CN115594846B - Polyimide film with improved adhesion and moisture permeation rate and method of preparing the same - Google Patents
Polyimide film with improved adhesion and moisture permeation rate and method of preparing the same Download PDFInfo
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- CN115594846B CN115594846B CN202211116434.9A CN202211116434A CN115594846B CN 115594846 B CN115594846 B CN 115594846B CN 202211116434 A CN202211116434 A CN 202211116434A CN 115594846 B CN115594846 B CN 115594846B
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- dianhydride
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- 229920001721 polyimide Polymers 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title description 5
- GTDPSWPPOUPBNX-UHFFFAOYSA-N ac1mqpva Chemical compound CC12C(=O)OC(=O)C1(C)C1(C)C2(C)C(=O)OC1=O GTDPSWPPOUPBNX-UHFFFAOYSA-N 0.000 claims abstract description 41
- 239000000178 monomer Substances 0.000 claims abstract description 35
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 26
- CBCKQZAAMUWICA-UHFFFAOYSA-N 1,4-phenylenediamine Chemical compound NC1=CC=C(N)C=C1 CBCKQZAAMUWICA-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000011347 resin Substances 0.000 claims abstract description 19
- 229920005989 resin Polymers 0.000 claims abstract description 19
- 150000004985 diamines Chemical class 0.000 claims abstract description 17
- 230000035699 permeability Effects 0.000 claims abstract description 16
- HLBLWEWZXPIGSM-UHFFFAOYSA-N 4-Aminophenyl ether Chemical compound C1=CC(N)=CC=C1OC1=CC=C(N)C=C1 HLBLWEWZXPIGSM-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000000853 adhesive Substances 0.000 claims abstract description 15
- 230000001070 adhesive effect Effects 0.000 claims abstract description 15
- 239000004952 Polyamide Substances 0.000 claims abstract description 13
- 239000002253 acid Substances 0.000 claims abstract description 13
- 229920002647 polyamide Polymers 0.000 claims abstract description 13
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical group C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000006068 polycondensation reaction Methods 0.000 claims abstract description 9
- 238000002360 preparation method Methods 0.000 claims abstract description 7
- 238000010345 tape casting Methods 0.000 claims abstract description 4
- 239000012298 atmosphere Substances 0.000 claims abstract description 3
- 230000001681 protective effect Effects 0.000 claims abstract description 3
- 238000006243 chemical reaction Methods 0.000 claims description 21
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 7
- 229920005575 poly(amic acid) Polymers 0.000 claims description 7
- 238000004321 preservation Methods 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- ZBMISJGHVWNWTE-UHFFFAOYSA-N 3-(4-aminophenoxy)aniline Chemical compound C1=CC(N)=CC=C1OC1=CC=CC(N)=C1 ZBMISJGHVWNWTE-UHFFFAOYSA-N 0.000 claims description 4
- 239000003880 polar aprotic solvent Substances 0.000 claims description 4
- 238000005266 casting Methods 0.000 claims description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 2
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000002904 solvent Substances 0.000 abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 7
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 108010025899 gelatin film Proteins 0.000 description 10
- 238000006116 polymerization reaction Methods 0.000 description 7
- 238000001035 drying Methods 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 239000012299 nitrogen atmosphere Substances 0.000 description 5
- ZCILODAAHLISPY-UHFFFAOYSA-N biphenyl ether Natural products C1=C(CC=C)C(O)=CC(OC=2C(=CC(CC=C)=CC=2)O)=C1 ZCILODAAHLISPY-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 2
- 238000005187 foaming Methods 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- USIUVYZYUHIAEV-UHFFFAOYSA-N diphenyl ether Natural products C=1C=CC=CC=1OC1=CC=CC=C1 USIUVYZYUHIAEV-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000005476 soldering Methods 0.000 description 1
- 238000011895 specific detection Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
Classifications
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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
- C08G73/1003—Preparatory processes
- C08G73/1007—Preparatory processes from tetracarboxylic acids or derivatives and diamines
- C08G73/1028—Preparatory processes from tetracarboxylic acids or derivatives and diamines characterised by the process itself, e.g. steps, continuous
-
- 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
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
Abstract
The invention discloses a polyimide film with improved adhesive force and moisture permeability rate and a preparation method thereof, which relate to the technical field of polyimide films, and are prepared by carrying out polycondensation reaction on a dianhydride monomer and a diamine monomer to obtain polyamide acid resin, and then carrying out tape casting film forming and thermal imidization treatment, wherein the dianhydride monomer comprises 3,3', 4' -biphenyl tetracarboxylic dianhydride and 4,4' -biphenyl ether dianhydride, and the mole percentage of the dianhydride monomer is 70-99: 1 to 30; the diamine monomer comprises p-phenylenediamine and diaminodiphenyl ether, and the mole percentage of the diamine monomer is 70-99: 1 to 30; the preparation method comprises the steps of adding p-phenylenediamine and diaminodiphenyl ether into a solvent under a protective atmosphere, then adding 3,3', 4' -biphenyl tetracarboxylic dianhydride and 4,4' -biphenyl ether dianhydride in batches for polycondensation reaction, and carrying out tape casting film formation and thermal imidization to obtain the polyimide film. The polyimide film of the invention has the adhesive strength of more than 0.75kgf/cm and the water vapor permeability coefficient of 0.155g/mm 2 24h or more, and has important application in the field of integrated circuits.
