CN108117654A - Dimensionally-stablepolyimide polyimide film and preparation method thereof - Google Patents
Dimensionally-stablepolyimide polyimide film and preparation method thereof Download PDFInfo
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- CN108117654A CN108117654A CN201611080978.9A CN201611080978A CN108117654A CN 108117654 A CN108117654 A CN 108117654A CN 201611080978 A CN201611080978 A CN 201611080978A CN 108117654 A CN108117654 A CN 108117654A
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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
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- 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
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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
- 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
Abstract
The invention discloses a kind of Dimensionally-stablepolyimide polyimide films and preparation method thereof.The preparation method comprises the following steps：1) aromatic diamine and aromatic dianhydride are weighed in proportion, it is spare；Wherein：The aromatic diamine is made of rigid aromatic diamine and ODA, wherein rigid aromatic diamine accounts for the 15~30% of aromatic diamine integral molar quantity；Aromatic dianhydride is the combination of PMDA and BPDA, and the wherein mole of BPDA accounts for the 0~40% of aromatic dianhydride integral molar quantity；2) rigid aromatic diamine and partially aromatic dianhydride is taken to be placed in polar non-solute and react, obtains the orderly segment blocked with rigid aromatic diamine；3) ODA is added in into orderly segment, remaining aromatic dianhydride is added in after dissolving and is reacted, obtains having rule copolyamide acid resin solution by what orderly segment induced；4) gained polyamic acid resin solution routinely technique salivation, hot-imide to get.
Description
Technical field
The present invention relates to Kaptons, and in particular to a kind of Dimensionally-stablepolyimide polyimide film and its preparation side
Method.
Background technology
As electronic product is fast-developing towards thin light short and small direction, flexible printed-circuit board market is promoted to expand rapidly
Greatly, important insulating substrate of polyimides (PI) film as flexible printed-circuit board, demand also increases year by year, steady to size
Qualitative requirement is also higher and higher, is mainly reflected in coefficient of thermal expansion, elasticity modulus, percent thermal shrinkage and water absorption rate these indexs
On, that is, requiring the coefficient of thermal expansion of PI films, elasticity modulus is in 4.0~5.0GPa, percent thermal shrinkage close to 18ppm/ DEG C of copper foil
＜ 0.05%, water absorption rate ＜ 2.0%.At present, although China prepares electron level PI films using stretch processes, it obtains
The PI film dimensions stability arrived is poor, can't be used as high-end flexibility coat copper plate base material film, so, domestic flexibility coat copper plate
Manufacturer is nearly all using imported products such as Japan, South Korea.
For domestic high-end PI film productions present situation, the exploitation of Dimensionally-stablepolyimide polyimide film receives domestic major
The concern of enterprise, colleges and universities and institute.The patent of invention of 101358034 A of Publication No. CN, using PMDA, BPDA, ODA
It is mutually combined with PDA monomers and prepares three component polyamic acid (PAA) resins, wherein PDA additive amounts >=60%, BPDA add
Three kinds of resins, are then blended, dimensional stability Kapton are prepared by amount≤10%.The CTE of the film is
18ppm/ DEG C, elasticity modulus is in 4.0GPa, percent thermal shrinkage 0.06%, tensile strength 300MPa, and elongation at break 60% is comprehensive
It is higher to close performance, is mainly used in flexible circuit board FPC, realizes the high performance of FPC.For another example Publication No. CN
102558860 A patents of invention in addition to using PMDA, BPDA, ODA and PDA monomer, also add benzimidazole diamines list
Body, the similary resin syntheses processes being blended again using the copolymerization of three components, obtains CTE down to 8ppm/ DEG C, elasticity modulus 6.8GPa,
The PI films of percent thermal shrinkage 0.01%.From the point of view of these existing patented technologies, in order to improve the dimensional stability of PI films,
The monomer of rigid structure, such as PMDA, BPDA and PDA are added, and rigid unitary additive amount is bigger, dimensional stability is higher.
