研究目的
To understand the mechanism of crystallization in Eu2O3 doped 30BaO-15TiO2-55GeO2 (BT1.67G + 0.5Eu) glass system through a comparative study of linear, nonlinear and model-free reaction kinetics, and to analyze their microstructure, thermal, optical, photoluminescent and electrical properties.
研究成果
Eu2O3 doped BT1.67G glass-ceramics were successfully synthesized with controlled crystallization. The crystallization is diffusion-controlled surface crystallization with zero and constant nucleation rates. The glass-ceramics contain Ba2TiGe2O8 nanocrystals (20-100 nm), show enhanced photoluminescence, high dielectric constant (up to 210 at 5 MHz), low loss, and exhibit hysteresis loops indicating ferroelectric domains. The study provides optimized heat-treatment conditions for transparent glass-ceramics with potential applications in optoelectronics.
研究不足
The study is limited to a specific glass composition and Eu2O3 doping level. The transparency of glass-ceramics decreases with longer heat-treatment times due to increased crystallite size and scattering. The hysteresis loop shows small polarization values, indicating challenges in achieving strong ferroelectric properties in the nanocomposite system.
1:Experimental Design and Method Selection:
The study used melt quenching technique for glass synthesis, followed by controlled crystallization through heat-treatment. Crystallization kinetics were analyzed using linear (Kissinger, Augis-Bennett, Ozawa, Matusita) and nonlinear (Avrami-Erofeev) solid state reaction models, and model-free Friedman method.
2:Sample Selection and Data Sources:
A glass with composition 30BaO-15TiO2-55GeO2 doped with
3:5 mol% Eu2O3 was prepared from high purity raw materials. Samples were heat-treated at 750°C for varying durations (3, 6, 9, 12, 15 h). List of Experimental Equipment and Materials:
Raw materials included GeO2 (Sigma-Aldrich), BaCO3 (Fluka Chemica), TiO2 (Merck India Ltd.), Eu2O3 (Sigma Aldrich). Equipment included DSC (NETZSCH STA 449 F3), dilatometer (NETZSCH DIL 402 PC), XRD (PANalytical XPERT-PRO MPD), FESEM (Carl Zeiss Gemini Suprat 35 VP), TEM (FEI TecnaiG2 30ST), FTIR spectrometer (Perkin-Elmer Frontier), UV-Vis-NIR spectrophotometer (Perkin-Elmer Lambda 950), spectrofluorometer (Photon Technology International Quanta Master), prism coupler (Metricon 2010/M), LCR meter (Hioki 3532-50 Hitester), and ceramic multilayer actuator test bench (aixCMA).
4:Experimental Procedures and Operational Workflow:
Glass was melted at 1300°C for 2 h, poured, annealed at 630°C, cut and polished. Heat-treatment was done at 750°C with heating/cooling rates of 1°C/min. Various characterizations (DSC, XRD, FESEM, TEM, FTIR, optical, dielectric, hysteresis) were performed.
5:Data Analysis Methods:
Kinetic parameters were analyzed using NetzschThermokinetics software. Crystallite size was calculated using Scherrer's formula. Optical band gap was determined using Tauc's plot. Dielectric and hysteresis properties were measured and analyzed.
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X-ray Diffractometer
XPERT-PRO MPD
PANalytical
Identification of crystal phases in powdered samples
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Field Emission Scanning Electron Microscope
Gemini Zeiss Suprat 35 VP
Carl Zeiss
Investigation of microstructure of etched glass-ceramic samples
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Transmission Electron Microscope
TecnaiG2 30ST
FEI
Obtaining TEM images of powdered glass-ceramic samples
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FTIR Spectrometer
Frontier FT-IR/FIR Spectrometer
Perkin-Elmer
Recording FTIR reflectance spectra
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UV-Vis-NIR Spectrophotometer
Lambda 950
Perkin-Elmer
Recording optical absorption and transmission spectra
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Differential Scanning Calorimetry
STA 449 F3
NETZSCH
Thermal analysis to determine glass transition, crystallization, and melting temperatures
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Dilatometer
DIL 402 PC
NETZSCH
Measurement of coefficient of thermal expansion, glass transition temperature, and softening temperature
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Spectrofluorometer
Quanta Master
Photon Technology International
Recording fluorescence emission and excitation spectra
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Prism Coupler
2010/M
Metricon
Measuring refractive index
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LCR Meter
3532-50 Hitester
Hioki
Measuring dielectric constant, loss, and dissipation factors
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Ceramic Multilayer Actuator Test Bench
aixCMA
Measuring hysteresis loops (P-E loops)
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