研究目的
Synthesis of new hybrid materials by solution and melt techniques using PbF2-containing matrices, analysis of their properties and establishing of mechanisms of luminescent centers formation.
研究成果
Hybrid materials based on metal-organic complexes and PbF2 matrices were successfully synthesized using glass-melt and co-precipitation techniques, exhibiting wide luminescence bands. The exchange reaction forming Pb-complexes occurs at room temperature during co-precipitation but is enhanced by heat treatment, allowing production under milder conditions to avoid thermal destruction and achieve higher concentrations of luminescent centers.
研究不足
The synthesis completeness varied with different phosphors; for Liq, the reaction did not go completely, and heat treatment was needed to increase HM centers. The techniques may involve thermal destruction risks in melt process, and co-precipitation might not fully form desired complexes without additional treatment.
1:Experimental Design and Method Selection:
The study involved synthesizing hybrid materials using two techniques: glass-melt technique and co-precipitation technique. The glass-melt technique involved melting pre-synthesized glasses and adding organic phosphors, while the co-precipitation technique involved mixing aqueous and organic solutions to precipitate PbF2 with organic components.
2:Sample Selection and Data Sources:
Organic phosphors and ligands were synthesized or purchased, including Liq, Gaq3, Eu(L1)3Phen, and NTA. Inorganic matrices were PbF2 powders and PbF2-based oxyfluoride glasses (M1, M2, M3 compositions).
3:List of Experimental Equipment and Materials:
Equipment included D2 Phaser diffractometer for XRD, VEGA-3 LMU SEM, Fluorolog FL3-22 spectrofluorimeter for PL measurements, and OriginPro software for data analysis. Materials included PbF2, SiO2, ZnO, B2O3, Pb(NO3)2, HF, ethanol, and various organic compounds from suppliers like Sigma-Aldrich, Merck, Aldrich, Acros Organics, and LANHIT Ltd.
4:Experimental Procedures and Operational Workflow:
For glass-melt technique, glasses were synthesized at 850-900°C, melted with phosphors at 600-800°C, and cast. For co-precipitation, solutions were mixed, precipitated with HF, washed, dried, and some samples heat-treated at 200°C.
5:Data Analysis Methods:
XRD analysis used EVA and TOPAS software, SEM images were analyzed, PL spectra and decay kinetics were measured and processed with OriginPro software using Gaussian decomposition and exponential fitting.
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