Description
Technical Field
The invention relates to the technical field of polyimide films, in particular to a polyimide film with improved adhesive force and moisture permeability rate and a preparation method thereof.
Background
The polyamide acid prepared from 3,3', 4' -biphenyl tetracarboxylic dianhydride (s-BPDA) and p-Phenylenediamine (PDA) can be subjected to tape casting film forming and imidization treatment to obtain a polyimide film, and the polyimide film has high dimensional stability and excellent mechanical properties and is widely used in the field of integrated circuits. However, polyimide films prepared from the above s-BPDA/PDA components have poor surface activity, low adhesion, and are disadvantageous for forming laminates with other materials; in addition, the polyimide film has a low moisture permeability, and when used as a substrate for electronic parts, the polyimide film is exposed to a high temperature during a soldering process, and moisture in the film is vaporized, thereby causing foaming or peeling of the film.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a polyimide film with improved adhesive force and moisture permeability rate and a preparation method thereof, and the polyimide film has excellent mechanical property and high dimensional stability, and also has good adhesive strength and water vapor permeability coefficient.
The polyimide film with improved adhesive force and moisture permeability is prepared through polycondensation of diamine monomer and diamine monomer to obtain polyamide acid resin, casting to form film and thermal imidizing; the dianhydride monomer comprises 3,3', 4' -biphenyl tetracarboxylic dianhydride and 4,4' -biphenyl ether dianhydride, and the mole percentage of the dianhydride monomer is 70-99: 1 to 30; the diamine monomer comprises p-phenylenediamine and diaminodiphenyl ether, and the mole percentage of the diamine monomer is 70-99: 1 to 30.
Preferably, the diaminodiphenyl ether is selected from one of 3,4 '-diaminodiphenyl ether, 4' -diaminodiphenyl ether or a combination thereof.
Preferably, the mole percentage of the p-phenylenediamine and diaminodiphenyl ether is 80-95: 5 to 20.
Preferably, the mole percentage of the 3,3', 4' -biphenyl tetracarboxylic dianhydride and the 4,4' -biphenyl ether dianhydride is 80-95: 5 to 20.
Preferably, the 4,4' -diphenyl ether dianhydride and the diaminodiphenyl ether are used in an amount of 5 to 30 percent of the total mole fraction of all monomers.
All of the above monomers, including the dianhydride monomers and diamine monomers used in the reaction.
The invention also provides a preparation method of the polyimide film with improved adhesive force and moisture permeability, which comprises the following steps:
s1, under the protective atmosphere, adding p-phenylenediamine and diaminodiphenyl ether into a polar aprotic solvent, and stirring and dissolving to obtain a diamine solution;
s2, adding 3,3', 4' -biphenyl tetracarboxylic dianhydride and 4,4' -biphenyl ether dianhydride into diamine solution in batches for polycondensation reaction to prepare polyamide acid resin;
and S3, casting the polyamic acid resin into a film, and performing gradient thermal imidization treatment to obtain the polyimide film.
Preferably, in S1, the polar aprotic solvent is selected from one or more of N-methylpyrrolidone, N-dimethylformamide, and N, N-dimethylacetamide.
Preferably, in S2, the reaction temperature of the polycondensation reaction is 20-30 ℃ and the reaction time is 1-24 h.
