CN112812559A - Insulating PI film and preparation method thereof - Google Patents

Insulating PI film and preparation method thereof Download PDF

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Publication number
CN112812559A
CN112812559A CN202110118506.2A CN202110118506A CN112812559A CN 112812559 A CN112812559 A CN 112812559A CN 202110118506 A CN202110118506 A CN 202110118506A CN 112812559 A CN112812559 A CN 112812559A
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film
parts
insulating
nano
boron carbide
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叶爱磊
戴玮洁
韩仲友
谈纪金
祁浩
周枫韵
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Suzhou Tailun Electronic Material Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18—Manufacture of films or sheets
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
    • C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
    • C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • C08G73/1003—Preparatory processes
    • C08G73/1007—Preparatory processes from tetracarboxylic acids or derivatives and diamines
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
    • C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
    • C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • C08G73/1067—Wholly aromatic polyimides, i.e. having both tetracarboxylic and diamino moieties aromatically bound
    • C08G73/1071—Wholly aromatic polyimides containing oxygen in the form of ether bonds in the main chain
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2379/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2361/00 - C08J2377/00
    • C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
    • C08J2379/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2425/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Derivatives of such polymers
    • C08J2425/02—Homopolymers or copolymers of hydrocarbons
    • C08J2425/04—Homopolymers or copolymers of styrene
    • C08J2425/08—Copolymers of styrene
    • C08J2425/12—Copolymers of styrene with unsaturated nitriles
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2471/00—Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
    • C08J2471/02—Polyalkylene oxides
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2227—Oxides; Hydroxides of metals of aluminium
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/34—Silicon-containing compounds
    • C08K3/36—Silica
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/38—Boron-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00—Use of ingredients characterised by shape
    • C08K7/02—Fibres or whiskers
    • C08K7/04—Fibres or whiskers inorganic
    • C08K7/14—Glass

Abstract

The invention discloses an insulating PI film which is characterized by comprising the following components in parts by weight: 30-70 parts of pyromellitic dianhydride; 20-60 parts of biphenyl tetracarboxylic dianhydride; 20-50 parts of PPD; 20-60 parts of ODA; 5-20 parts of polyalkylene glycol; 5-20 parts of a styrene-acrylonitrile copolymer; 3-10 parts of aluminum oxide; 5-15 parts of superfine glass wool; 3-15 parts of mixed nano particles; 40-90 parts of a solvent. In the invention, the polyalkylene glycol and the styrene-acrylonitrile copolymer are compounded for use, so that the insulating property and the strength of the PI film are improved; the addition of the alumina and the superfine glass wool further improves the insulating property and the heat resistance; when the nano silicon dioxide and the nano silicon nitride are compounded for use, the reduction of the insulating property can not be caused on the premise of obviously improving the high temperature resistance, the strength and the scratch resistance of the PI film, so that the comprehensive performance of the PI film can be improved.

