CN115594846A - Polyimide film having improved adhesive force and moisture permeation rate and method for preparing the same - Google Patents
Polyimide film having improved adhesive force and moisture permeation rate and method for preparing the same Download PDFInfo
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- CN115594846A CN115594846A CN202211116434.9A CN202211116434A CN115594846A CN 115594846 A CN115594846 A CN 115594846A CN 202211116434 A CN202211116434 A CN 202211116434A CN 115594846 A CN115594846 A CN 115594846A
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- polyimide film
- dianhydride
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- permeation rate
- moisture permeation
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- 229920001721 polyimide Polymers 0.000 title claims abstract description 39
- 239000000853 adhesive Substances 0.000 title claims abstract description 13
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 13
- 238000000034 method Methods 0.000 title claims description 7
- 239000000178 monomer Substances 0.000 claims abstract description 30
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 24
- 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
- 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 18
- 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 17
- WKDNYTOXBCRNPV-UHFFFAOYSA-N bpda Chemical compound C1=C2C(=O)OC(=O)C2=CC(C=2C=C3C(=O)OC(C3=CC=2)=O)=C1 WKDNYTOXBCRNPV-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229920005575 poly(amic acid) Polymers 0.000 claims abstract description 14
- 150000004985 diamines Chemical class 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
- 230000035699 permeability Effects 0.000 claims abstract description 8
- 150000008064 anhydrides Chemical class 0.000 claims abstract description 7
- 238000005266 casting Methods 0.000 claims abstract description 7
- 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 14
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 239000004952 Polyamide Substances 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 6
- 229920002647 polyamide Polymers 0.000 claims description 6
- 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
- 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 6
- 238000002360 preparation method Methods 0.000 abstract description 5
- 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
- 238000011156 evaluation Methods 0.000 description 4
- 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
- 238000012360 testing method Methods 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000007547 defect Effects 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
- 230000002349 favourable effect Effects 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000012643 polycondensation polymerization Methods 0.000 description 1
- 238000005476 soldering Methods 0.000 description 1
- 238000011895 specific detection 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, relating to the technical field of polyimide films, and the polyimide film is obtained by performing polycondensation reaction on a dicarboxylic anhydride monomer and a diamine monomer to obtain polyamic acid resin, and then performing casting film forming and thermal imidization treatment, wherein the dicarboxylic anhydride monomer comprises 3,3',4,4' -biphenyl tetracarboxylic dianhydride and 4,4' -biphenyl ether dianhydride, the molar percentage of the dicarboxylic anhydride monomer is 70-99: 1 to 30; the diamine monomer comprises p-phenylenediamine and diaminodiphenyl ether, and the molar percentage is 70-99: 1 to 30; the preparation method comprises the steps of adding p-phenylenediamine and diaminodiphenyl ether into a solvent under the protective atmosphere, then adding 3,3',4,4' -biphenyl tetracarboxylic dianhydride and 4,4' -biphenyl ether dianhydride in batches for polycondensation, forming a film through casting, and carrying out thermal imideAnd (5) dissolving to obtain the polyimide film. The polyimide film of the present invention has an adhesive strength of 0.75kgf/cm or more and a water vapor permeability of 0.155g/mm 2 More than 24h, 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 permeation rate and a preparation method thereof.
Background
Polyamic acid prepared from 3,3',4,4' -biphenyltetracarboxylic dianhydride (s-BPDA) and p-Phenylenediamine (PDA) is subjected to casting film formation and imidization to obtain a polyimide film which has high dimensional stability and excellent mechanical properties and is widely applied to the field of integrated circuits. However, the polyimide film prepared from the above s-BPDA/PDA component has poor surface activity and low adhesion, and is not favorable for forming a laminate with other materials; the polyimide film has a low moisture permeation rate, and when used as a substrate for electronic parts, the polyimide film is brought into a high-temperature state by soldering treatment, and moisture in the film is vaporized, thereby causing blistering 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 permeation rate and a preparation method thereof.