But research shows when preparing PI films using hot imidization method, if stiff backbone ingredient is bigger, PAA films 150~
200 DEG C of thermal degradation reactions are fiercer, film difficulty it is bigger in addition can not continuous production (《The basis of polyimides and application》,
Japanese polyimides research association compiles, chief editor：The modern refined husband of well, horizontal Tian Linan are compiled for 2002, and p76. He Fei peaks and Wu Zhongwen are translated), system
The high-quality inert type Kapton continuous mass production of taking measurements in Yue Liao China.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of Dimensionally-stablepolyimide polyimide films and preparation method thereof.This
Invention the method is simple to operation, Kapton coefficient of thermal expansion obtained≤22ppm/ DEG C, and elasticity modulus >=
4.0GPa, percent thermal shrinkage≤0.05%, water absorption rate ＜ 2.0%, tensile strength >=200MPa, elongation at break >=50%.
The preparation method of Dimensionally-stablepolyimide polyimide film of the present invention, comprises the following steps：
1) aromatic diamine and aromatic dianhydride are weighed in proportion, it is spare；Wherein：
The aromatic diamine is by rigid aromatic diamine and 4, and 4 ' ,-diaminodiphenyl ether (ODA) composition, wherein, rigidity
Aromatic diamine is selected from 1,4- diaminobenzenes (PDA), 4,4 '-benzidine (DBZ) and 2- (4- aminophenyls) -5- amino
One kind of benzoxazole (BZA) or arbitrary two or more combination, the rigidity aromatic diamine account for aromatic diamine total moles
The 15~30% of amount；
Aromatic dianhydride be pyromellitic acid dianhydride (PMDA) and 3,3 ', 4, the combination of 4 '-biphenyl tetracarboxylic dianhydride (BPDA),
Wherein, 3,3 ', 4, the mole of 4 '-biphenyl tetracarboxylic dianhydride accounts for the 0~40% of aromatic dianhydride integral molar quantity；
2) rigid aromatic diamine and partially aromatic dianhydride is taken to be placed in polar non-solute and react, is obtained with rigidity
The orderly segment of aromatic diamine sealing end；Wherein, the molar ratio of rigid aromatic diamine and aromatic dianhydride is n：N-1, n=4
~10；
3) 4,4 ' are added in into the orderly segment blocked with rigid aromatic diamine obtained by step 2) ,-diamino hexichol
Ether adds in remaining aromatic dianhydride and is reacted after dissolving, obtain having rule copolyamide acid tree by what orderly segment induced
Lipoprotein solution；
4) by the polyamic acid resin solution obtained by step 3) routinely technique salivation, hot-imide, it is steady to obtain size
Sizing Kapton.
In the step 1) of above-mentioned preparation method, molar ratio and the prior art phase of the aromatic diamine and aromatic dianhydride
Together, it is specially 0.9~1.1：1, it is preferably 0.95~1.05：1, more preferably 0.99~1.01：1.In the step, preferably rigidly
Aromatic diamine accounts for the 20~30% of aromatic diamine integral molar quantity, preferably 3, and 3 ', 4, the mole of 4 '-biphenyl tetracarboxylic dianhydride
Account for the 5~25% of aromatic dianhydride integral molar quantity.
The step 2) of above-mentioned preparation method and 3) in, the temperature and time of reaction and polyamic acid resin in the prior art are molten
The polycondensation reaction of liquid is identical, and specifically, the temperature of reaction can be 0~80 DEG C, preferably 0~60 DEG C, more preferable 0~50 DEG C, instead
The total time answered is usually 3~12h.When adding in aromatic dianhydride with aromatic diamine reaction, it is preferred to use it adds in batches,
Reaction can so be made more uniformly, more completely.
In above-mentioned preparation method, the polar non-solute can be conventional selection of the prior art, specifically may be used
Be selected from DMAC N,N' dimethyl acetamide (DMAC), N,N-dimethylformamide (DMF), n-methyl-2-pyrrolidone (NMP),
N, N- diethyl acetamide and one kind in N, N- diethylformamide or arbitrary two or more combination.Work as aprotic, polar
During more than the selected as above two of solvent combination, the proportioning between them can be arbitrary proportioning.The aprotic, polar
The dosage of solvent is same as the prior art, can be specifically when aromatic diamine, aromatic dianhydride and polar non-solute are anti-
When should form polyamic acid resin solution, the solid content in the polyamic acid resin solution is controlled in 10~30w/w%, preferably 12
~25w/w%, further preferably 15~21w/w%.