Description

Insulating PI film and preparation method thereof
Technical Field
The invention relates to the field of PI films, in particular to an insulating PI film and a preparation method thereof.
Background
As a special engineering material, PI films (polyimide films) have been widely used in the fields of aviation, aerospace, electrical/electronic, microelectronics, nano, liquid crystal, separation films, lasers, locomotives, automobiles, precision machinery, and automatic office machines. The PI film has excellent properties, and is widely applied to more and more electronic products, and with the development of products to which the PI film is applied, higher requirements are put on the properties of the PI film, such as insulation property, heat resistance, strength and the like, for example, the PI insulating film needs to have good insulation property, heat resistance and proper strength at the same time to meet the application requirements. Therefore, how to improve the comprehensive performance of the PI film is a problem that needs to be solved urgently.
Disclosure of Invention
The technical problem to be solved by the present invention is to provide an insulating PI film and a method for manufacturing the same, aiming at the above-mentioned deficiencies in the prior art.
In order to solve the technical problems, the invention adopts the technical scheme that: an insulating PI film comprises the following components in parts by weight:
Figure BDA0002921185940000011
Figure BDA0002921185940000021
preferably, the solvent is any one or more of N, N-dimethylformamide, dimethylacetamide and triethylamine.
Preferably, the mixed nanoparticles are a mixture of nano-silica and nano-boron carbide.
Preferably, the mass ratio of the nano silicon dioxide to the nano boron carbide in the mixed nanoparticles is 2: 1.
Preferably, the particle size of the nano silicon dioxide and the particle size of the nano boron carbide are both 20-60 nm.
Preferably, the insulating PI film comprises the following components in parts by weight:
Figure BDA0002921185940000022
preferably, the insulating PI film comprises the following components in parts by weight:
Figure BDA0002921185940000023
preferably, the insulating PI film comprises the following components in parts by weight:
Figure BDA0002921185940000031
preferably, the method for preparing the insulating PI film includes the steps of:
1) mixing nano silicon dioxide and nano boron carbide and preparing a dispersion liquid;
2) adding pyromellitic dianhydride, biphenyl tetracarboxylic dianhydride, PPD, ODA, polyalkylene glycol, styrene-acrylonitrile copolymer, alumina, superfine glass wool and the dispersion liquid obtained in the step 1) into a solvent, and uniformly mixing;
3) coating the mixture obtained in the step 2) on a release layer, curing to form a semi-finished PI film, and then pressing another release layer on the surface of the semi-finished PI film to obtain the insulated PI film.
The invention has the beneficial effects that:
the insulating PI film has excellent insulating property, high temperature resistance and strength; the polyalkylene glycol and the styrene-acrylonitrile copolymer are compounded for use, so that the insulating property and the strength of the PI film are improved; the addition of the alumina and the superfine glass wool further improves the insulating property and the heat resistance; when the nano silicon dioxide and the nano silicon nitride are compounded for use, the reduction of the insulating property can not be caused on the premise of obviously improving the high temperature resistance, the strength and the scratch resistance of the PI film, so that the comprehensive performance of the PI film can be improved; the insulating PI film has excellent comprehensive performance and the preparation method is simple.
Detailed Description
The present invention is further described in detail below with reference to examples so that those skilled in the art can practice the invention with reference to the description.
It will be understood that terms such as "having," "including," and "comprising," as used herein, do not preclude the presence or addition of one or more other elements or groups thereof.
The invention provides an insulating PI film which comprises the following components in parts by weight:
Figure BDA0002921185940000041
wherein the solvent is any one or more of N, N-dimethylformamide, dimethylacetamide and triethylamine.
Wherein the mixed nano particles are a mixture of nano silicon dioxide and nano boron carbide. In a further preferred embodiment, the mass ratio of the nano-silicon dioxide to the nano-boron carbide in the mixed nanoparticles is 2: 1. The particle sizes of the nano silicon dioxide and the boron carbide are both 20-60 nm.
The nano silicon dioxide has a rigid inner core structure, and can improve the strength and the insulating property of the PI film. The introduction of the nano boron carbide can obviously improve the high temperature resistance of the PI film and further improve the strength, but the introduction of the single nano boron carbide can easily reduce the insulating property of the PI film. When the nano silicon dioxide and the nano silicon nitride are compounded for use, the reduction of the insulating property can not be caused on the premise of obviously improving the high temperature resistance, the strength and the scratch resistance of the PI film, so that the comprehensive performance of the PI film can be improved.
Pyromellitic dianhydride is used as rigid dianhydride, so that the hardness can be improved; the strength can be improved by compounding the biphenyl tetracarboxylic dianhydride and the pyromellitic dianhydride. PPD (p-phenylenediamine) is rigid diamine and can enhance rigidity, ODA (diaminodiphenyl ether) is flexible diamine and can enhance flexibility, and p-phenylenediamine and diaminodiphenyl ether are compounded for use to balance rigidity and flexibility, so that the obtained PI film has proper rigidity and flexibility.
The addition of the polyalkylene glycol can effectively improve the insulating property of the PI film, the styrene-acrylonitrile copolymer can improve the strength and the heat resistance of the PI film, the compounding of the polyalkylene glycol and the styrene-acrylonitrile copolymer can improve the comprehensive performance of the PI film,
the addition of the alumina can improve corona resistance and insulation performance, the superfine glass wool has the outstanding advantages of light weight, low heat conductivity coefficient, good thermal insulation performance, corrosion resistance and heat resistance, and the insulation performance and mechanical performance of the PI film can be further improved by compounding the superfine glass wool with the alumina.