Preferably, in S3, the specific operation of the gradient thermal imidization treatment is as follows: the heat preservation is carried out for 5-10 min at 100-130 ℃, for 5-10 min at 180-200 ℃, for 5-10 min at 230-250 ℃, for 5-10 min at 300-320 ℃ and for 5-10 min at 400-420 ℃.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the invention, the flexible ether linkage content in the prepared polyamide acid resin is regulated by introducing biphenyl ether monomer-4, 4' -biphenyl ether dianhydride and diaminodiphenyl ether and regulating the consumption of the biphenyl ether monomer, and compared with the traditional preparation of the polyamide acid resin by polycondensating 3,3', 4' -biphenyl tetracarboxylic dianhydride monomer and p-phenylenediamine monomer, the flexible ether linkage is introduced into a macromolecular sequence structure, so that the flexibility of a molecular chain is improved, and the adhesive strength of the prepared polyimide film is increased.
2. According to the invention, biphenyl ether monomers and other polymerization monomers are uniformly dispersed in a solvent through an in-situ polymerization method, diamine monomers are dissolved in an organic solvent through adjusting the feeding sequence of reaction monomers, and dianhydride is added in batches, so that diamine and dianhydride are fully and uniformly mixed for polycondensation reaction to form a random polymer, the compactness and regularity of polymer molecular chains of 3,3', 4' -biphenyl tetracarboxylic dianhydride units and p-phenylenediamine units are reduced, the permeability of the molecular chains to water vapor is increased, and the moisture permeability of the film is improved.
3. The invention improves the adhesive strength and the water vapor permeability coefficient of the film on the basis of keeping the excellent performance (excellent mechanical property and high dimensional stability) of the polyimide film prepared by the original s-BPDA/PDA component, the adhesive strength of the film is kept above 0.75kgf/cm, and the water vapor permeability coefficient is kept at 0.155g/mm 2 The film is prevented from foaming or peeling off under high-temperature welding for more than 24 hours, and the defects in the application process are overcome.
Detailed Description
The technical scheme of the invention is described in detail through specific embodiments.
Example 1
S1, adding 12.31g of p-phenylenediamine and 1.22g of 4,4 '-diaminodiphenyl ether into a 500ml reaction bottle under a nitrogen atmosphere, then adding 200ml of N, N-dimethylacetamide as a solvent, setting the reaction temperature to 25 ℃, uniformly stirring for 30min, and after confirming that the monomer is dissolved, adding 33.50g of 3,3',4 '-biphenyltetracarboxylic dianhydride and 1.86g of 4,4' -biphenylether dianhydride into the polymerization bottle in four times, and reacting for 12h to finally obtain the polyamic acid resin.
S2, carrying out vacuum defoaming treatment on the polyamide acid resin for 12 hours, and then forming a film on a carrier and drying to prepare a gel film.
S3, heating the gel film in a gradient way, and performing thermal imidization reaction: the polyimide film is finally formed by heat preservation at 120 ℃ for 5min, 180 ℃ for 5min, 250 ℃ for 5min, 320 ℃ for 5min and 400 ℃ for 5 min.
Example 2
S1, adding 12.31g of p-phenylenediamine and 1.22g of 3,4 '-diaminodiphenyl ether into a 500ml reaction bottle under a nitrogen atmosphere, then adding 200ml of N, N-dimethylacetamide as a solvent, setting the reaction temperature to 25 ℃, uniformly stirring for 30min, and after confirming that the monomers are dissolved, adding 28.22g of 3,3',4 '-biphenyltetracarboxylic dianhydride and 7.44g of 4,4' -biphenylether dianhydride into the polymerization bottle in four times for reaction, and finally obtaining the polyamic acid resin.
S2, carrying out vacuum defoaming treatment on the polyamide acid resin for 12 hours, and then forming a film on a carrier and drying to prepare a gel film.
S3, heating the gel film in a gradient way, and performing thermal imidization reaction: the polyimide film is finally formed by heat preservation at 120 ℃ for 5min, 180 ℃ for 5min, 250 ℃ for 5min, 320 ℃ for 5min and 400 ℃ for 5 min.