Present invention additionally comprises the Dimensionally-stablepolyimide polyimide films being prepared by the above method.
Compared with prior art, the method have the characteristics that：
1st, sequentially added first using rigid aromatic diamine and the rigid rigid short chain segment molecule of aromatic dianhydride synthesis
ODA and remaining rigid aromatic dianhydride, being made has rule copolymerization PAA resins；The local order formed using rigid short chain segment molecule
Structure induces follow-up molecule segment ordered arrangement, promotes the generation being orientated in face, increases molecule interchain bulk density, reaches reduction
The CTE of gained film, the purpose for improving elasticity modulus and tensile strength, embody good dimensional stability.
2nd, rigid aromatic diamine mole is reduced to less than the 30% of diamines integral molar quantity, hot imidization system can be mitigated
Rigid chain segment is in 150~200 DEG C of extent of thermal degradation, effective reduction film difficulty, moreover, preparation process is not required to be divided into during standby
3 components prepare PAA resins, and preparation process is simple to operation.
3rd, the film coefficient of thermal expansion as made from the method for the invention≤22ppm/ DEG C, elasticity modulus >=4.0GPa, heat
Shrinking percentage≤0.05%, water absorption rate ＜ 2.0%, tensile strength >=200MPa, elongation at break >=50%.
Specific embodiment
With reference to specific embodiment, the present invention is described in further detail, to more fully understand present disclosure, but
The present invention is not limited to following embodiments.
Embodiment 1
The BZA of 15mol is added in 175kg DMAc, stirs 0.5h, adds the PMDA of 12.5mol, 1h is reacted, then adds
Enter the ODA of 85mol, stirring and dissolving 0.5h, add in the PMDA of 67.1mol, react 1h, add in the BPDA of 20mol, react 5h, obtain
To polyamic acid resin solution.Resin is coated on steel band by polyamic acid resin solution after defoaming by scraper, heating
(160 DEG C) removing solvents, obtain PAA films, then through simple tension, it is thin to obtain dimensional stability PI for 420 DEG C of hot-imides
Film.
Embodiment 2
The BZA of the DBZ and 15mol of 10mol are added in 175kg DMAc, stirs 0.5h, adds the PMDA of 12.5mol
With the BPDA of 8.3mol, 1h is reacted, adds ODA, the stirring and dissolving 0.5h of 75mol, adds in the PMDA of 67.1mol, reacts 1h,
The BPDA of 11.7mol is added in, 5h is reacted, obtains polyamic acid resin solution.Polyamic acid resin solution is passed through after defoaming
Resin coated in (162 DEG C) removing solvents on steel band, are heated, is obtained PAA films by scraper, then through simple tension, 400 DEG C of hot acyls
Imidization obtains dimensional stability PI films.
Embodiment 3
The BZA of the DBZ and 15mol of PDA, 10mol of 5mol are added in 136kg DMAc, 0.5h is stirred, adds
The BPDA of the PMDA and 8.3mol of 16.7mol react 1h, add ODA, the stirring and dissolving 0.5h of 70mol, add in 62.9mol
PMDA, react 1h, add in the BPDA of 11.7mol, react 5h, obtain polyamic acid resin solution.Polyamic acid resin is passed through
Resin is coated on steel band by scraper after defoaming, heats (163 DEG C) removing solvents, obtains PAA films, then through unidirectional drawing
It stretches, 450 DEG C of hot-imides obtain dimensional stability PI films.
