研究目的
To design and evaluate dual-functionalized POSS derivatives as fillers for simultaneously lowering the refractive index and improving the thermomechanical properties of PMMA.
研究成果
The dual-functionalized POSS fillers effectively lower the refractive index and enhance thermal and mechanical properties of PMMA. The methacrylate ester-tethered POSS showed the best performance, demonstrating the potential for designing multi-functional polymeric materials with improved stability.
研究不足
The study is limited to PMMA as the polymer matrix and specific POSS derivatives; miscibility issues were observed with F+C18 POSS, leading to opacity. The effects may vary with other polymers or higher filler concentrations.
1:Experimental Design and Method Selection:
The study involved designing POSS derivatives with dual functional groups (fluoroalkyl and acrylate ester) to enhance miscibility and properties in PMMA. Syntheses were based on established sol-gel methods, and characterization included NMR, MS, SEM, UV-vis, refractive index measurements, DMA, DSC, and TGA.
2:Sample Selection and Data Sources:
PMMA (Mw = 800,000) was used as the polymer matrix. POSS fillers (F+MMA, F+CP, F+C18) were synthesized and mixed with PMMA in chloroform solutions.
3:List of Experimental Equipment and Materials:
Equipment included JEOL EX-400 NMR spectrometer, Thermo Fisher Scientific EXACTIVE mass spectrometer, JEOL JSM-5600 SEM, SHIMADZU UV-3600 spectrophotometer, Abbe refractometer DR-M4, Seiko Instrument SDM5600/DMS210 DMA, SII DSC 6220, and EXSTAR TG/DTA 6220 TGA. Materials included trimethoxy(3,3,3-trifluoropropyl)silane, 3-(trichlorosilyl)propyl methacrylate, trichlorocyclopentylsilane, trichloro(octadecyl)silane, sodium hydroxide, PMMA, THF, triethylamine, and chloroform.
4:Experimental Procedures and Operational Workflow:
POSS derivatives were synthesized via hydrolysis and condensation reactions. PMMA composites were prepared by mixing POSS and PMMA in chloroform, casting into films, and drying. Measurements were performed on the films for transparency, refractive index, thermal stability, and mechanical properties.
5:Data Analysis Methods:
Refractive indices were analyzed using the Lorentz-Lorenz and Vuks equations. Thermal and mechanical data were analyzed from TGA, DSC, and DMA curves.
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NMR Spectrometer
EX-400
JEOL
Measurement of NMR spectra for structural characterization of synthesized compounds.
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Mass Spectrometer
EXACTIVE
Thermo Fisher Scientific
Obtaining mass spectra for compound identification.
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SEM
JSM-5600
JEOL
Imaging surface morphologies of hybrid films to check for phase separation.
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UV-vis-NIR Spectrophotometer
UV-3600
SHIMADZU
Recording UV-vis transmittance spectra to measure film transparency.
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Abbe Refractometer
DR-M4
ATAGO
Determining refractive indices of polymer composites.
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DMA
SDM5600/DMS210
Seiko Instrument
Performing dynamic mechanical analysis to evaluate storage moduli and mechanical properties.
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DSC
DSC 6220
Seiko Instrument
Carrying out differential scanning calorimetry to measure glass transition temperatures.
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TGA
EXSTAR TG/DTA 6220
Seiko Instrument
Performing thermogravimetric analysis to assess thermal stability and degradation temperatures.
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Solid-State Purification System
Glasscontour System
Joerg Meyer
Purification of solvents like THF and triethylamine.
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