阅读说明：本技术 一种聚酰亚胺薄膜 (Polyimide film ) 是由 王文静 于 2019-09-03 设计创作，主要内容包括：本发明公开了一种聚酰亚胺薄膜,包括基膜,所述基膜包括四甲酸二酐、二氨基二苯醚和二甲基乙酰胺；设置于基膜表面的覆膜；所述覆膜包括有芳香二胺、联苯二酐和石墨烯,所述覆膜通过芳香二胺和联苯二酐以及石墨烯聚合而成。本申请方案中,基膜采用均聚或共聚的方法制备的聚酰亚胺薄膜,其强度、刚性和尺寸稳定性均较现有聚酰亚胺薄膜有了显著提高。利用刚性和强度强度的基膜的性能,在原有的性能再增加覆膜,覆膜也许采用均聚或共聚的方法制备的聚酰亚胺薄膜,并且再添加石墨烯,使得整体的性能有提升一个等级,由于现有市场上的聚酰亚胺薄膜。(The invention discloses a polyimide film, which comprises a base film, wherein the base film comprises tetracarboxylic dianhydride, diaminodiphenyl ether and dimethylacetamide; a film disposed on the surface of the base film; the film comprises aromatic diamine, biphenyl dianhydride and graphene, and is formed by polymerizing the aromatic diamine, the biphenyl dianhydride and the graphene. In the scheme of the application, the strength, rigidity and dimensional stability of the polyimide film prepared by adopting a homopolymerization or copolymerization method for the base film are obviously improved compared with those of the existing polyimide film. The performance of a base film with rigidity and strength is utilized, a film is additionally arranged on the original performance, the film may be a polyimide film prepared by a homopolymerization or copolymerization method, and graphene is additionally added, so that the overall performance is improved by one grade, and the polyimide film on the existing market is utilized.)

1. A polyimide film comprising a base film, characterized in that: the base film comprises tetracarboxylic dianhydride, diaminodiphenyl ether and dimethylacetamide;

a film disposed on the surface of the base film;

the film comprises aromatic diamine, biphenyl dianhydride and graphene, and is formed by polymerizing the aromatic diamine, the biphenyl dianhydride and the graphene.

The preparation method comprises the following steps:

A. the base film treatment step:

(1) raw material preparation

Grinding, crushing, screening, drying and drying tetracarboxylic dianhydride and diaminodiphenyl ether;

(2) resin synthesis

Sequentially adding the tetracarboxylic dianhydride and the diaminodiphenyl ether treated in the step (1) into a dimethylacetamide solution according to a mass ratio for dissolving and reacting to obtain a polyamic acid solution, defoaming, and performing a salivation process;

(3) steel strip slobbering

Carrying out steel belt casting on the polyamic acid resin solution obtained in the step (2) to prepare a polyamic acid solid film;

(4) imidization treatment

Firstly, gradually heating a polyamic acid solid film after casting to a volatilization temperature required by a desolventizing agent and a temperature close to that required during stretching; thereafter, the film is longitudinally stretched; finally, high-temperature treatment is carried out to convert the polyamic acid into polyimide;

(5) film formation

Performing biaxial stretching and heat treatment on the film subjected to imidization treatment in the step (4) to obtain a polyimide film finished product;

B. the film coating treatment step:

(1) raw material treatment

Grinding, crushing and drying aromatic diamine, biphenyl dianhydride and graphene;

(2) resin synthesis

Sequentially adding the aromatic diamine and the biphenyl dianhydride processed in the step (1) into a dimethylacetamide solution according to a required mass ratio for dissolving and reacting, synthesizing graphene oxide by graphene through a hummers method, preparing a dispersion liquid, preparing the solution and the dispersion liquid into a film through a spin coating method to obtain a polyamic acid solution, and performing a salivation process after defoaming;

(3) steel strip slobbering

Carrying out steel belt casting on the polyamic acid resin solution obtained in the step (2) to prepare a polyamic acid solid film;

(4) imidization treatment

Firstly, gradually heating a polyamic acid solid film after casting to a volatilization temperature required by a desolventizing agent and a temperature close to that required during stretching; thereafter, the film is longitudinally stretched; finally, high-temperature treatment is carried out to convert the polyamic acid into polyimide;

(5) film formation

Performing biaxial tension and heat treatment on the film subjected to imidization treatment in the step (4) to obtain a polyimide film finished product

Carrying out mold closing treatment on the basis of A and B;

and (3) bonding the base film and the covering film through a high-temperature resistant adhesive at high temperature.

