WO2020101225A1 - Composition de précurseur de polyimide contenant un composé à base de dianhydride réticulable et un antioxydant, et film de polyimide produit à partir de celle-ci - Google Patents

Composition de précurseur de polyimide contenant un composé à base de dianhydride réticulable et un antioxydant, et film de polyimide produit à partir de celle-ci Download PDF

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Publication number
WO2020101225A1
WO2020101225A1 PCT/KR2019/014506 KR2019014506W WO2020101225A1 WO 2020101225 A1 WO2020101225 A1 WO 2020101225A1 KR 2019014506 W KR2019014506 W KR 2019014506W WO 2020101225 A1 WO2020101225 A1 WO 2020101225A1
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Prior art keywords
dianhydride
precursor composition
polyimide precursor
polyimide
polyimide film
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PCT/KR2019/014506
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English (en)
Korean (ko)
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황인환
이익상
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에스케이씨코오롱피아이 주식회사
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Publication of WO2020101225A1 publication Critical patent/WO2020101225A1/fr

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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
    • C08G73/1003—Preparatory processes
    • C08G73/1007—Preparatory processes from tetracarboxylic acids or derivatives and diamines
    • C08G73/101—Preparatory processes from tetracarboxylic acids or derivatives and diamines containing chain terminating or branching agents
    • C08G73/1014—Preparatory processes from tetracarboxylic acids or derivatives and diamines containing chain terminating or branching agents in the form of (mono)anhydrid
    • 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
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/49—Phosphorus-containing compounds
    • C08K5/51—Phosphorus bound to oxygen
    • C08K5/52—Phosphorus bound to oxygen only
    • C08K5/521—Esters of phosphoric acids, e.g. of H3PO4

Definitions

  • the present invention relates to a polyimide precursor composition comprising a crosslinkable dianhydride compound and an antioxidant, and a polyimide film prepared therefrom.
  • Polyimide (PI) is a polymer material with thermal stability based on a rigid aromatic backbone and has mechanical properties such as excellent strength, chemical resistance, weather resistance, and heat resistance based on the chemical stability of the imide ring.
  • polyimide is in the spotlight as a high-performance polymer material that can be applied to a wide range of industries such as electronics, communications, and optics due to its excellent electrical properties such as insulation properties and low dielectric constant.
  • the precursor polyamic acid In order to prepare a high molecular weight polyimide, the precursor polyamic acid must be prepared in high molecular weight, but as the molecular weight of the polyamic acid increases, the viscosity of the polyamic acid solution also increases.
  • polyimide resins undergo chemical changes, that is, oxidation reactions, due to light, heat, pressure, shear force, etc. in the presence of oxygen.
  • This oxidation reaction causes a problem of deteriorating the heat resistance and mechanical properties of the polyimide film produced by generating a change in physical properties by cutting, crosslinking, etc. of the molecular chain in the polyimide resin.
  • a method of adding a small amount of an additive such as an antioxidant is used, and the antioxidant removes oxygen atoms of an already oxidized polyimide resin, thereby stabilizing the polyimide resin.
  • an additive such as an antioxidant
  • a phosphate compound and a sulfur compound are typically used.
  • antioxidants have properties that decompose at high temperatures, and in particular, in the production of polyimide resins, it is common that high temperature heat treatment for imidization is involved, so that the antioxidants are decomposed to reduce the antioxidant effect. In some cases, there is a problem that these effects are not exerted at all.
  • An object of the present invention is to provide a polyimide precursor composition and a polyimide film prepared therefrom, while the viscosity of the polyamic acid solution is kept low to provide high process handling properties, but simultaneously satisfy the heat resistance and mechanical properties of the polyimide film produced therefrom. Is to do.
  • one or more dianhydride monomers and one or more diamine monomers include a polyamic acid solution and an antioxidant prepared by polymerization in an organic solvent, wherein the dianhydride monomer is a crosslinkable dianhydride
  • the polyimide precursor composition containing the compound is disclosed as an essential factor for the realization of the polyimide film satisfying the above properties.
  • the present invention has a practical purpose to provide a specific embodiment thereof.
