研究目的
Establishing the role of polysiloxane precursors in the synthesis of aligned porous polymer derived silicon oxycarbide ceramics and understanding the evolution of pore structure during crosslinking and pyrolysis.
研究成果
Aligned macroporous Si-O-C ceramics with bimodal porosity were successfully synthesized. The pore structure evolution is influenced by precursor composition, with TMTVS playing a key role in porosity formation. Samples exhibited specific surface areas of 77-160 m2/g and pore volumes of 0.18-0.29 cm3/g, suitable for applications like filtering, gas adsorption, and electrochemical storage. Future work could focus on optimizing precursor ratios and scaling up the synthesis process.
研究不足
The study is limited to specific polysiloxane precursors and compositions; variations in precursors or processing parameters may affect results. The use of LDH for alignment and the pyrolysis conditions may not be optimized for all applications. The yield and porosity characteristics are dependent on precursor ratios, which could be further optimized.
1:Experimental Design and Method Selection:
The study uses a pyrolysis route to synthesize aligned porous Si-O-C ceramics from polysiloxane precursors, with hydrotalcite (LDH) added to achieve aligned macroporosity during crosslinking. The methodology involves crosslinking of polymer mixtures followed by pyrolysis in an inert atmosphere.
2:Sample Selection and Data Sources:
Three polymeric precursor samples (R02, R10, R18) with varying weight ratios of PHMS to TMTVS (R=2, 10, 18) were synthesized. PDMS content was fixed at 75% of PHMS weight, and LDH amount equal to TMTVS weight.
3:List of Experimental Equipment and Materials:
Precursors include polymethylhydrosiloxane (PHMS), vinyl terminated polydimethylsiloxane (PDMS), cyclic tetramethyl-tetravinlycyclotetrasiloxane (TMTVS), hydrotalcite (LDH), and platinum catalyst. Equipment includes FT-IR spectrometer, TGA/DTG analyzer, tubular furnace, XRD, SEM, FE-SEM, BET analyzer, and X-ray computed tomography.
4:Experimental Procedures and Operational Workflow:
Precursors were mixed and stirred with Pt catalyst, cured at 230°C on a hot plate, and pyrolyzed in a tubular furnace at 4°C/min to 1000°C in argon atmosphere with 1h dwell time. Characterization involved FT-IR, TGA, XRD, SEM, FE-SEM, BET, BJH, and X-ray CT.
5:Data Analysis Methods:
Data were analyzed using FT-IR for chemical bonds, TGA for thermal decomposition, XRD for amorphous nature, SEM and FE-SEM for pore morphology, BET and BJH for surface area and pore size distribution, and X-ray CT for pore alignment and size.
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FT-IR Spectrometer
FT-IR 4200
JASCO
Used for Fourier transform infrared spectroscopy to check chemical compositions and analyze bonds in precursors and samples.
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TGA/DTG Analyzer
DTG-60
Shimadzu
Used for thermogravimetric analysis and differential thermal gravimetric analysis to study thermal decomposition behavior.
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XRD
Ultima IV
Rigaku
Used for powder X-ray diffraction to establish the amorphous nature of pyrolyzed ceramics.
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SEM
EVO-18
Carl Zeiss
Used for scanning electron microscopy to analyze surface pores and morphology.
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FE-SEM
ApreoS
FEI
Used for field emission scanning electron microscopy to show aligned porosity and nanopores.
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BET Analyzer
BESORP-mini II
Not specified
Used for Brunauer-Emmett-Teller analysis to determine specific surface area and pore size distribution.
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X-ray Computed Tomography
Not specified
GE
Used to find the morphology and shape of pores in pyrolyzed samples.
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Polymethylhydrosiloxane
Not specified
Sigma Aldrich
Base polymer precursor used in the synthesis of ceramics.
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Vinyl Terminated Polydimethylsiloxane
Not specified
Sigma Aldrich
Pore-forming agent in the precursor mixture.
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Cyclic Tetramethyl-tetravinlycyclotetrasiloxane
Not specified
Sigma Aldrich
Added to improve cross-linking density and structural stability.
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Hydrotalcite
Not specified
Sigma-Aldrich
Used to attain aligned macroporosity during crosslinking.
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Platinum Catalyst
Platinum (0)-1,3-divinyl-1,1,3,3-tetramethyldisiloxane complex solution in xylene
Sigma Aldrich
Catalyst for curing reactions.
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