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Method for preparing submicron polyimide self-supporting film by adopting spin-coating method

A technology of self-supporting film and polyimide, which is applied to the device for coating liquid on the surface, coating, pretreatment surface, etc., can solve the problem of low efficiency of supporting polyimide film, easy cracking of the film, warping of the film To solve the problems of bubbling experiment, simplify the bubbling test device, high yield, and easy process

Inactive Publication Date: 2012-08-08
BEIJING UNIV OF CHEM TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has deficiencies in the process of preparing large-area films. During the preparation of large-area self-supporting polyimide films, due to the rigidity of the aluminum frame, slight warping will cause the entire film to be warped, and the fragile film is very fragile. It is prone to cracking, the efficiency of preparing self-supporting polyimide films is low and the yield is also very low, and it is even more insufficient to prepare large-area submicron films

Method used

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  • Method for preparing submicron polyimide self-supporting film by adopting spin-coating method
  • Method for preparing submicron polyimide self-supporting film by adopting spin-coating method
  • Method for preparing submicron polyimide self-supporting film by adopting spin-coating method

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Experimental program
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Effect test

Embodiment 1

[0037]A: In an ice bath environment, use a magnet to provide stirring. First weigh 0.27035g of p-phenylenediamine and add it to a three-necked flask, then add 20ml of N,N-dimethylacetamide, stir until completely dissolved, then add 0.73898g of 3,3',4,4'-biphenyltetracarboxylic acid Dianhydride, continue to stir for about 6 hours to a uniform curd-like viscous substance, take it out and put it in the refrigerator for later use;

[0038] B: Dilute the polyamic acid solution in step A to 438cp with N,N-dimethylacetamide, filter it with a microporous filter, leave it for a period of time until the bubbles in the solution are completely eliminated, and then use step-by-step spinning Spin-coat polyamic acid solution on a 4-inch clean silicon wafer, the spin-coating parameter is 500rpm for 15s, and then 1500rpm for 30s, (or two other schemes: if diluted to 353cp, the spin-coating parameter is 500rpm for 15s , then 1000rpm for 30s; or if diluted to 198cp, spin coating parameters are ...

Embodiment 2

[0044] A: In an ice bath environment, use a magnet to provide stirring. First weigh 0.5006g of 4,4'-diaminodiphenyl ether into a three-necked flask, then add 20ml of N,N-dimethylacetamide, stir until completely dissolved, then add 0.54803g of pyromellitic dianhydride, continue Stir for about 6 hours to a uniform curd-like viscous substance, take it out and put it in the refrigerator for later use;

[0045] B: Dilute the polyamic acid solution in step A to 760cp, filter it with a microporous filter, leave it for a period of time until the bubbles in the solution are completely eliminated, and use the step-by-step spin coating method on a clean float with a diameter of 8cm The polyamic acid solution was spin-coated on the glass, and then the polyamic acid solution was further diluted and spin-coated to prepare polyamic acid films under three different conditions: ①760cp, 2500rpm②288cp, 1000rpm③288cp, 1500rpm;

[0046] C: Pre-baking the polyamic acid gel film prepared by the spi...

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Abstract

A method for preparing a submicron polyimide self-supporting film by adopting a spin-coating method belongs to the technical field of polyimide self-supporting films. The method comprises the following steps: firstly, preparing a polyamic acid solution, diluting and filtering; preparing a submicron polyamide acid film by adopting the spin-coating method and preliminary drying; secondly, coating the polyamic acid solution with the high solid content on the edge of the submicron polyamide acid film and homogenizing; carrying out thermal treatment and finishing an imidization process; placing a polyimide film with a substrate in a hot mixed solution of deionized water and alcohol; after a period of time, slightly tilting an edge thick film area by using a surgical knife along the edge of the substrate; clamping the thick film area by using tweezers and gradually removing the film from the substrate from the outside to the inside; and drying in air to obtain the polyimide self-supporting film. The film prepared by the method disclosed by the invention has the characteristics of uniformity in thickness distribution, large area, low surface roughness and the like. The method is simple in preparation process and is high in finished product rate.

Description

technical field [0001] The invention relates to a preparation method of a submicron self-supporting polyimide film applied to aspects such as short-wavelength optics and laser inertial confinement fusion (ICF), and belongs to the technical field of polyimide self-supporting films. Background technique [0002] Submicron self-supporting polymer films are widely used in extreme ultraviolet and X-ray optics. Due to its excellent mechanical properties, good temperature adaptability and blocking effect on extreme ultraviolet radiation, polyimide gradually replaced the previous polypropylene, parylene, polycarbonate, etc. in the late 1990s. material, becoming the first choice for the preparation of metal membrane support materials. The superior performance of polyimide is manifested in: a. The thermal decomposition temperature of polyimide can be as high as 600°C, and it is still not brittle in liquid helium with a thermodynamic temperature of 4K. It is the best thermal stability...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J5/18C08J7/02C08L79/08B05C11/08B05D3/02
Inventor 武德珍孙庆荣陈田祥胡渭陈勇
Owner BEIJING UNIV OF CHEM TECH
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