Differential scanning calorimetry, x-ray diffraction and F19 nuclear magnetic resonance investigations of the crystallization of InF3-based glasses

Abstract

Results of differential scanning calometry ͑DSC͒, x-ray diffraction ͑XRD͒, and 19 F nuclear magnetic resonance ͑NMR͒ of InF 3 -based glasses, treated at different temperatures, ranging from glass transition temperature (T g ) to crystallization temperature (T c ), are reported. The main features of the experimental results are as follows. DSC analysis emphasizes several steps in the crystallization process. Heat treatment at temperatures above T g enhances the nucleation of the first growing phases but has little influence on the following ones. XRD results show that several crystalline phases are formed, with solid state transitions when heated above 680 K. The 19 F NMR results show that the spin-lattice relaxation, for the glass samples heat treated above 638 K, is described by two time constants. For samples treated below this temperature a single time constant T 1 was observed. Measurements of the 19 F spin-lattice relaxation time (T 1 ), as a function of temperature, made possible the identification of the mobile fluoride ions. The activation energy, for the ionic motion, in samples treated at crystallization temperature was found to be 0.18Ϯ0.01 eV.

Influence of thermal treatment on spectroscopic properties of Er3+ ions in multicomponent InF3-based glasses

“…However, it is important information from DSC and XRD measurements that crystallization proceeds in a multi-step mechanism. It is also consistent with results obtained for the quaternary InF 3 -ZnF 2 -BaF 2 -SrF 2 (IZBS) system belonging to the same family of fluoride glasses [10]. Fig.…”

Magnetic resonance study of the crystallization behavior of InF3-based glasses doped with Cu2+, Mn2+ and Gd3+

“…As an element-selective method, sensitive to local interactions, as homo-and hetero-dipolar interactions and nuclear electric quadrupolar couplings, NMR line shapes and relaxation times studies can provide valuable information on the microscopic nature of glass materials and their crystallization phenomena [20][21][22][23][24].…”

“…In a previous paper we reported a DSC, XRD and 19 F nuclear magnetic resonance (NMR) investigation of the crystallization and nucleation processes occurring in the fluoroindate glass 40InF 3 -20ZnF 2 -20SrF 2 -20BaF 2 . Samples were treated at different temperatures, ranging from glass transition temperature (T g ) to crystallization temperature (T c ), and several crystalline phases were identified in the annealed samples [23]. In this work, glass samples doped with very small concentration (%100 ppm) of paramagnetic ions, such as Cu 2+ , Mn 2+ and Gd 3+ were studied by EPR and 19 F NMR relaxation.…”

IR transmission and emission spectra of erbium ions in fluoroindate glass

“…Thus, several different crystallization steps may occur. The XRD and DSC analysis of fluoroindate glass after heat treatment suggest a more complex crystal growth mechanism, with forming of several crystalline phases and solid-state transitions [17]. Additionally, the crystallization mechanism may be different when temperature of heating is changed or when several mechanisms occur simultaneously [18].…”