Preparation method of high-temperature-resistant polyimide film with low thermal expansion coefficient
A technology of polyimide film and low thermal expansion coefficient, which is applied in the preparation and application field of polyimide, and can solve the problems of easy peeling or falling off of thin film devices, so as to improve the degree of linearization, increase the distance and increase the space The effect of steric hindrance
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[0020] A kind of preparation method of the high temperature resistant polyimide film of low coefficient of thermal expansion, comprises the following steps:
[0021] 1) Carrying out amidation reaction of diamine monomer and dianhydride monomer in an aprotonated solvent to obtain a polyamic acid solution;
[0022] Wherein, the ratio of the amount of the input substance of the diamine monomer to the dianhydride monomer is 1:0.5-1:2;
[0023] The dianhydride monomer is more than one of the following three compounds:
[0024]
[0025] The diamine monomer is more than one of the following five compounds:
[0026]
[0027] 2) after defoaming the obtained polyamic acid solution, a uniform liquid film is made by coating or casting;
[0028] 3) Gradient temperature rise to carry out thermal imidization reaction, and after film formation, the polyimide film is obtained.
[0029] Gradient heating is as follows: the liquid film is heated at a heating rate of 1-10°C / min to 60°C-40...
Embodiment 1
[0031] In a 100ml three-necked flask, add p-phenylenediamine C 6 h 8 N 2 2.1628g (0.020mol), first add 25g N,N-dimethylacetamide to dissolve the diamine, then add 4,4'-(hexafluoroisopropylene) diphthalic anhydride C 19 h 6 f 6 o 6 )8.8848g (0.020mol), then add 20.9639gN,N-dimethylacetamide C 4 h 9 NO, the reaction was stirred at room temperature for 24 h to obtain a polyamic acid (PAA) solution.
[0032] Coating the polyamic acid solution to obtain a polyamic acid film, then raising the temperature at a heating rate of 2-8°C / min, keeping it at 120-140°C for 0.5min, and then raising the temperature to 160-180°C at the same heating rate 0.5min, then raise the temperature to 250-270°C and keep it for 0.5min, then raise the temperature to 330-350°C and keep it for 0.5min. After gradient imidization, a high-temperature-resistant polyimide film with low thermal expansion coefficient is obtained. The measured CTE was 35 ppm / K.
Embodiment 2
[0034] In 100ml there-necked flask, add 2-(4-aminophenyl)-5-aminobenzimidazole (C 13 h 12 N 4 ) 4.4854g (0.020mol), first add 25g N,N-dimethylacetamide to dissolve the diamine, then add 4,4'-(hexafluoroisopropylene) diphthalic anhydride (C 19 h 6 f 6 o 6 ) 8.8848g (0.020mol), and then add 28.4808g N,N-dimethylacetamide, stir and react at room temperature for 24h to obtain a polyamic acid (PAA) solution.
[0035] Coat the polyamic acid solution to obtain a polyamic acid film, then raise the temperature at a heating rate of 2-8°C / min, keep it at 120-140°C for 0.5min, then raise the temperature to 160-180°C and keep it for 0.5min, then raise the temperature Keep the temperature at 250-270°C for 0.5min, then raise the temperature to 330-350°C and keep it for 0.5min. After gradient imidization, a high-temperature-resistant polyimide film with low thermal expansion coefficient is obtained. The measured CTE was 10 ppm / K.
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