Embodiment 4
The BZA of 25mol is added in 175kg DMAc, 0.5h is stirred, adds the PMDA and 20mol of 0.8mol
BPDA reacts 1h, adds ODA, the stirring and dissolving 0.5h of 75mol, adds in the PMDA of 50mol, reacts 1h, is eventually adding
The PMDA of 28.8mol reacts 5h, obtains polyamic acid resin solution.Polyamic acid resin solution is passed through into scraper after defoaming
By resin coated in (168 DEG C) removing solvents on steel band, are heated, PAA films are obtained, then through simple tension, 470 DEG C of hot acid imides
Change, obtain dimensional stability PI films.
Embodiment 5
The BZA of 30mol is added in 176kg NMP, stirs 0.5h, adds the PMDA of 25mol, 1h is reacted, adds
The ODA of 70mol, stirring and dissolving 0.5h add in the BPDA of 20mol, react 1h, are eventually adding the PMDA of 54.6mol, react 5h,
Obtain polyamic acid resin solution.Resin after defoaming by scraper is coated on steel band by polyamic acid resin solution, is added
(158 DEG C) removing solvents of heat, obtain PAA films, then through simple tension, it is thin to obtain dimensional stability PI for 440 DEG C of hot-imides
Film.
Embodiment 6
The PDA of 20mol is added in 166kg DMAc and kg NMP, stirs 0.5h, adds the BPDA of 16.7mol, instead
1h is answered, adds the ODA of 80mol, stirring and dissolving 0.5h, adds in the BPDA of 3.3mol, reacts 1h, adds the PMDA of 60mol,
1h is reacted, is eventually adding the PMDA of 19.6mol, 5h is reacted, obtains polyamic acid resin solution.Polyamic acid resin solution is passed through
Resin is coated on steel band by scraper after defoaming, heats (161 DEG C) removing solvents, obtains PAA films, then through unidirectional drawing
It stretches, 400 DEG C of hot-imides obtain dimensional stability PI films.
Embodiment 7
20mol PDA and 10mol DBZ are added in 200kg DMAc, stir 0.5h, add the PMDA of 25mol, instead
1h is answered, adds the ODA of 70mol, stirring and dissolving 0.5h, adds in the BPDA of 20mol, 1h is reacted, adds 54.6mol's
PMDA reacts 5h, obtains polyamic acid resin solution.Polyamic acid resin solution is coated resin by scraper after defoaming
On steel band, (165 DEG C) removing solvents are heated, obtain PAA films, then through simple tension, 430 DEG C of hot-imides obtain ruler
Very little stable type PI films.
Embodiment 8
Embodiment 7 is repeated, unlike, DMAc mass is 167kg, does not add DBZ, addition 10mol BZA.
Embodiment 9
Embodiment 7 is repeated, unlike, DMAc mass is 162kg, and rigid aromatic diamine only adds 30mol PDA, no
Add DBZ and BZA.
Embodiment 10
20mol PDA and 7mol BZA are added in 163kg DMAc, stir 0.5h, add the PMDA of 22.5mol, instead
1h is answered, adds the ODA of 73mol, stirring and dissolving 0.5h, adds in the PMDA of 67.1mol, 1h is reacted, is eventually adding 10mol's
BPDA reacts 5h, obtains polyamic acid resin solution.Polyamic acid resin solution is coated resin by scraper after defoaming
On steel band, (165 DEG C) removing solvents are heated, obtain PAA films, then through simple tension, 400 DEG C of hot-imides obtain ruler
Very little stable type PI films.
Embodiment 11
Embodiment 10 is repeated, unlike, DMAc mass is 227kg, does not add BPDA, and PMDA additive amounts are 99.6mol.
Embodiment 12
Embodiment 10 is repeated, unlike, solvent is that 170kg DMF, PMDA additive amount are 69.6mol, BPDA additive amounts
For 30mol.
Embodiment 13
Embodiment 10 is repeated, unlike, solvent is that 120kg DMAc and 53kg DMF, PMDA additive amount are 59.6mol,
BPDA additive amounts are 40mol.