The polyimide film with improved adhesive force and moisture permeability rate is obtained by performing polycondensation reaction on a dicarboxylic anhydride monomer and a diamine monomer to obtain a polyamic acid resin, and performing casting film forming and thermal imidization treatment; the binary anhydride monomer comprises 3,3',4,4' -biphenyl tetracarboxylic dianhydride and 4,4' -biphenyl ether dianhydride, and the molar percentage is 70-99: 1 to 30; the diamine monomer comprises p-phenylenediamine and diaminodiphenyl ether, and the molar percentage is 70-99: 1 to 30.
Preferably, the diaminodiphenyl ether is selected from one of 3,4 '-diaminodiphenyl ether, 4,4' -diaminodiphenyl ether or a combination thereof.
Preferably, the mole percentage of the p-phenylenediamine and the diaminodiphenyl ether is 80-95: 5 to 20.
Preferably, the mole percentage of 3,3',4,4' -biphenyl tetracarboxylic dianhydride and 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% based on the total mole fraction of all monomers.
All of the above monomers, including the dianhydride monomer and the diamine monomer used in the reaction.
The invention also provides a preparation method of the polyimide film with improved adhesive force and moisture permeation rate, which comprises the following steps:
s1, adding p-phenylenediamine and diaminodiphenyl ether into a polar aprotic solvent under a protective atmosphere, and stirring for dissolving to obtain a diamine solution;
s2, adding 3,3',4,4' -biphenyl tetracarboxylic dianhydride and 4,4' -biphenyl ether dianhydride into the diamine solution in batches, and carrying out polycondensation reaction to obtain polyamic acid resin;
and S3, casting the polyamide 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: preserving heat for 5-10 min at 100-130 ℃, preserving heat for 5-10 min at 180-200 ℃, preserving heat for 5-10 min at 230-250 ℃, preserving heat for 5-10 min at 300-320 ℃, and preserving heat for 5-10 min at 400-420 ℃.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the invention, biphenyl ether monomer-4,4 ' -biphenyl ether dianhydride and diaminodiphenyl ether are introduced, and the amount of the biphenyl ether monomer is adjusted to adjust the content of flexible ether bonds in the prepared polyamide acid resin, compared with the traditional polyamide acid resin prepared by condensation polymerization of 3,3',4,4' -biphenyl tetracarboxylic dianhydride monomer and p-phenylenediamine monomer, the flexible ether bonds are introduced into a macromolecular sequence structure, so that the flexibility of a molecular chain is increased, and the bonding strength of the prepared polyimide film is increased.
2. The invention makes biphenyl ether monomer and other polymerization monomer uniformly disperse in solvent by in-situ polymerization, dissolves diamine monomer into organic solvent by adjusting the feeding sequence of reaction monomer, then adds dianhydride in batches, makes diamine and dianhydride fully and uniformly mixed to carry out polycondensation reaction to form irregular polymer, reduces the compactness and regularity of polymer molecular chains of 3,3',4,4' -biphenyl tetracarboxylic dianhydride unit and p-phenylenediamine unit, thereby increasing the permeability of molecular chains to water vapor and improving the moisture permeability rate of film.
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, the water vapor permeability coefficient is kept at 0.155g/mm 2 And over 24 hours, the phenomena of foaming or peeling of the film under high-temperature welding are avoided, and the defects in the application process are overcome.
Detailed Description
The technical means of the present invention will be described in detail below with reference to specific examples.
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 be 25 ℃, uniformly stirring for 30min, after confirming that monomers are completely dissolved, adding 33.50g of 3,3',4,4 '-biphenyltetracarboxylic dianhydride and 1.86g of 4,4' -biphenylether dianhydride into a polymerization reaction bottle for four times, and reacting for 12h to finally obtain the polyamide acid resin.
S2, performing vacuum defoaming treatment on the polyamic 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 manner, and performing thermal imidization: comprises the steps of preserving heat at 120 ℃ for 5min, preserving heat at 180 ℃ for 5min, preserving heat at 250 ℃ for 5min, preserving heat at 320 ℃ for 5min, preserving heat at 400 ℃ for 5min, and finally forming the polyimide film.