Example 3
S1, adding 10.39g of p-phenylenediamine and 4.80g of 3,4 '-diaminodiphenyl ether into a 500ml reaction bottle under a nitrogen atmosphere, then adding 200ml of N, N-dimethylacetamide as a solvent, setting the reaction temperature to 25 ℃, uniformly stirring for 30min, and after confirming that the monomers are dissolved, adding 24.71g of 3,3',4 '-biphenyltetracarboxylic dianhydride and 11.16g of 4,4' -biphenylether dianhydride into the polymerization bottle in four times for reaction for 12h to finally obtain the polyamic acid resin.
S2, carrying out vacuum defoaming treatment on the polyamide acid resin for 12 hours, and then forming a film on a carrier and drying to prepare a gel film.
S3, heating the gel film in a gradient way, and performing thermal imidization reaction: the polyimide film is finally formed by heat preservation at 120 ℃ for 5min, 180 ℃ for 5min, 250 ℃ for 5min, 320 ℃ for 5min and 400 ℃ for 5 min.
Example 4
S1, adding 9.07g of p-phenylenediamine and 7.20g of 4,4 '-diaminodiphenyl ether into a 500ml reaction bottle under a nitrogen atmosphere, adding 200ml of N, N-dimethylacetamide as a solvent, setting the reaction temperature to 25 ℃, uniformly stirring for 30min, confirming that the monomers are dissolved, adding 28.22g of 3,3',4 '-biphenyl tetracarboxylic dianhydride and 7.44g of 4,4' -biphenyl ether dianhydride into the polymerization bottle in four times, and reacting for 12h to finally obtain the polyamic acid resin.
S2, carrying out vacuum defoaming treatment on the polyamide acid resin for 12 hours, and then forming a film on a carrier and drying to prepare a gel film.
S3, heating the gel film in a gradient way, and performing thermal imidization reaction: the polyimide film is finally formed by heat preservation at 120 ℃ for 5min, 180 ℃ for 5min, 250 ℃ for 5min, 320 ℃ for 5min and 400 ℃ for 5 min.
Comparative example
S1, adding 12.96g of p-phenylenediamine into a 500ml reaction bottle under a nitrogen atmosphere, then adding 200ml of N, N-dimethylacetamide as a solvent, setting the reaction temperature to 25 ℃, uniformly stirring for 30min, after confirming that the monomer is dissolved, adding 35.20g of 3,3', 4' -biphenyl tetracarboxylic dianhydride into the polymerization bottle for four times, and reacting for 12h to finally obtain the polyamic acid resin.
S2, carrying out vacuum defoaming treatment on the polyamide acid resin for 12 hours, and then forming a film on a carrier and drying to prepare a gel film.
S3, heating the gel film in a gradient way, and performing thermal imidization reaction: the polyimide film is finally formed by heat preservation at 120 ℃ for 5min, 180 ℃ for 5min, 250 ℃ for 5min, 320 ℃ for 5min and 400 ℃ for 5 min.
The polyimide films prepared in examples 1 to 4 and comparative examples of the present invention were subjected to performance test, and specific detection performances and indexes are as follows:
(a) And (3) evaluating the mechanical properties of the film: the elastic modulus is adopted to represent the mechanical property of the film, and the film is tested according to GB/T1040-2018;
(b) Evaluation of film dimensional stability: the linear thermal expansion Coefficient (CTE) is used for representing the dimensional stability of the film, and the film is tested according to GB/T1036-2008;
(c) Film adhesive strength was evaluated: testing was performed according to GB/T4851-2014;
(d) Evaluation of film water vapor transmission coefficient: the test was performed according to GB/T2653-2010.
The detection results are shown in Table 1.
