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Polyimide film with high orientation stability and preparation method thereof

A technology of polyimide film and high orientation, which is applied in the field of high orientation stability polyimide film and its preparation, can solve the problems of inconvenient processing, lower orientation degree, wrinkles, etc., and improve orientation stability and flexibility sexual effect

Active Publication Date: 2022-05-06
GUILIN ELECTRICAL EQUIP SCI RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The polyimide film undergoes longitudinal stretch orientation and transverse stretch orientation, and its linear expansion coefficient is very low. At this time, the orientation degree of the entire molecular chain of the polyimide film is very high, and the deorientation process is proceeding slowly at the same time. In the future, the orientation stress will disappear slowly, and the chain segments with small activation energy will slowly tend to be random, and the degree of orientation will be relatively reduced. The macroscopically shows that the coefficient of thermal expansion will increase, the surface flatness of the film will become worse, and wrinkles will appear, which will bring great harm to the subsequent processing. Inconvenient, graphitized film brings performance differences between batches

Method used

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  • Polyimide film with high orientation stability and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Example 1: Preparation of one-dimensional polyimide film with high orientation stability

[0022] 1) Mix 0.09kg of nano-calcium carbonate (with a particle size of 100nm), 0.01kg of nano-graphene (with a particle size of 80nm) and 1kg of N,N-dimethylacetamide, and shear at a speed of 1800r / min for 2h to obtain Inorganic filler dispersion, spare;

[0023] 2) According to the conventional polyamic acid synthesis method, at a temperature of 25°C, 29.86 kg of 4,4-diaminodiphenyl ether, 10.75 kg of p-phenylenediamine and 399 kg of N,N-dimethylethylene Put the amide into the reactor, then add 16.02kg of 3,3',4,4'-benzophenone tetracarboxylic dianhydride and 43.37kg of pyromellitic dianhydride in sequence, and then add the 1.1kg of inorganic filler prepared in step 1) to disperse solution, and reacted for 5 hours to obtain 500kg polyamic acid resin solution with a solid content of 20% and a viscosity of 12000mpa·s;

[0024]3) According to the conventional casting method, the ...

Embodiment 2

[0026] Embodiment 2: Preparation of one-dimensional polyimide film with high orientation stability

[0027] 1) According to the conventional in-situ polyamic acid synthesis method, at a temperature of 25°C, put 0.4kg of nano-calcium phosphate (with a particle size of 35nm) and 300kg of N-methylpyrrolidone into the reactor, mix and stir for 1 hour, and then put 37.33kg of 4,4-diaminodiphenyl ether and 13.44kg of 1,3-m-phenylenediamine were completely dissolved, and then 20.02kg of 3,3',4,4'-benzophenone tetraacid dianhydride and 54.21kg of pyromellitic dianhydride was reacted for 10 hours to obtain 500kg of polyamic acid resin solution with a solid content of 25% and a viscosity of 50000mpa s;

[0028] 2) According to the conventional casting method, the polyamic acid resin is defoamed and then enters the casting system to prepare a self-supporting film. The obtained self-supporting film is sent to an imine furnace, preheated at 190°C, and stretched transversely (horizontal dra...

Embodiment 3

[0030] Example 3: Preparation of one-dimensional polyimide film with high orientation stability

[0031] 1) Mix 0.8kg of nano-calcium oxide (with a particle size of 200nm) and 8kg of N,N-dimethylacetamide evenly, shear at 1800r / min for 2h, and disperse homogeneously for 0.5h to obtain an inorganic filler dispersion, which is set aside;

[0032] 2) According to the conventional polyamic acid synthesis method, at a temperature of 25°C, 22.71kg of 4,4-diaminodiphenyl ether, 14.98kg of 3,4-diaminodiphenyl ether and 558kg of N,N- Put dimethylacetamide into the reactor, then add 11.12kg of 3,3',4,4'-biphenyltetracarboxylic dianhydride and 32.99kg of pyromellitic dianhydride in sequence, and then add 1.1kg of the prepared dispersion , reacted for 5h to obtain 500kg polyamic acid resin; its solid content was 15%, and its viscosity was 30000mpa·s;

[0033] 3) According to the conventional casting method, the polyamic acid resin solution is defoamed and sent to the casting system to pr...

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Abstract

The invention discloses a method for preparing a polyimide film with high orientation stability, which comprises the following steps: 1) mixing two kinds of aromatic diamines, two kinds of aromatic dianhydrides and inorganic fillers or inorganic filler dispersions in an aprotic React in a polar solvent to obtain a polyamic acid resin solution; 2) Defoam the polyamic acid resin solution and then salivate into a film; 3) The self-supporting film is sent to the imine furnace after being stretched longitudinally or not, and then preheated , transverse stretching and sizing treatment to obtain one-dimensional or two-dimensional highly oriented polyimide film; 4) the gained one-dimensional or two-dimensional highly oriented polyimide film is firstly After high-temperature treatment, that is, heat treatment at 200-400°C for 4-20s, and then freezing treatment, that is, freezing at 0-10°C for 1-10s, the product is obtained. The film prepared by the method of the invention has better flexibility, and still has higher orientation stability and dimensional stability after long-term storage.

Description

technical field [0001] The invention relates to a polyimide film, in particular to a polyimide film with high orientation stability and a preparation method thereof. Background technique [0002] With the high integration and high density of electronic components, the heat on the surface increases sharply, which affects the performance stability and service life of electronic devices. There is an urgent need for the emergence of a high heat dissipation material that can export heat in time to solve the heating of electronic devices. question. Graphite material has the advantages of low coefficient of linear expansion (CTE) and high thermal conductivity, and is currently the mainstream to solve the heat dissipation problem of electronic components. Graphite film has high thermal conductivity in the sheet direction of hexagonal network structure, and can be prepared by expansion method and polymer pyrolysis method. The expansion method is to prepare graphite flakes from natu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08J5/18C08L79/08C08G73/10C08K3/04C08K3/22C08K3/26C08K3/32
CPCC08J5/18C08G73/1071C08G73/1042C08G73/1007C08J2379/08C08K2003/265C08K2201/011C08K3/042C08K2201/003C08K2003/2206C08K2003/325C08K3/32
Inventor 姬亚宁潘钦鹏青双桂唐必连
Owner GUILIN ELECTRICAL EQUIP SCI RES INST