研究目的
Investigating the effects of sintering temperature on the microstructure and luminescence properties of LuAG:Pr ceramics, using a Czochralski-grown single crystal as reference.
研究成果
Increasing sintering temperature from 1400 to 1700 °C promotes structural improvements in LuAG:Pr ceramics towards single crystal characteristics, eliminating amorphous phase which enhances RL and reduces TL. F-related defects synergize with Pr3+ transitions, detrimentally affecting 4f-5d scintillation. Future work should explore fluorescence lifetime and low-temperature TL.
研究不足
The ceramic samples were optically opaque, limiting light collection to the surface. The study did not include fluorescence lifetime decay or low-temperature TL measurements, which are suggested for future work. The presence of defects and amorphous phase may affect results, and sintering was done without aids, which could be optimized.
1:Experimental Design and Method Selection:
The study involved sintering LuAG:Pr ceramics at temperatures from 1400 to 1700 °C for 20 h in air without sintering aids, and comparing them to a Czochralski-grown single crystal. Various analytical techniques were used to characterize microstructure and luminescence.
2:Sample Selection and Data Sources:
Powders of (Lu0.99Pr0.01)3Al5O12 were synthesized via co-precipitation method, calcined at 1000 °C, pressed into pellets, and sintered. A single crystal was used as reference.
3:99Pr01)3Al5O12 were synthesized via co-precipitation method, calcined at 1000 °C, pressed into pellets, and sintered. A single crystal was used as reference. List of Experimental Equipment and Materials:
3. List of Experimental Equipment and Materials: Equipment included Rigaku Ultima IV X-ray diffractometer, Hitachi S3400 or S4800 SEM, Thermo-Scientific Nicolet 6700 FT-IR spectrometer, Freiberg Instruments Lexsyg Research spectrofluorometer with Varian Medical Systems VF-50J X-ray tube, Andor Technology Shamrock 163 spectrograph and DU920P-BU Newton CCD camera, Horiba Jobin-Yvon Fluorolog 3, and Thermo Scientific Harshaw TLD reader model 3500. Materials included Lu2O3 (99.995%, HEFA Rare Earth Canada Co.), nitric acid (Certified A.C.S., Spectrum), aluminum nitrate (98%, Alfa Aesar), praseodymium nitrate (99.9%, Acros Organics), ammonium hydroxide (Certified A.C.S Plus, Fisher Scientific), ultrapure water, and ethanol.
4:Materials included Lu2O3 (995%, HEFA Rare Earth Canada Co.), nitric acid (Certified A.C.S., Spectrum), aluminum nitrate (98%, Alfa Aesar), praseodymium nitrate (9%, Acros Organics), ammonium hydroxide (Certified A.C.S Plus, Fisher Scientific), ultrapure water, and ethanol. Experimental Procedures and Operational Workflow:
4. Experimental Procedures and Operational Workflow: Powders were co-precipitated, washed, dried, calcined, pressed into pellets, and sintered. Density was measured by Archimedes method, XRD for structural analysis, SEM for imaging and grain size determination, ATR FTIR for vibrational analysis, PL and PLE for photoluminescence, RL for radioluminescence under X-ray excitation, and TL for thermoluminescence after annealing and irradiation.
5:Data Analysis Methods:
Data analysis included calculating density relative to theoretical value, lattice parameter from XRD peaks, grain size using ASTM E 112-96, spectral fitting with Gaussian bands for RL and PL, and normalization and correction for surface area in TL measurements.
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X-ray diffractometer
Ultima IV
Rigaku
Used for X-ray diffraction measurements to analyze crystal structure and lattice parameters.
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Scanning electron microscope
S3400 or S4800
Hitachi
Used for imaging microstructure and determining grain size.
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FT-IR spectrometer
Nicolet 6700
Thermo-Scientific
Used for attenuated total reflectance Fourier transform infrared spectroscopy to analyze vibrational modes.
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Spectrograph
Shamrock 163
Andor Technology
Used to disperse light for spectral analysis in RL measurements.
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CCD camera
DU920P-BU Newton
Andor Technology
Used to detect light in RL measurements.
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Thermoluminescence dosimeter reader
3500
Thermo Scientific Harshaw
Used for thermoluminescence measurements to study electronic defects.
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Spectrofluorometer
Lexsyg Research
Freiberg Instruments
Used for radioluminescence measurements under X-ray excitation.
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Fluorolog
3
Horiba Jobin-Yvon
Used for photoluminescence emission and excitation measurements.
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Hydraulic press
Used to press powder into pellets for sintering.
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X-ray tube
VF-50J
Varian Medical Systems
Part of the spectrofluorometer for X-ray excitation in RL measurements.
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