研究目的
To investigate the thermal curing, pyrolysis behavior, and fluorescence properties of a novel silicon-containing hybrid polymer (DPHES) with C C and Si H linkages, and to understand its structure-property relationship for potential use as light-emitting materials with excellent thermal stability.
研究成果
DPHES exhibits excellent thermal stability and moderate fluorescence properties due to its crosslinked structure formed via cyclotrimerization, addition, and hydrosilylation reactions. It shows potential as a light-emitting material with high thermal resistance, as evidenced by TGA and fluorescence emission spectra.
研究不足
The study is limited to the specific polymer DPHES; generalizability to other silicon-containing polymers may require further investigation. Pyrolysis analysis was conducted at fixed temperatures (650°C and 750°C), which may not cover all degradation scenarios. Fluorescence properties were measured in solution and solid state, but practical applications in devices were not tested.
1：Experimental Design and Method Selection:
The study involved synthesis of DPHES, thermal curing, and characterization using various analytical techniques to understand curing mechanisms, pyrolysis behavior, and fluorescence properties.
2：Sample Selection and Data Sources:
DPHES was synthesized from reagents like n-butyllithium, diphenyldichlorosilane, etc., and crosslinked under controlled thermal conditions.
3：List of Experimental Equipment and Materials:
Instruments included DSC, FTIR spectrometer, Py-GC/MS, TGA, fluorescence spectrophotometer, GPC, NMR spectrometer. Materials included n-butyllithium, diphenyldichlorosilane, triflic acid, LiAlH4, solvents like THF and diethyl ether.
4：Experimental Procedures and Operational Workflow:
DPHES was synthesized via a multi-step reaction under nitrogen, purified, and crosslinked by heating in a vacuum oven. Characterization involved FTIR before and after curing, DSC for curing behavior, Py-GC/MS for pyrolysis products, TGA for thermal stability, and fluorescence spectroscopy for optical properties.
5：Data Analysis Methods:
Data were analyzed using instrument-specific software, with pyrolysis products identified via mass spectrometry comparison to NIST library.
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Bruker ARX-400 spectrometer
ARX-400
Bruker
Used for recording 1H and 13C-NMR spectra.
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F-7000 fluorescence spectrophotometer
F-7000
Hitachi
Used for measuring fluorescence spectra at room temperature.
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Agilent 7890A gas chromatograph
7890A
Agilent
Coupled with mass spectrometer for GC/MS analysis.
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Agilent 5975C mass spectrometer
5975C
Agilent
Used in electron impact mode for mass spectrometry.
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Nicolet 5700 spectrometer
5700
Nicolet
Used for obtaining FTIR spectra of samples.
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GPC system
Equipped with Waters 1515 Isocratic HPLC pump and Waters 2414 refractive index detector
Waters
Used for measuring molecular weight and its distribution.
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TGA/SDTA-851e thermogravimetric analyzer
SDTA-851e
Mettler Toledo
Used for thermogravimetric analysis to evaluate thermal stability.
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DSC 822e instrument
822e
Mettler Toledo
Used for differential scanning calorimetry studies.
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PY-2020iD pyrolyzer
PY-2020iD
FrontierLab
Used for pyrolysis coupled with GC/MS for analyzing pyrolysis products.
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