TABLE 1 Performance data for polyimide films prepared in examples 1-4 and comparative example
According to the performance test results of the table, the polyimide film provided by the application has the following characteristicsThe polyimide film prepared by the original s-BPDA/PDA composition is kept excellent in mechanical property and high in dimensional stability, meanwhile, the adhesive force and the moisture permeability rate of the polyimide film are improved, the adhesive strength is kept above 0.75kgf/cm, and the water vapor permeability coefficient is kept at 0.155 (g/mm) 2 24 h) or more, has important applications in the field of integrated circuits.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (8)
1. The polyimide film with improved adhesive force and moisture permeability is prepared by performing polycondensation reaction on a dianhydride monomer and a diamine monomer to obtain polyamide acid resin, and performing tape casting film forming and thermal imidization treatment, and is characterized in that the dianhydride monomer comprises 3,3', 4' -biphenyl tetracarboxylic dianhydride and 4,4' -biphenyl ether dianhydride, and the mole percentage of the dianhydride monomer is 70-99: 1-30 parts; the diamine monomer comprises p-phenylenediamine and diaminodiphenyl ether, and the molar percentage of the diamine monomer is 70-99: 1-30 parts;
the preparation method of the polyimide film with improved adhesive force and moisture permeability comprises the following steps:
s1, under the protective atmosphere, adding p-phenylenediamine and diaminodiphenyl ether into a polar aprotic solvent, and stirring and dissolving to obtain a diamine solution;
s2, adding 3,3', 4' -biphenyl tetracarboxylic dianhydride and 4,4' -biphenyl ether dianhydride into diamine solution in batches for polycondensation reaction to prepare polyamide acid resin;
and S3, casting the polyamic acid resin into a film, and performing gradient thermal imidization treatment to obtain the polyimide film.
2. The polyimide film having improved adhesion and moisture permeation rate of claim 1, wherein the diaminodiphenyl ether is selected from one of 3,4 '-diaminodiphenyl ether, 4' -diaminodiphenyl ether, or a combination thereof.
3. The polyimide film with improved adhesion and moisture permeation rate according to claim 1 or 2, wherein the mole percentage of p-phenylene diamine and diaminodiphenyl ether is 80 to 95: 5-20.
4. The polyimide film having improved adhesion and moisture permeation rate according to claim 1, wherein the mole percentage of 3,3', 4' -biphenyltetracarboxylic dianhydride and 4,4' -biphenyl ether dianhydride is 80 to 95: 5-20.
5. The polyimide film with improved adhesion and moisture permeation rate according to claim 1, wherein the 4,4' -biphenyl ether dianhydride and diaminodiphenyl ether are used in an amount of 5 to 30% of the total mole fraction of all monomers.
6. The polyimide film having improved adhesion and moisture permeation rate according to claim 1, wherein the polar aprotic solvent in S1 is selected from one or more of N-methylpyrrolidone, N-dimethylformamide, N-dimethylacetamide.
7. The polyimide film having improved adhesion and moisture permeation rate according to claim 1, wherein in S2, the reaction temperature of the polycondensation reaction is 20 to 30 ℃ and the reaction time is 1 to 24 hours.
8. The polyimide film having improved adhesion and moisture permeation rate according to claim 1, wherein the gradient thermal imidization treatment in S3 is specifically performed as follows: the heat preservation is carried out at 100-130 ℃ for 5-10 min, 180-200 ℃ for 5-10 min, 230-250 ℃ for 5-10 min, 300-320 ℃ for 5-10 min and 400-420 ℃ for 5-10 min.
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| CN1898084A (en) * | 2004-09-21 | 2007-01-17 | Lg化学株式会社 | Metallic laminate and method for preparing thereof |
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| CN102443264A (en) * | 2011-10-14 | 2012-05-09 | 宁波今山电子材料有限公司 | Production method for formable polyimide film |
| CN107134542A (en) * | 2017-04-10 | 2017-09-05 | 珠海亚泰电子科技有限公司 | Transparent single-side coated copper plate manufacture craft |
| WO2022098042A1 (en) * | 2020-11-04 | 2022-05-12 | 피아이첨단소재 주식회사 | Polyimide film having high dimensional stability, and method for manufacturing same |
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| CN1898084A (en) * | 2004-09-21 | 2007-01-17 | Lg化学株式会社 | Metallic laminate and method for preparing thereof |
| CN102391532A (en) * | 2011-08-26 | 2012-03-28 | 朱宏清 | Biaxially oriented polyimide film for flexible printed circuit board base material and preparation method of biaxially oriented polyimide film |
| CN102443264A (en) * | 2011-10-14 | 2012-05-09 | 宁波今山电子材料有限公司 | Production method for formable polyimide film |
| CN107134542A (en) * | 2017-04-10 | 2017-09-05 | 珠海亚泰电子科技有限公司 | Transparent single-side coated copper plate manufacture craft |
| WO2022098042A1 (en) * | 2020-11-04 | 2022-05-12 | 피아이첨단소재 주식회사 | Polyimide film having high dimensional stability, and method for manufacturing same |
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