  • the present invention is a polyamic acid solution prepared by polymerizing one or more dianhydride monomers and one or more diamine monomers in an organic solvent;
  • the dianhydride monomer includes a crosslinkable dianhydride compound, and the crosslinkable dianhydride compound provides a polyimide precursor composition comprising at least one triple bond in a molecular structure.
  • the present invention also, when using the polyimide precursor composition, the solid content is high, the process handling can be improved due to the relatively low viscosity, of course, the polyimide film produced therefrom exhibits excellent heat resistance and mechanical properties Found.
  • dianhydride dianhydride
  • dianhydride is intended to include its precursors or derivatives, which may not technically be dianhydrides, but nevertheless react with diamines to form polyamic acids. And this polyamic acid can be converted back to polyimide.
  • Diamine as used herein is intended to include precursors or derivatives thereof, which may not technically be diamines, but will nevertheless react with dianhydrides to form polyamic acids, which polyamic acids are again polydi Can be converted to mead.
  • the polyimide precursor composition according to the present invention includes: a polyamic acid solution prepared by polymerizing one or more dianhydride monomers and one or more diamine monomers in an organic solvent; And
  • the dianhydride monomer includes a crosslinkable dianhydride compound, and the crosslinkable dianhydride compound comprises at least one triple bond in a molecular structure.
  • the polyimide precursor composition may contain 10 to 20% by weight of solids based on the total weight.
  • the polyimide precursor composition may have a viscosity at 23 ° C of 1,000 to 20,000 cP range, specifically 2,000 to 10,000 cP range, and more specifically 3,000 to 6,000 cP range.
  • the polyimide precursor composition having such a viscosity has an advantage of easy handling in the process in terms of fluidity, and may be advantageous in film forming. Specifically, when the viscosity of the polyimide precursor composition exceeds the above range, higher pressure must be applied by friction with the pipe when the polyimide precursor composition is moved through the pipe during the polyimide production process. Process costs are increased and handling is degraded. In addition, the higher the viscosity, the more time and cost may be required for the mixing process.
  • the content of the dianhydride monomer may be 88 to 99.5 mol%, and the content of the crosslinkable dianhydride compound may be 0.5 to 12 mol%.
  • the content of the dianhydride monomer may be 90 to 99 mol%, and the content of the crosslinkable dianhydride compound may be 1 to 10 mol%.
  • a polyimide precursor composition is prepared by adding a crosslinkable dianhydride-based compound to exceed the above range, the flexibility of the polyimide film may be lowered and formation of a film may be difficult. Since the heat resistance and mechanical properties of the polyimide film produced may be deteriorated, it is not preferable.
  • the crosslinkable dianhydride-based compound may be a compound represented by Formula 1 below.
  • L is a C2-C6 alkynyl group
  • R 1 and R 2 may each independently be selected from the group consisting of C 1 -C 3 alkyl groups, aryl groups, carboxylic acid groups, hydroxy groups, fluoroalkyl groups and sulfonic acid groups,
  • R 1 and R 2 are plural, they may be the same or different from each other,
  • n and m are each independently an integer of 0-3.
  • the crosslinkable dianhydride-based compound may be Ethynylbisphthalicanhydride (EBPA) represented by Chemical Formula 1-1.
  • EBPA Ethynylbisphthalicanhydride
  • the triple bond included in the molecular structure of the cross-linkable dianhydride-based compound is that three electron pairs are involved in the bond, and consists of one sigma ( ⁇ ) bond and two pi ( ⁇ ) bonds. Due to the ⁇ bond, the triple bond shows an unsaturation, which causes an addition reaction or a polymerization reaction well, and has a property of easily cutting.
  • the polyimide precursor composition of the present invention includes a crosslinkable dianhydride-based compound containing the triple bond, and a polyamic acid chain produced by polymerization reaction of a dianhydride monomer and a diamine monomer is a crosslinkable dianhydride system It may include two or more polyamic acid chains having a triple bond derived from the compound.
  • the polyimide precursor composition comprising a polyamic acid chain having the above-described structure has a similar degree to a conventional polyimide precursor composition that is not derived from a crosslinkable dianhydride-based compound since crosslinking between triple bonds is not formed in a solution state. It can represent the viscosity of.