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 be 25 ℃, uniformly stirring for 30min, after confirming that monomers are completely dissolved, adding 28.22g of 3,3',4,4 '-biphenyl tetracarboxylic dianhydride and 7.44g of 4,4' -biphenyl ether dianhydride into a polymerization reaction bottle for four times, and reacting for 12h to finally obtain the polyamic acid resin.
And S2, carrying out vacuum defoaming treatment on the polyamic acid resin for 12h, and then forming a film on the carrier and drying to prepare a gel film.
S3, heating the gel film in a gradient manner, and carrying out thermal imidization: comprises the steps of preserving heat at 120 ℃ for 5min, preserving heat at 180 ℃ for 5min, preserving heat at 250 ℃ for 5min, preserving heat at 320 ℃ for 5min, preserving heat at 400 ℃ for 5min, and finally forming the polyimide film.
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 be 25 ℃, uniformly stirring for 30min, after confirming that monomers are completely dissolved, adding 24.71g of 3,3',4,4 '-biphenyltetracarboxylic dianhydride and 11.16g of 4,4' -biphenylether dianhydride into a polymerization reaction bottle for four times, and reacting for 12h to finally obtain the polyamide acid resin.
S2, performing vacuum defoaming treatment on the polyamic 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 manner, and carrying out thermal imidization: comprises the steps of preserving heat at 120 ℃ for 5min, preserving heat at 180 ℃ for 5min, preserving heat at 250 ℃ for 5min, preserving heat at 320 ℃ for 5min, preserving heat at 400 ℃ for 5min, and finally forming the polyimide film.
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, then adding 200ml of N, N-dimethylacetamide as a solvent, setting the reaction temperature to be 25 ℃, uniformly stirring for 30min, after confirming that monomers are completely dissolved, adding 28.22g of 3,3',4,4 '-biphenyl tetracarboxylic dianhydride and 7.44g of 4,4' -biphenyl ether dianhydride into a polymerization reaction bottle for four times, reacting for 12h, and finally obtaining the polyamic acid resin.
And S2, carrying out vacuum defoaming treatment on the polyamic acid resin for 12h, and then forming a film on the carrier and drying to prepare a gel film.
S3, heating the gel film in a gradient manner, and carrying out thermal imidization: comprises keeping the temperature at 120 ℃ for 5min, keeping the temperature at 180 ℃ for 5min, keeping the temperature at 250 ℃ for 5min, keeping the temperature at 320 ℃ for 5min, and keeping the temperature at 400 ℃ for 5min to finally form the polyimide film.
Comparative example
S1, adding 12.96g of p-phenylenediamine into a 500ml reaction bottle in a nitrogen atmosphere, then adding 200ml of N, N-dimethylacetamide as a solvent, setting the reaction temperature to be 25 ℃, uniformly stirring for 30min, after confirming that monomers are completely dissolved, adding 35.20g of 3,3',4,4' -biphenyltetracarboxylic dianhydride into the polymerization reaction bottle for four times, and reacting for 12h to finally obtain the polyamic acid resin.
And S2, carrying out vacuum defoaming treatment on the polyamic acid resin for 12h, and then forming a film on the carrier and drying to prepare a gel film.
S3, heating the gel film in a gradient manner, and carrying out thermal imidization: comprises the steps of preserving heat at 120 ℃ for 5min, preserving heat at 180 ℃ for 5min, preserving heat at 250 ℃ for 5min, preserving heat at 320 ℃ for 5min, preserving heat at 400 ℃ for 5min, and finally forming the polyimide film.
The polyimide films prepared in the examples 1 to 4 and the comparative example of the invention are subjected to performance tests, and the specific detection performance and indexes are as follows:
(a) Evaluation of mechanical properties of the films: 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 dimensional stability of the film is characterized by a linear Coefficient of Thermal Expansion (CTE) and tested according to GB/T1036-2008;
(c) Evaluation of film adhesion strength: testing according to GB/T4851-2014;
(d) Evaluation of film Water vapor Transmission coefficient: the test was performed according to GB/T26253-2010.