2. The polyimide film according to claim 1, wherein: the temperature of the imidization treatment in the step (4) in the base film treatment step is 400 ℃.

3. The polyimide film according to claim 1, wherein: the temperature of the imidization treatment in the coating film treatment step (4) is 380 to 410 ℃.

Technical Field

The invention relates to the technical field of polyimide films, in particular to a polyimide film.

Background

Polyimide film (PIF) is a new type of high temperature resistant organic polymer film. It has high modulus, low shrinkage, high strength, low water absorption, hydrolysis resistance, radiation resistance, no toxicity, excellent insulating property and heat oxidation resistance. It is called "gold film" because it is one of the most expensive film materials in the world at present. It is a key insulating material for electric power and electric appliances, and also a key material for manufacturing and packaging microelectronics.

The preparation method provided by the invention has the advantages that the temperature for directly mixing the accelerant and the dehydrating agent with the polyamic acid solution is-20-0 ℃, only a small part of chemical imidization is realized, the improvement on the performance of the polyimide film is limited, and the traditional method for improving the modulus of the polyimide film is to prepare the hybrid film of the polyimide film by adding the rigid inorganic nano filler and adopting an in-situ polymerization method, so that the prepared film has poor myocardial infarction.

Disclosure of Invention

Technical problem to be solved

Aiming at the defects of the prior art, the invention provides a polyimide film, which solves the problem of polyimide films.

(II) technical scheme

In order to achieve the purpose, the invention provides the following technical scheme: a polyimide film comprising a base film, characterized in that: the base film comprises tetracarboxylic dianhydride, diaminodiphenyl ether and dimethylacetamide;

a film disposed on the surface of the base film;

the film comprises aromatic diamine, biphenyl dianhydride and graphene, and is formed by polymerizing the aromatic diamine, the biphenyl dianhydride and the graphene.

The preparation method comprises the following steps:

A. the base film treatment step:

(1) raw material preparation

Grinding, crushing, screening, drying and drying tetracarboxylic dianhydride and diaminodiphenyl ether;

(2) resin synthesis

Sequentially adding the tetracarboxylic dianhydride and the diaminodiphenyl ether treated in the step (1) into a dimethylacetamide solution according to a mass ratio for dissolving and reacting to obtain a polyamic acid solution, defoaming, and then performing a salivation process;

(3) steel strip slobbering

Carrying out steel belt casting on the polyamic acid resin solution obtained in the step (2) to prepare a polyamic acid solid film;

(4) imidization treatment

Firstly, gradually heating a polyamic acid solid film after casting to a volatilization temperature required by a desolventizing agent and a temperature close to that required during stretching; thereafter, the film is longitudinally stretched; finally, high-temperature treatment is carried out to convert the polyamic acid into polyimide;

(5) film formation

Performing biaxial tension and heat treatment on the film subjected to imidization treatment in the step (4) to obtain a polyimide film finished product;

B. the film coating treatment step:

(1) raw material treatment

Grinding, crushing and drying aromatic diamine, biphenyl dianhydride and graphene;

(2) resin synthesis

Sequentially adding the aromatic diamine and the biphenyl dianhydride processed in the step (1) into a dimethylacetamide solution according to a required mass ratio for dissolving and reacting, synthesizing graphene oxide by graphene through a hummers method, preparing a dispersion liquid, preparing the solution and the dispersion liquid into a film through a spin coating method to obtain a polyamic acid solution, and performing a hydrostomia process after defoaming;

(3) steel strip slobbering

Carrying out steel belt casting on the polyamic acid resin solution obtained in the step (2) to prepare a polyamic acid solid film;

(4) imidization treatment

Firstly, gradually heating a polyamic acid solid film after casting to a volatilization temperature required by a desolventizing agent and a temperature close to that required during stretching; thereafter, the film is longitudinally stretched; finally, high-temperature treatment is carried out to convert the polyamic acid into polyimide;

(5) film formation

Performing biaxial tension and heat treatment on the film subjected to imidization treatment in the step (4) to obtain a polyimide film finished product

Carrying out mold closing treatment on the basis of A and B;

and (3) bonding the base film and the covering film through a high-temperature resistant adhesive at high temperature.

