A kind of high temperature resistant neutron radiation resistant polyimide composite film and its preparation method
A polyimide and composite film technology, which is applied in the field of high temperature resistant functional polymer materials, can solve the problems of poor quality of boron-containing polyimide and less doping of boron elements, and achieves easy process amplification and dispersion. Good performance, improve the effect of dispersibility
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[0056] A preparation method of boron-containing polyimide, specifically comprising the following steps:
[0057] 1) Preparation of polyamic acid glue: under inert gas protection conditions, dissolve the diamine monomer in an aprotic polar organic solvent. After the diamine monomer is completely dissolved, add the metered ratio of dianhydride monomer in batches body, mechanically stirred for more than 5 hours, by adding an aprotic polar organic solvent to adjust the solid content range of polyamic acid to 6% to 15%, and the apparent viscosity of polyamic acid glue to 10000 to 15000mPa.s;
[0058] 2) Micron-scale or nano-scale boron-containing powder pretreatment: Stir and disperse the boron-containing powder in an alcohol solution (water / alcohol mass ratio is 1:9, alcohol includes ethanol, methanol, isopropanol), and the boron-containing powder The mass ratio of the powder to the aqueous ethanol solution is 1: (5-10), and a silane coupling agent containing 0.1-5 wt% of the boro...
Embodiment 1
[0064] In a 250mL three-neck bottle equipped with a mechanical stirring device, weigh 8.010g (40mmol) of 4,4'-diaminodiphenyl ether (ODA) and dissolve it in 100ml of N,N-dimethylformamide (DMF) solvent After the diamine is completely dissolved, add 11.916g (40mmol) biphenyltetracarboxylic dianhydride (BPDA) in batches. At this time, the solid content of the solution is about 15%. In the process of mechanical stirring, observe the polyamic acid (PAA) glue Viscosity changes, the phenomenon of "climbing rods" occurs when the viscosity is too high, and the measured intrinsic viscosity is 2.75dL / g. Add DMF solvent to dilute until the apparent viscosity is about 12000mPa.s.
[0065] Weigh 8.5g (30wt%) micron-sized boron carbide (B 4 C) Powder, ultrasonically dispersed in 50ml DMF solvent for 1h, then added to the above PAA glue by wet mixing, and stirred at high speed for 3h to obtain evenly dispersed B 4 C-PAA glue, the solid content of the system is about 9%. Will B 4 C-PAA gl...
Embodiment 2
[0068] On the basis of the PAA glue synthesized in Example 1, weigh 3.5g (15wt%) micron-sized boron carbide (B) coated with 2wt% KH550 4 C) Powder, ultrasonically dispersed in 50ml DMF solvent for 1h, then added to the above PAA glue by wet mixing, and stirred at high speed for 3h to obtain evenly dispersed B 4 C-PAA glue, the solid content of the system is about 9%. Will B 4 After the C-PAA glue solution was vacuum degassed for 5 hours, it was coated on a clean glass plate to form a film, and the thermal imidization process was the same as in Example 1. BPDA-ODA / B prepared by this process 4C polyimide composite film has high surface uniformity and good folding resistance. 2 The 5% thermal weight loss temperature is as high as 593°C, the tensile strength is 456MPa, and the thermal neutron permeability I / I when the thickness of the composite film is 130μm 0 0.82, neutron protection performance is poor.
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