In a preferred embodiment, the method for preparing the insulating PI film includes the steps of:
1) mixing nano silicon dioxide and nano boron carbide and preparing a dispersion liquid;
2) adding pyromellitic dianhydride, biphenyl tetracarboxylic dianhydride, PPD, ODA, polyalkylene glycol, styrene-acrylonitrile copolymer, alumina, superfine glass wool and the dispersion liquid obtained in the step 1) into a solvent, and uniformly mixing;
3) coating the mixture obtained in the step 2) on a release layer, curing to form a semi-finished PI film, and then pressing another release layer on the surface of the semi-finished PI film to obtain the insulated PI film.
Further specific examples and comparative examples are provided below to further illustrate the present invention.
The test methods used in the following examples are all conventional methods unless otherwise specified.
Example 1
An insulating PI film comprising the following components in parts by weight:
Figure BDA0002921185940000051
wherein the solvent is N, N-dimethylformamide. The mixed nano particles are a mixture of nano silicon dioxide and nano boron carbide, the mass ratio of the nano silicon dioxide to the nano boron carbide in the mixed nano particles is 2:1, and the particle sizes of the nano silicon dioxide and the nano boron carbide are both 20-60 nm.
The preparation method of the insulating PI film comprises the following steps:
1) firstly, taking N, N-dimethylformamide, mixing nano silicon dioxide and nano boron carbide in N, N-dimethylformamide and preparing into a dispersion liquid;
2) adding pyromellitic dianhydride, biphenyl tetracarboxylic dianhydride, PPD, ODA, polyalkylene glycol, styrene-acrylonitrile copolymer, alumina, superfine glass wool and the dispersion liquid obtained in the step 1) into the residual N, N-dimethylformamide, and uniformly mixing;
3) coating the mixture obtained in the step 2) on a release layer, curing at the low temperature of 100-150 ℃ for 5-15min to form a semi-finished PI film, and then laminating another release layer on the surface of the semi-finished PI film to obtain the insulating PI film.
Example 2
An insulating PI film comprises the following components in parts by weight:
Figure BDA0002921185940000061
wherein the solvent is N, N-dimethylformamide. The mixed nano particles are a mixture of nano silicon dioxide and nano boron carbide, the mass ratio of the nano silicon dioxide to the nano boron carbide in the mixed nano particles is 2:1, and the particle sizes of the nano silicon dioxide and the nano boron carbide are both 20-60 nm.
The preparation method is the same as that of example 1.
Example 3
An insulating PI film comprises the following components in parts by weight:
Figure BDA0002921185940000071
wherein the solvent is N, N-dimethylformamide. The mixed nano particles are a mixture of nano silicon dioxide and nano boron carbide, the mass ratio of the nano silicon dioxide to the nano boron carbide in the mixed nano particles is 2:1, and the particle sizes of the nano silicon dioxide and the nano boron carbide are both 20-60 nm.
The preparation method is the same as that of example 1.
Comparative example 1
The only difference from example 1 is that: the components of the composition do not include polyalkylene glycol and styrene-acrylonitrile copolymer.
Comparative example 2
The only difference from example 1 is that: the composition does not include alumina.
Comparative example 3
The only difference from example 1 is that: the composition does not include superfine glass wool.
Comparative example 4
The only difference from example 1 is that: the composition does not include mixed nanoparticles.
Comparative example 5
The only difference from example 1 is that: the mixed nanoparticles are replaced by nanosilica.
Comparative example 6
The only difference from example 1 is that: the mixed nanoparticles are replaced by nano boron carbide.
The volume resistivity, heat distortion temperature and surface hardness of the PI film samples obtained in examples 1 to 3 and comparative examples 1 to 6 were measured by the following methods:
the volume resistivity test method comprises the following steps: measured according to GB/T1410-2006;
surface hardness: measured according to GB/T6739-2006.
The results are shown in table 1 below:
Figure BDA0002921185940000081
as can be seen from the comparison results of examples 1-3 and comparative examples 1-5, the PI film obtained by the invention has excellent insulating property, high temperature resistance, high hardness and excellent scratch resistance.
From the comparison results of example 1 with comparative example 1, it can be seen that the polyalkylene glycol and styrene-acrylonitrile copolymer can improve the strength and heat resistance of the PI film;
from the comparison results of example 1 and comparative example 2, it can be seen that the addition of alumina can improve the insulating property of the PI film;
from the comparison result of the example 1 and the comparative example 3, the superfine glass wool can improve the insulating property and the heat resistance of the PI film;
from the comparison result of the embodiment 1 and the comparative example 4, the addition of the mixed nanoparticles can obviously improve the insulating property, the high temperature resistance and the surface hardness of the PI film, and further, the results of the comparative examples 5 and 6 are combined, so that the effect obtained by singly using any one of the nano silicon dioxide and the nano boron carbide is not as good as the effect obtained by compounding the nano silicon dioxide and the nano boron carbide, and the effect of compounding the nano silicon dioxide and the nano boron carbide can not cause the reduction of the insulating property on the premise of obviously improving the high temperature resistance, the strength and the scratch resistance of the PI film, which shows that the combination property of the PI film is improved by the complementation enhancement of the nano silicon dioxide and the nano.
While embodiments of the invention have been disclosed above, it is not limited to the applications listed in the description and the embodiments, which are fully applicable in all kinds of fields of application of the invention, and further modifications may readily be effected by those skilled in the art, so that the invention is not limited to the specific details without departing from the general concept defined by the claims and the scope of equivalents.

