研究目的
To synthesize and characterize phosphotellurite binary glasses and glass-ceramics in the TeO2–Ba(PO3)2 system, investigating their thermal, structural, and optical properties for photonic applications.
研究成果
The study successfully synthesized stable phosphotellurite glasses and glass-ceramics in the TeO2–Ba(PO3)2 system, with samples containing 2-6 mol% Ba(PO3)2 forming transparent glass-ceramics without heat treatment. Incorporation of Ba(PO3)2 increased thermal stability, making samples suitable for optical fiber fabrication. Crystallization of α-TeO2 and γ-TeO2 phases was identified, and nonlinear optical experiments showed large effective nonlinear extinction coefficients, particularly in high-TeO2 samples. The materials are promising for photonic applications such as Raman amplifiers, nonlinear waveguides, and optical limiters.
研究不足
The strong OH absorption band in the infrared region limits transparency beyond 3 μm, which could be improved by melting in dry-atmosphere. Samples with low Ba(PO3)2 content (TBP1 and TBP2) easily crystallize and were not obtained in bulk form. Optical damage occurred at high laser intensities (>10 GW/cm2) during nonlinear measurements. The study focuses on binary systems, and further optimization for specific applications may be needed.
1:Experimental Design and Method Selection:
The study synthesized phosphotellurite binary glasses with composition (100-x)TeO2–xBa(PO3)2 (x=1-20 mol%) using the conventional melt-quenching method in covered gold crucibles under air. Properties were investigated using differential scanning calorimetry (DSC), X-ray diffraction (XRD), Raman spectroscopy, transmission electron microscopy (TEM), linear optical absorption from UV to NIR, IR transmittance, and optical limiting experiments. Rietveld analysis was used for phase crystallization investigation.
2:Sample Selection and Data Sources:
Glass samples were prepared with varying Ba(PO3)2 concentrations (1-20 mol%) using raw materials TeO2 (99.99% purity) and Ba(PO3)2 (99% purity) from Prichem Tech and Aldrich. Samples were labeled TBP1 to TBP20 based on composition.
3:99% purity) and Ba(PO3)2 (99% purity) from Prichem Tech and Aldrich. Samples were labeled TBP1 to TBP20 based on composition. List of Experimental Equipment and Materials:
3. List of Experimental Equipment and Materials: Equipment included a muffle furnace for melting, gold crucibles, stainless steel mould, translational mixer (SpeedMixer), BRUKER XRD equipment, TA Instrument Model 2910 DSC, Cary 500 Double-beam spectrophotometer, Perkin-Elmer FTIR Spectrum 2000, LabRAM HR micro Raman from Horiba Jobin Yvon, FEI Tecnai G2 F20 TEM, and a Q-switched and mode-locked Nd:YAG laser for nonlinear measurements. Materials included TeO2, Ba(PO3)2, and optical components like lenses, filters, and detectors.
4:Experimental Procedures and Operational Workflow:
Raw materials were mixed, melted at 700-850°C, cast into moulds, annealed, and slowly cooled. Characterizations involved XRD for crystallinity, DSC for thermal properties, Raman and FTIR for structural analysis, TEM for microstructure, and optical measurements for linear and nonlinear properties. Nonlinear experiments used a picosecond laser at 532 nm with controlled intensity and polarization.
5:Data Analysis Methods:
Data analysis included Rietveld refinement for XRD, deconvolution of Raman spectra, and solving the intensity propagation equation for nonlinear extinction coefficients. Statistical techniques and software tools like Crystbox for TEM indexing were employed.
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X-ray diffractometer
BRUKER
BRUKER
Used for X-ray diffraction measurements to study crystallinity and phase analysis of glass samples.
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FTIR spectrometer
Spectrum 2000
Perkin-Elmer
Used for infrared transmittance measurements.
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Transmission electron microscope
Tecnai G2 F20
FEI
Used for high-resolution TEM and SAED to investigate microstructure and crystallinity.
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Differential scanning calorimeter
Model 2910
TA Instrument
Used to determine glass transition temperature (Tg), onset of crystallization (Tx), and thermal stability parameters.
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Spectrophotometer
Cary 500
Varian
Used for UV-visible-near infrared absorption/extinction spectra measurements.
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Raman spectrometer
LabRAM HR
Horiba Jobin Yvon
Used for Raman scattering spectra to analyze structural properties.
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Laser
Nd:YAG
Used for nonlinear optical measurements and optical limiting experiments.
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Translational mixer
SpeedMixer
SpeedMixer
Used for thorough mixing of raw materials.
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Muffle furnace
Used for melting glass samples.
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Gold crucible
Used for melting glass samples to avoid corrosion.
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Stainless steel mould
Used for casting glass melts.
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Formvar coated grid
300 mesh
Formvar
Used for TEM sample preparation.
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Pulse-picker
Used to extract single pulses from the laser pulse train.
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Glan prism
Used for controlling linear polarization of the laser beam.
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λ/2 plate
Used for controlling intensity and polarization of the laser beam.
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Lens
Used for focusing the laser beam on the sample.
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Photodetector
Used for measuring transmitted and reference laser intensities.
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Digital oscilloscope
Used for recording detector outputs.
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Optical filters
Used to change the incident light intensity on samples.
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