  • one or more crosslinks may be formed by radical reaction between triple bonds contained in different polyamic acid chains.
  • the polyimide precursor composition comprises a first polyamic acid chain having a triple bond derived from a crosslinkable dianhydride compound, and a second polyamic acid chain having a triple bond derived from a crosslinkable dianhydride compound. It may include, and may be a structure including a plurality of polyamic acid chains having a triple bond.
  • radicals derived from a pi bond cut from each of the first triple bond included in the first polyamic acid chain and the second triple bond included in the second polyamic acid chain are formed.
  • the first polyamic acid chain and the second polyamic acid chain may be crosslinked.
  • the first polyamic acid chain and the second polyamic acid chain can form crosslinks between the polyimide chains by the above reaction in the imidation process, and in addition to the first polyamic acid chain and the second polyamic acid chain. Since the plurality of polyamic acid chains each include a plurality of triple bonds, crosslinking as described above may be formed therebetween.
  • crosslinking mechanical properties and heat resistance can be significantly improved compared to polyimide that does not include crosslinking.
  • a polyimide precursor composition having a very high molecular weight to increase the heat resistance and mechanical properties of the polyimide film
  • a polyimide precursor composition is prepared using a crosslinkable dianhydride-based compound, it is relatively Even when a low-viscosity polyimide precursor composition is used, it is possible to exert a similar level of heat resistance and mechanical properties to a polyimide film prepared from a high-viscosity polyimide precursor composition.
  • the antioxidant may have a 5% by weight decomposition temperature of 380 ° C or higher, and specifically 5% by weight decomposition temperature of 400 ° C or higher.
  • the antioxidant may include a compound represented by Formula 2 below.
  • R 1a to R 6a may each independently be selected from the group consisting of C1-C3 alkyl groups, aryl groups, carboxyl groups, hydroxy groups, fluoroalkyl groups, and sulfonic acid groups,
  • R 1a to R 6a are plural, they may be the same or different from each other,
  • n1 is an integer from 1 to 4,
  • n1 to m6 are each independently an integer of 0 to 3.
  • n1 in Formula 2 may be 1, m1 to m6 may be 0, and more specifically, the antioxidant may be a compound of Formula 2-1.
  • antioxidants Since these antioxidants have low volatility and excellent thermal stability, they do not decompose or volatilize during the production process of the polyimide film, and thus exhibit an effect of preventing oxidation of the amide group or the imide group of the polyimide film in the polyimide precursor composition. Can be.
  • the antioxidant may include 0.1 to 2.5 parts by weight based on 100 parts by weight of the solid content of the polyimide precursor composition, and more specifically, 0.1 to 2.0 parts by weight based on 100 parts by weight of the solid content of the polyimide precursor composition.
  • the polyimide precursor composition may be produced by polymerization of one or more dianhydride monomers and one or more diamine monomers.
  • the dianhydride monomer that can be used in the production of the polyamic acid of the present invention may be an aromatic tetracarboxylic dianhydride.
  • the aromatic tetracarboxylic dianhydride is pyromellitic dianhydride (or PMDA), 3,3 ', 4,4'-biphenyltetracarboxylic dianhydride (or BPDA), 2,3,3 ', 4'-biphenyltetracarboxylic dianhydride (or a-BPDA), oxydiphthalic dianhydride (or ODPA), diphenylsulfone-3,4,3', 4'-tetracarboxylic Dianhydride (or DSDA), bis (3,4-dicarboxyphenyl) sulfide dianhydride, 2,2-bis (3,4-dicarboxyphenyl) -1,1,1,3,3,3- Hexafluoropropane dianhydride, 2,3,3 ', 4'-benzophenonetetracarboxylic dianhydride, 3,3', 4,4'-benzophenonetetracarboxylic dianhydride (
  • PMDA pyromellitic dianhydrides
  • s-BPDA '-biphenyltetracarboxylic dianhydride
  • a-BPDA 2,3,3', 4'-biphenyltetracarboxylic dianhydride It may include.
  • the diamine monomers that can be used in the production of the polyamic acid of the present invention are aromatic diamines, and are classified as follows.