Embodiment 14
20mol PDA and 7mol BZA are added in 166kg DMAc, stir 0.5h, add the PMDA of 20.3mol, instead
1h is answered, adds the ODA of 73mol, stirring and dissolving 0.5h, adds in the PMDA of 59.3mol, 1h is reacted, is eventually adding 20mol's
BPDA reacts 5h, obtains polyamic acid resin solution.Polyamic acid resin solution is coated resin by scraper after defoaming
On steel band, (166 DEG C) removing solvents are heated, obtain PAA films, then through simple tension, 400 DEG C of hot-imides obtain ruler
Very little stable type PI films.
Embodiment 15
20mol PDA and 7mol BZA are added in 167kg DMAc, stir 0.5h, add the PMDA of 23.6mol, instead
1h is answered, adds the ODA of 73mol, stirring and dissolving 0.5h, adds in the PMDA of 56.7mol, 1h is reacted, is eventually adding 20mol's
BPDA reacts 5h, obtains polyamic acid resin solution.Polyamic acid resin solution is coated resin by scraper after defoaming
On steel band, (166 DEG C) removing solvents are heated, obtain PAA films, then through simple tension, 400 DEG C of hot-imides obtain ruler
Very little stable type PI films.
Embodiment 16
20mol PDA and 7mol BZA are added in 166kg DMAc, stir 0.5h, add the PMDA of 24.3mol, instead
1h is answered, adds the ODA of 73mol, stirring and dissolving 0.5h, adds in the PMDA of 55.3mol, 1h is reacted, is eventually adding 20mol's
BPDA reacts 5h, obtains polyamic acid resin solution.Polyamic acid resin solution is coated resin by scraper after defoaming
On steel band, (166 DEG C) removing solvents are heated, obtain PAA films, then through simple tension, 400 DEG C of hot-imides obtain ruler
Very little stable type PI films.
Comparative example 1
20mol PDA and 7mol BZA are added in 166kg DMAc, stir 0.5h, add the PMDA of 18mol, reaction
1h adds the ODA of 73mol, stirring and dissolving 0.5h, adds in the PMDA of 61.6mol, reacts 1h, is eventually adding 20mol's
BPDA reacts 5h, obtains polyamic acid resin solution.Polyamic acid resin solution is coated resin by scraper after defoaming
On steel band, (165 DEG C) removing solvents are heated, obtain PAA films, then through simple tension, 400 DEG C of hot-imides obtain PI
Film.
Comparative example 2
20mol PDA and 7mol BZA are added in 166kg DMAc, stir 0.5h, add the PMDA of 24.6mol, instead
1h is answered, adds the ODA of 73mol, stirring and dissolving 0.5h, adds in the PMDA of 55mol, 1h is reacted, is eventually adding 20mol's
BPDA reacts 5h, obtains polyamic acid resin solution.Polyamic acid resin solution is coated resin by scraper after defoaming
On steel band, (170 DEG C) removing solvents are heated, obtain PAA films, then through simple tension, 400 DEG C of hot-imides obtain PI
Film.
Comparative example 3
Embodiment 9 is repeated, unlike, DMAc additive amounts are 160kg, and the additive amount of PDA is 33mol, the additive amount of ODA
For 67mol.
By various embodiments above and each comparative example proportioning data preparation such as the following table 1：
Table 1：
PI film performances made from the various embodiments described above and each comparative example are detected, as a result such as table 2 below：
Table 2：
Claims (5)
1. the preparation method of Dimensionally-stablepolyimide polyimide film, comprises the following steps：
1) aromatic diamine and aromatic dianhydride are weighed in proportion, it is spare；Wherein：
The aromatic diamine is by rigid aromatic diamine and 4, and 4 ' ,-diaminodiphenyl ether composition, wherein, rigid aromatic series two
Amine is one kind selected from 1,4- diaminobenzenes, 4,4 '-benzidine and 2- (4- aminophenyls) -5- An base benzoxazoles or appoints
It anticipates two or more combinations, the rigidity aromatic diamine accounts for the 15~30% of aromatic diamine integral molar quantity；
Aromatic dianhydride be pyromellitic acid dianhydride and 3,3 ', 4, the combination of 4 '-biphenyl tetracarboxylic dianhydride, wherein, 3,3 ', 4,4 '-
The mole of biphenyl tetracarboxylic dianhydride accounts for the 0~40% of aromatic dianhydride integral molar quantity；
2) rigid aromatic diamine and partially aromatic dianhydride is taken to be placed in polar non-solute and react, is obtained with rigid fragrance
The orderly segment of race's diamines sealing end；Wherein, the molar ratio of rigid aromatic diamine and aromatic dianhydride is n：N-1, n=4~10；
3) to add in 4,4 ' in the orderly segment of rigid aromatic diamine sealing end ,-diaminodiphenyl ether is molten obtained by step 2)
Remaining aromatic dianhydride is added in after solution to be reacted, obtain by orderly segment induce have rule copolyamide acid resin it is molten
Liquid；
4) by the polyamic acid resin solution obtained by step 3) routinely technique salivation, hot-imide, obtain dimensional stability
Kapton.
