研究目的
To evaluate which synthesis method (microwave-assisted precipitation, gel-combustion, sol–gel, and Pechini) leads to the best results in terms of composition, purity phase, and luminescence of Ca2Y7.76Ce0.12Tb0.12(SiO4)6O2 phosphors, and to understand the processes during thermal decomposition and structural changes.
研究成果
Ce3+, Tb3+-doped yttrium silicate apatite phosphors with improved photoluminescence characteristics were successfully prepared using various wet chemical methods. Gel-combustion, sol–gel, and Pechini methods produced pure hexagonal apatite, while precipitation required excess TEOS to enhance phase purity. Luminescence properties were influenced by phase composition and excitation wavelength, with potential applications in optoelectronics. Future work should explore other preparative conditions to optimize the synthesis.
研究不足
The precipitation method showed deviations in Ca2+ and Y3+ content due to differences in precipitation rates and solubility products, leading to secondary phases. The methods may require optimization for lower firing temperatures and better phase purity. The study is preliminary and focused on specific synthesis conditions; further research is needed on other parameters like pH and surfactants.
1：Experimental Design and Method Selection:
Four synthesis routes (microwave-assisted precipitation, gel-combustion, sol–gel, and Pechini) were used to prepare gel precursors for yttrium silicate apatite phosphors. The thermal decomposition was analyzed using TGA-FT-IR coupling, and various characterization techniques (SEM, XRD, FTIR, ICP-OES, luminescence spectroscopy) were employed to assess the phosphors.
2：Sample Selection and Data Sources:
Precursors were synthesized from specific chemical reagents to achieve the stoichiometric composition Ca2Y7.76Ce0.12Tb0.12(SiO4)6O2. Samples were thermally treated at 1400°C for 4 hours to form phosphor powders.
3：76Ce12Tb12(SiO4)6OSamples were thermally treated at 1400°C for 4 hours to form phosphor powders.
List of Experimental Equipment and Materials:
3. List of Experimental Equipment and Materials: Materials included nitric acid, yttrium oxide, calcium nitrate tetrahydrate, tetraethyl orthosilicate (TEOS), cerium nitrate hexahydrate, terbium nitrate pentahydrate, sodium hydroxide, citric acid, ethylene glycol, L-aspartic acid, and ethanol. Equipment included a microwave oven (MILESTONE), peristaltic pump (HEIDOLPH 5201), heating mantle, TGA/SDTA851 instrument (Mettler Toledo), FT-IR spectrometer (Thermo Scientific Nicolet 6700), X-ray diffractometer (Philips PW-1710/00), ICP-OES spectrometer (Perkin Elmer OPTIMA 2100 DV), SEM (Hitachi 8230), and spectrofluorimeter (JASCO FP-6500).
4：0).
Experimental Procedures and Operational Workflow:
4. Experimental Procedures and Operational Workflow: For each synthesis method, precursors were prepared by mixing reactants under controlled conditions (e.g., temperature, stirring), followed by drying and thermal treatment. Characterization involved thermal analysis, structural and morphological examination, chemical composition analysis, and luminescence measurements.
5：Data Analysis Methods:
Data were analyzed using techniques such as Debye-Scherrer formula for crystallite size calculation, FT-IR spectra interpretation, XRD pattern comparison with standard files, and luminescence intensity measurements.
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