Preferably, the temperature of the imidization treatment in the step (4) of the base film treatment is 400 ℃.

Preferably, the temperature of the imidization treatment in (4) in the coating treatment step is 380 to 410 ℃.

(III) advantageous effects

The invention provides a polyimide film. The method has the following beneficial effects:

in the scheme of the application, the strength, rigidity and dimensional stability of the polyimide film prepared by adopting a homopolymerization or copolymerization method for the base film are obviously improved compared with those of the existing polyimide film. The performance of the base film with rigidity and strength is utilized, the film is additionally coated on the original performance, the film is a polyimide film prepared by adopting a homopolymerization or copolymerization method, and graphene is additionally added, so that the overall performance is improved by one grade, and the polyimide film on the existing market is utilized.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.

The invention provides a technical scheme that: a polyimide film includes a base film including tetracarboxylic dianhydride, diaminodiphenyl ether, and dimethylacetamide;

a film disposed on the surface of the base film;

the film comprises aromatic diamine, biphenyl dianhydride and graphene, and is formed by polymerizing the aromatic diamine, the biphenyl dianhydride and the graphene.

The preparation method comprises the following steps:

A. a base film treatment step:

(1) raw material preparation

Grinding, crushing, screening, drying and drying tetracarboxylic dianhydride and diaminodiphenyl ether;

(2) resin synthesis

Sequentially adding the tetracarboxylic dianhydride and the diaminodiphenyl ether treated in the step (1) into a dimethylacetamide solution according to a mass ratio for dissolving and reacting to obtain a polyamic acid solution, defoaming, and then performing a salivation process;

(3) steel strip slobbering

Carrying out steel belt casting on the polyamic acid resin solution obtained in the step (2) to prepare a polyamic acid solid film;

(4) imidization treatment

Firstly, gradually heating a polyamic acid solid film after casting to a volatilization temperature required by a desolventizing agent and a temperature close to that required during stretching; thereafter, the film is longitudinally stretched; finally, high-temperature treatment is carried out to convert the polyamic acid into polyimide;

(5) film formation

Performing biaxial tension and heat treatment on the film subjected to imidization treatment in the step (4) to obtain a polyimide film finished product;

B. a film coating treatment step:

(1) raw material treatment

Grinding, crushing and drying aromatic diamine, biphenyl dianhydride and graphene;

(2) resin synthesis

Sequentially adding the aromatic diamine and the biphenyl dianhydride processed in the step (1) into a dimethylacetamide solution according to a required mass ratio for dissolving and reacting, synthesizing graphene oxide by graphene through a hummers method, preparing a dispersion liquid, preparing the solution and the dispersion liquid into a film through a spin coating method to obtain a polyamic acid solution, and performing a hydrostomia process after defoaming;

(3) steel strip slobbering

Carrying out steel belt casting on the polyamic acid resin solution obtained in the step (2) to prepare a polyamic acid solid film;

(4) imidization treatment

Firstly, gradually heating a polyamic acid solid film after casting to a volatilization temperature required by a desolventizing agent and a temperature close to that required during stretching; thereafter, the film is longitudinally stretched; finally, high-temperature treatment is carried out to convert the polyamic acid into polyimide;

(5) film formation

Performing biaxial tension and heat treatment on the film subjected to imidization treatment in the step (4) to obtain a polyimide film finished product

Carrying out mold closing treatment on the basis of A and B;

and (3) bonding the base film and the covering film through a high-temperature resistant adhesive at high temperature.

Specifically, the temperature of the imidization treatment in the step (4) in the base film treatment step is 400 ℃.

Specifically, the temperature of the imidization treatment in the step (4) of coating film treatment is 380 to 410 ℃.

It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.

Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.