2. preparation method according to claim 1, it is characterised in that：In step 1), aromatic diamine and aromatic dianhydride
Molar ratio be 0.9~1.1：1.
3. preparation method according to claim 1, it is characterised in that：In step 1), the rigidity aromatic diamine accounts for virtue
The 20~30% of fragrant race's diamines integral molar quantity.
4. preparation method according to claim 1, it is characterised in that：In step 1), described 3,3 ', 4,4 '-biphenyl tetracarboxylic acid
The mole of acid dianhydride accounts for the 5~25% of aromatic dianhydride integral molar quantity.
5. the Dimensionally-stablepolyimide polyimide film that method any one of Claims 1 to 4 is prepared.
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| CN110372896A (en) * | 2019-06-20 | 2019-10-25 | 重庆文理学院 | A kind of heat treatment process of low thermal expansion coefficient polyimide |
| CN110437615A (en) * | 2019-08-15 | 2019-11-12 | 无锡高拓新材料股份有限公司 | A kind of dedicated FPC substrate Kapton of LED and preparation method thereof |
| CN111892818A (en) * | 2020-03-27 | 2020-11-06 | 中天电子材料有限公司 | Polyimide colorless transparent film and preparation method and application thereof |
| CN114456381A (en) * | 2022-02-11 | 2022-05-10 | 无锡顺铉新材料有限公司 | Method for preparing polyimide film by uniaxial tension |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109438702A (en) * | 2018-09-29 | 2019-03-08 | 苏州市新广益电子有限公司 | It is a kind of for the TPI film of FPC industry and its preparation and processing method |
| CN109824896A (en) * | 2019-03-12 | 2019-05-31 | 黄山金石木塑料科技有限公司 | A kind of heat resistant and wear resistant polyimide type resin and the preparation method and application thereof |
| CN109824896B (en) * | 2019-03-12 | 2021-07-13 | 黄山金石木塑料科技有限公司 | High-temperature-resistant wear-resistant polyimide resin and preparation method and application thereof |
| CN110372896A (en) * | 2019-06-20 | 2019-10-25 | 重庆文理学院 | A kind of heat treatment process of low thermal expansion coefficient polyimide |
| CN110437615A (en) * | 2019-08-15 | 2019-11-12 | 无锡高拓新材料股份有限公司 | A kind of dedicated FPC substrate Kapton of LED and preparation method thereof |
| CN110437615B (en) * | 2019-08-15 | 2021-12-10 | 无锡高拓新材料股份有限公司 | FPC (flexible printed circuit) base material polyimide film special for LED (light-emitting diode) and preparation method thereof |
| CN111892818A (en) * | 2020-03-27 | 2020-11-06 | 中天电子材料有限公司 | Polyimide colorless transparent film and preparation method and application thereof |
| CN111892818B (en) * | 2020-03-27 | 2022-12-16 | 中天电子材料有限公司 | Polyimide colorless transparent film and preparation method and application thereof |
| CN114456381A (en) * | 2022-02-11 | 2022-05-10 | 无锡顺铉新材料有限公司 | Method for preparing polyimide film by uniaxial tension |
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