研究目的
Investigating the correlation between molecular structure and dielectric properties of carbonyl-containing polyimide dielectrics to develop materials with excellent thermal resistance and superior dielectric properties for high-temperature capacitor applications.
研究成果
The research successfully developed aromatic carbonyl-containing polyimides with excellent thermal resistance and dielectric properties. CPI-5, with carbonyl and sulfonyl groups, showed optimal performance, including high energy density and efficiency. The findings provide insights into molecular design for polymer dielectrics, suggesting future studies could expand on structural variations and practical applications.
研究不足
The study focuses on specific molecular structures and may not cover all possible variations; potential optimization areas include exploring a wider range of diamines or processing conditions to further enhance properties.
1:Experimental Design and Method Selection:
A series of aromatic carbonyl-containing polyimides (CPI) were synthesized via a conventional two-step thermal imidization method to study the structure-property correlation. The design rationale was to vary molecular structures (linked structures, length of repeating unit, linked positions) and analyze their effects on thermal and dielectric properties.
2:Sample Selection and Data Sources:
Five CPI samples (CPI-1 to CPI-5) were prepared using benzophenone 3,3',4,4'-tetracarboxylic dianhydride (BTDA) and different diamines (ODA, 134APB, 144APB, MDA, mDS). Selection criteria included varying polar groups and structural features to assess their impact.
3:List of Experimental Equipment and Materials:
Materials: 3,3'-Diaminodiphenyl sulfone (mDS), 4,4'-Diaminodiphenyl ether (ODA), 1,3-bis(4-aminophenoxy) benzene (134APB), 1,4-bis(4-aminophenoxy) benzene (144APB), 4,4'-diaminodiphenylmethane (MDA), benzophenone 3,3',4,4'-tetracarboxylic dianhydride (BTDA), N,N-dimethylacetamide (DMAc). Equipment: Nicolet iS50 FTIR spectrometer, TA instruments DSC Q100, TA instruments TGA Q500, Rigaku D/max-2500 X-ray diffractometer, Novocontrol broadband dielectric spectrometer (BDS), breakdown instrument (CS9920B), modified Sawyer-Tower circuit.
4:Experimental Procedures and Operational Workflow:
Synthesis involved reacting diamines and BTDA in DMAc to form polyamic acid (PAA), casting into films, and thermal imidization (baking at 100°C for 2 h, 150°C for 1 h, 200°C for 1 h, 250°C for 1 h, 350°C for 0.5 h). Characterization included FTIR, DSC, TGA, WAXRD, dielectric spectroscopy, breakdown strength measurement, and D-E loop analysis.
5:5 h). Characterization included FTIR, DSC, TGA, WAXRD, dielectric spectroscopy, breakdown strength measurement, and D-E loop analysis. Data Analysis Methods:
5. Data Analysis Methods: Dielectric properties analyzed using BDS for frequency and temperature scans; breakdown strength analyzed with Weibull statistics; energy density calculated from D-E loops; thermal properties determined from DSC and TGA curves.
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FTIR spectrometer
iS50
Nicolet
Record Fourier Transform Infrared spectra for chemical structure analysis
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DSC
Q100
TA instruments
Perform differential scanning calorimetry to determine glass transition temperatures
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TGA
Q500
TA instruments
Conduct thermogravimetric analysis to measure decomposition temperatures
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X-ray diffractometer
D/max-2500
Rigaku
Perform wide-angle X-ray diffraction measurements to study crystallinity
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Broadband dielectric spectrometer
BDS
Novocontrol
Investigate dielectric constant and loss over frequency and temperature ranges
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Breakdown instrument
CS9920B
Measure dielectric breakdown strength using electrostatic pull-down method
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Sawyer-Tower circuit
Collect high-field electric displacement-electric field (D-E) loops for dielectric analysis
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