The results are shown in Table 1.
TABLE 1 Performance data of polyimide films prepared in examples 1-4 and comparative example
According to the results of the above-mentioned property tests, the polyimide film provided by the present application has excellent mechanical properties and high dimensional stability of the polyimide film prepared by maintaining the original s-BPDA/PDA composition, and simultaneously improves the adhesive force and moisture permeation rate of the polyimide film, the adhesive strength is maintained above 0.75kgf/cm, and the water vapor permeation coefficient is maintained at 0.155 (g/mm) 2 24 h) or more, has important applications in the field of integrated circuits.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered as the technical solutions and the inventive concepts of the present invention within the technical scope of the present invention.
Claims (9)
1. A polyimide film with improved adhesive force and moisture permeability rate is obtained by performing polycondensation reaction on a dicarboxylic anhydride monomer and a diamine monomer to obtain polyamide acid resin, and then performing casting film forming and thermal imidization treatment, and is characterized in that the dicarboxylic anhydride monomer comprises 3,3',4,4' -biphenyl tetracarboxylic dianhydride and 4,4' -biphenyl ether dianhydride, and the molar percentage is 70-99: 1 to 30; the diamine monomer comprises p-phenylenediamine and diaminodiphenyl ether, and the molar percentage is 70-99: 1 to 30.
2. The polyimide film having improved adhesion and moisture permeation rate according to claim 1, wherein the diaminodiphenyl ether is selected from one of 3,4 '-diaminodiphenyl ether, 4,4' -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-phenylenediamine and diaminodiphenyl ether is 80 to 95:5 to 20.
4. The polyimide film having improved adhesion and moisture permeation rate according to any one of claims 1 to 3, wherein the mole percentage of 3,3',4,4' -biphenyltetracarboxylic dianhydride and 4,4' -biphenylether dianhydride is 80 to 95:5 to 20.
5. The polyimide film having improved adhesion and moisture permeation rate according to any one of claims 1 to 4, wherein 4,4' -biphenyl ether dianhydride and diaminodiphenyl ether are used in an amount of 5 to 30% by mole of the total mole fraction of all monomers.
6. A method for preparing a polyimide film having improved adhesion and moisture permeation rate according to any one of claims 1 to 5, comprising the steps of:
s1, adding p-phenylenediamine and diaminodiphenyl ether into a polar aprotic solvent under a protective atmosphere, and stirring for dissolving to obtain a diamine solution;
s2, adding 3,3',4,4' -biphenyl tetracarboxylic dianhydride and 4,4' -biphenyl ether dianhydride into the diamine solution in batches, and carrying out polycondensation reaction to obtain polyamic acid resin;
and S3, casting the polyamic acid resin into a film, and performing gradient thermal imidization treatment to obtain the polyimide film.
7. The method for preparing a polyimide film having improved adhesion and moisture permeation rate according to claim 6, wherein in S1, the polar aprotic solvent is one or more selected from N-methylpyrrolidone, N-dimethylformamide, and N, N-dimethylacetamide.
8. The method for preparing a polyimide film having improved adhesion and moisture permeation rate according to claim 6, wherein the polycondensation reaction in S2 is carried out at a reaction temperature of 20 to 30 ℃ for a reaction time of 1 to 24 hours.
9. The method for preparing a polyimide film having improved adhesion and moisture permeation rate according to claim 6, wherein the specific operation of the gradient thermal imidization treatment in S3 is as follows: preserving heat for 5-10 min at 100-130 ℃, preserving heat for 5-10 min at 180-200 ℃, preserving heat for 5-10 min at 230-250 ℃, preserving heat for 5-10 min at 300-320 ℃, and preserving heat for 5-10 min at 400-420 ℃.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
-
2022
- 2022-09-14 CN CN202211116434.9A patent/CN115594846B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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| CN115594846B (en) | 2024-03-15 |
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