研究目的
To synthesize and characterize the A2SO4·SbF3 (A = Na+, NH4+, K+, Rb+) family of compounds, investigating the influence of cation size and coordination environment on their structural centricities and nonlinear optical properties.
研究成果
The synthesis of A2SO4·SbF3 compounds demonstrates that cation size and coordination environment significantly influence structural centricity, with K+ and Rb+ compounds being noncentrosymmetric and phase-matchable for SHG. This approach aids in designing new NLO materials.
研究不足
The study is limited to specific cations (Na+, NH4+, K+, Rb+) and may not generalize to other cations. Hydrothermal synthesis conditions might not be optimized for higher yields or purity. Theoretical calculations use GGA, which can underestimate band gaps.
1：Experimental Design and Method Selection:
Hydrothermal synthesis method was used to synthesize single crystals of A2SO4·SbF3 compounds by reacting A2SO4 and SbF3 in deionized water at 220 °C for 4 days, followed by slow cooling. Theoretical calculations using DFT in CASTEP were performed for electronic structure analysis.
2：Sample Selection and Data Sources:
Analytical grade reagents including (NH4)2SO4, Na2SO4, K2SO4, Rb2SO4, and SbF3 were used without purification. Single crystals were obtained with yields of 35–45% based on Sb.
3：List of Experimental Equipment and Materials:
Teflon autoclave for hydrothermal reactions; Rigaku Oxford Diffraction Synergy-R and Bruker D8 Venture diffractometers for single-crystal X-ray diffraction; Smart lab powder X-ray diffractometer for powder XRD; Vertex 70 FT-IR spectrometer for IR spectroscopy; Discovery TGA thermal analyzer for thermogravimetric analysis; PerkinElmer Lamda-900 UV/vis/NIR spectrophotometer for UV-vis diffuse reflectance; Q-switched Nd:YAG laser for SHG measurements.
4：Experimental Procedures and Operational Workflow:
Reactants were sealed in autoclaves, heated, cooled, washed with alcohol, and dried. Crystals were characterized by XRD, IR, TGA, UV-vis, and SHG. Data collection and refinement followed standard crystallographic procedures.
5：Data Analysis Methods:
Structures were solved using SHELX-2014 and refined with Olex2. Band structures and DOS were calculated using DFT with PBE functional in CASTEP. SHG efficiencies were compared to KDP reference.
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Rigaku Oxford Diffraction Synergy-R
Synergy-R
Rigaku Oxford Diffraction
Used for single-crystal X-ray diffraction data collection to determine crystal structures.
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Bruker D8 Venture diffractometer
D8 Venture
Bruker
Used for single-crystal X-ray diffraction data collection to determine crystal structures.
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PerkinElmer Lamda-900 UV/vis/NIR spectrophotometer
Lamda-900
PerkinElmer
Used for recording UV/Vis diffuse reflectance data to determine optical band gaps.
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Teflon autoclave
23 mL
Used for hydrothermal synthesis reactions to grow single crystals under high temperature and pressure.
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Smart lab powder X-ray diffractometer
Smart lab
Used for collecting X-ray powder diffraction patterns to verify phase purity and structure.
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Vertex 70 Fourier transform infrared spectrometer
Vertex 70
Used for obtaining IR spectra to analyze chemical bonds and functional groups.
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Discovery TGA thermal analyzer
Discovery TGA
Used for thermogravimetric analysis to study thermal stability and decomposition.
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Q-switched Nd:YAG laser
Used for powder second harmonic generation measurements to assess nonlinear optical properties.
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CASTEP program
Materials Studio
Used for density functional theory calculations to analyze band structures and density of states.
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