, we have significantly increased the precision of the results, and it was possible to resolve changes of the activation energy of the relaxation processes to within 0.5%. This has made sample aging effects that had previously been undetectable visible.
Amorphous indium oxide (In2O3) and 10-wt% SnO2 doped In2O3 (ITO) thin films were prepared by pulsed-laser deposition. These films were crystallized upon heating in vacuum at an effective heating rate of 0.00847 °C/s, while the evolution of the structure was observed by in situ X-ray diffraction measurements. Fast crystallization of the films is observed in the temperature ranges 165–210 °C and 185–230 °C for the In2O3 and ITO films, respectively. The crystallization kinetics is described by a reaction equation, with activation energies of 2.31 ± 0.06 eV and 2.41 eV and order of reactions of 0.75 ± 0.07 and 0.75 for the In2O3 and ITO films, respectively. The structures of the films observed here during heating are compared with those obtained upon film growth at different temperatures. The resistivity of the films depends on the evolution of the structure, the oxygen content and the activation of tin dopants in the films. A low resistivity of 5.5 × 10−4 Ω cm was obtained for the In2O3 and ITO films at room temperature, after annealing to 250 °C the resistivity of the ITO film reduces to 1.2 × 10−4 Ω cm.
The crystallization process of indium oxide thin films deposited by pulsed laser deposition was studied. X-ray diffraction was performed on amorphous films during real-time in situ annealing in vacuum at temperatures between 100 and 300 °C and a heating rate of 0.00847 °C/s. A fast crystallization was observed in the temperature range 165–210 °C. The crystallization kinetics obtained from the reaction equation shows activation energy of 2.31 eV, reaction order of 0.75 and reaction rate factor of 8.5×1022 Hz. The structures of the in situ annealed films were compared with that of the films grown at different temperatures. The resistivity of the films is related to the structure, oxygen pressure and growth temperature. A low resistivity of 3.5×10−4 Ω cm, which increased with increasing temperature and oxygen pressure, was obtained at 100 °C and 2 Pa. The increase in the resistivity was due to a depletion of oxygen vacancies. The optical refractive index of the films decreases with changes in the deposition conditions, with an average value being 2.04.