研究目的
Investigating the effect of Y2O3 on the glass transition kinetics, crystallization kinetics, phase separation, and crystallization behavior of 60ZnO–30B2O3–10SiO2 glass.
研究成果
Addition of Y2O3 decreases glass transition activation energy and increases crystallization activation energy, improving glass structure stability. Phase separation and crystallization are retarded, with crystal growth being mainly one-dimensional. This provides insights for developing glass ceramics with controlled micro- or nano-crystals on surfaces.
研究不足
The study is limited to specific glass compositions and Y2O3 doping levels up to 6 mol%. Non-isothermal methods may have inherent approximations. The use of HF acid for etching poses safety concerns. Potential optimizations include exploring higher doping concentrations, isothermal methods for kinetics, and alternative characterization techniques.
1:Experimental Design and Method Selection:
Non-isothermal differential thermal analysis (DSC), scanning electron microscopy (SEM), and X-ray powder diffraction (XRD) were used to study glass transition and crystallization kinetics. Theoretical models such as Kissinger and Moynihan were applied for activation energy calculations.
2:Sample Selection and Data Sources:
Glass samples with compositions 60ZnO–30B2O3–10SiO2 doped with 0, 2, 4, and 6 mol% Y2O3 were prepared using analytical grade chemicals. DSC data were collected at heating rates of 5, 10, 15, and 20 K/min.
3:List of Experimental Equipment and Materials:
Equipment includes DSC (Model STA449C), XRD (Model QUEST), SEM (FEI QUANTA-400 and ZEISS Sigma 500), FTIR spectrometer (PerkinElmer), and grinding machine. Materials include ZnO, H3BO3, SiO2, Y2O3, platinum crucible, electrical resistance furnace, graphite mould, HF acid, deionized water, gold for coating, and KBr for FTIR.
4:Experimental Procedures and Operational Workflow:
Raw materials were mixed, melted at 1350–1400 °C for 2 h, poured into moulds, annealed at 550–590 °C for 1 h, and cooled. DSC measurements were performed in nitrogen atmosphere. Samples were heat-treated at 893 K and 993 K for 5 h for phase separation and crystallization studies. Surfaces were polished, etched with HF, cleaned, and coated with gold for SEM. XRD patterns were recorded from 10–80° 2θ.
5:2θ. Data Analysis Methods:
5. Data Analysis Methods: Data analyzed using Kissinger and Moynihan models for activation energies, Augis-Bennett equation for Avrami exponent, Gaussian fitting for peak separation, and Jade software for XRD analysis. Crystallinity calculated from XRD integral areas.
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Scanning Electron Microscope
FEI QUANTA-400
FEI
Observing morphology of crystallite phase precipitated in glass.
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Scanning Electron Microscope
ZEISS Sigma 500
ZEISS
Observing morphology of crystallite phase precipitated in glass.
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Differential Scanning Calorimeter
STA449C
Germany
Measuring glass transition and crystallization behavior by heating samples and recording thermal effects.
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X-ray Powder Diffractometer
QUEST
America
Identifying precipitated crystallites and their crystallinity using Cu Kα radiation.
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Fourier Transform Infrared Spectrometer
PerkinElmer
Measuring FTIR absorption spectra of glass samples using KBr disc method.
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Grinding Machine
Mechanically mixing raw materials for glass preparation.
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Electrical Resistance Furnace
Melting glass samples in platinum crucible.
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Platinum Crucible
Container for melting glass samples.
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Graphite Mould
Mould for forming molten glass.
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