A kind of photosensitive polyimide composite material and preparation method thereof
A composite material and polyimide technology, applied in the field of photosensitive polyimide composite material and its preparation, can solve problems such as unfavorable use of polyimide, and achieve lower dielectric constant, i-line exposure sensitivity and resolution High, uniform and controllable thickness
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[0022] The invention provides a preparation method of a photosensitive polyimide composite material, which comprises the following steps: dissolving a diamine monomer, a functionalized graphene quantum dot and a dibasic anhydride monomer in an organic solvent successively, wherein the dibasic Anhydride monomers are added in batches; a polyamic acid solution is prepared by reacting for a preset time; then a photosensitive tertiary amine and a photoinitiator are successively mixed, and a mixed solution is obtained after stirring for a preset time; the mixed solution is spin-coated to obtain a photosensitive A polyamic acid film; a photosensitive polyimide composite material is obtained by gradient imidization within a certain temperature range; wherein, the functionalized graphene quantum dots are obtained by the citric acid pyrolysis method, and then the graphene quantum dots are prepared with diaminopyridine and The functionalized graphene quantum dots are obtained by amidation...
Embodiment 1
[0038] 1. Put 4.0g of citric acid in a 10 mL beaker and heat it in an oven at 200 °C for 30 minutes to obtain a brown solution, then dialyze the brown solution with a dialysis bag (molecular weight cut-off Da=500) for 3 days to obtain graphene quantum dots solution, and then freeze-dried for 3 days to obtain graphene quantum dot powders (GQDs);
[0039] 2. Disperse 1 g of GQDs in 100 mL of thionyl chloride and 30 mL of benzene solution, reflux at 80 °C for 12 h, wash the reflux product with tetrahydrofuran, and dry for 12 h to obtain acyl chloride GQDs powder; then 100 mg of acyl chloride GQDs Disperse the powder in tetrahydrofuran solution, add 20mg of 2,3-diaminopyridine, and react with nitrogen flow for 6 hours under stirring at room temperature, dialyze the product with a dialysis bag (molecular weight cut-off Da=500) for 3 days, and then freeze the dialysis product After drying for 3 days, aminopyridine functionalized graphene quantum dots (FGQDs-1) were obtained;
[004...
Embodiment 2
[0044] 1. Put 4.0 g of citric acid in a 10 mL beaker and heat it in an oven at 180 °C for 45 minutes to obtain a brown solution, then dialyze the brown solution with a dialysis bag (molecular weight cut-off Da=500) for 3 days to obtain graphene quantum dots solution, and then freeze-dried for 3 days to obtain graphene quantum dot powders (GQDs);
[0045] 2. Disperse 1 g of GQDs in 100 mL of thionyl chloride and 30 mL of benzene solution, reflux at 80 °C for 12 h, wash the reflux product with tetrahydrofuran, and dry for 12 h to obtain acyl chloride GQDs powder; then 100 mg of acyl chloride GQDs Disperse the powder in tetrahydrofuran solution, add 20mg of 2,6-diaminopyridine, and react with argon flow for 6 hours under stirring at room temperature, dialyze the product with a dialysis bag (molecular weight cut-off Da=500) for 3 days, and then freeze the dialysis product After drying for 3 days, aminopyridine functionalized graphene quantum dots (FGQDs-2) were obtained;
[0046]...
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