Claims (9)

1. An insulating PI film is characterized by comprising the following components in parts by weight:
Figure FDA0002921185930000011
2. the insulating PI film of claim 1 wherein the solvent is any one or more of N, N-dimethylformamide, dimethylacetamide and triethylamine.
3. The insulating PI film of claim 1, wherein the mixed nanoparticles are a mixture of nano-silica and nano-boron carbide.
4. The insulating PI film of claim 3 wherein a mass ratio of nanosilica and nano boron carbide in said mixed nanoparticles is 2: 1.
5. The insulating PI film of claim 4 wherein said nanosilica and said nanosborocarbide each have a particle size of 20-60 nm.
6. The insulating PI film of claim 5 comprising in parts by weight:
Figure FDA0002921185930000012
Figure FDA0002921185930000021
7. the insulating PI film of claim 5 comprising in parts by weight:
Figure FDA0002921185930000022
8. the insulating PI film of claim 5 comprising in parts by weight:
Figure FDA0002921185930000023
9. the insulating PI film according to any one of claims 2 to 8, wherein the preparation method comprises the steps of:
1) mixing nano silicon dioxide and nano boron carbide and preparing a dispersion liquid;
2) adding pyromellitic dianhydride, biphenyl tetracarboxylic dianhydride, PPD, ODA, polyalkylene glycol, styrene-acrylonitrile copolymer, alumina, superfine glass wool and the dispersion liquid obtained in the step 1) into a solvent, and uniformly mixing;
3) coating the mixture obtained in the step 2) on a release layer, curing to form a semi-finished PI film, and then pressing another release layer on the surface of the semi-finished PI film to obtain the insulated PI film.
CN202110118506.2A 2021-01-28 2021-01-28 Insulating PI film and preparation method thereof Pending CN112812559A (en)

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CN114369361A (en) * 2021-12-31 2022-04-19 广州惠利电子材料有限公司 Insulating PI membrane material

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114369361A (en) * 2021-12-31 2022-04-19 广州惠利电子材料有限公司 Insulating PI membrane material

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Application publication date: 20210518