  • 1,4-diaminobenzene or paraphenylenediamine, p-PDA
  • 1,3-diaminobenzene 1,4-diaminotoluene
  • 2,4-diaminotoluene 2,6-diaminotoluene
  • 3,5-dia Diamine having one structural benzene nucleus such as minobenzoic acid (or DABA), and the like, and a diamine having a relatively rigid structure
  • Diaminodiphenyl ethers such as 4,4'-diaminodiphenyl ether (or oxidianiline, ODA) and 3,4'-diaminodiphenyl ether, 4,4'-diaminodiphenylmethane (Methylenediamine), 3,3'-dimethyl-4,4'-diaminobiphenyl, 2,2'-dimethyl-4,4'-diaminobiphenyl, 2,2'-bis (trifluoromethyl ) -4,4'-diaminobiphenyl, 3,3'-dimethyl-4,4'-diaminodiphenylmethane, 3,3'-dicarboxy-4,4'-diaminodiphenylmethane , 3,3 ', 5,5'-tetramethyl-4,4'-diaminodiphenylmethane, bis (4-aminophenyl) sulfide, 4,4'-dia
  • diamine monomers that can be particularly preferably used in the present invention include paraphenylenediamine (p-PDA) and 1,3-diaminobenzene (MPD). , 2,4-diaminotoluene, 2,6-diaminotoluene and 3,5-diaminobenzoic acid (DABA).
  • p-PDA paraphenylenediamine
  • MPD 1,3-diaminobenzene
  • DABA 3,5-diaminobenzoic acid
  • the diamine monomer and the dianhydride monomer may be added in substantially equimolar amounts, and in detail, based on 100 mol% of the diamine monomer, the input amount of the dianhydride monomer is 99 mol% to It may be 101 mol%, and more specifically, based on 100 mol% of the diamine monomer, the amount of the dianhydride monomer may be 99 mol% to 99.9 mol%.
  • the dianhydride monomer may include a crosslinkable dianhydride-based compound, and the crosslinkable dianhydride-based compound may include at least one triple bond in a molecular structure.
  • the polyamic acid chain included in the polyimide precursor composition includes one or more polyamic acid chains having a triple bond derived from a crosslinkable dianhydride-based compound, and in step (c), imidization is performed.
  • one or more crosslinks may be formed by radical reaction between triple bonds included in different polyamic acid chains.
  • the polyimide precursor composition having a high molecular weight It is possible to secure a level of heat resistance and mechanical properties similar to those of polyimide films produced from.
  • the second composition In the dianhydride monomer component in excess, in the first composition when the dianhydride monomer component is excessive, in the second composition, the diamine monomer component in excess, the first and second compositions are mixed and used in these reactions And a method in which the whole diamine monomer component and the dianhydride monomer component are substantially equimolar and polymerized.
  • the polymerization method is not limited to the above examples, and any known method can be used.
  • the dianhydride monomer may be appropriately selected from the examples described above, and in detail, in addition to the crosslinkable dianhydride-based compound, pyromellitic dianhydride (PMDA), 3,3 ', 4,4'- Biphenyltetracarboxylic dianhydride (s-BPDA) and 2,3,3 ', 4'-biphenyltetracarboxylic dianhydride (a-BPDA), at least one member selected from the group consisting of It can contain.
  • PMDA pyromellitic dianhydride
  • s-BPDA 3,3 ', 4,4'- Biphenyltetracarboxylic dianhydride
  • a-BPDA 2,3,3 ', 4'-biphenyltetracarboxylic dianhydride
  • the diamine monomer may be appropriately selected from the examples described above, and specifically, paraphenylenediamine (p-PDA), 1,3-diaminobenzene (MPD), 2,4-diaminotoluene, 2,6 -One or more selected from the group consisting of diaminotoluene and 3,5-diaminobenzoic acid (DABA) can be preferably used.
  • p-PDA paraphenylenediamine
  • MPD 1,3-diaminobenzene
  • 2,4-diaminotoluene 2,6 -One or more selected from the group consisting of diaminotoluene and 3,5-diaminobenzoic acid (DABA)
  • DABA 3,5-diaminobenzoic acid
  • the polyimide film may be produced through a thermal imidization method, and chemical imidization method may be performed in parallel.
  • the thermal imidization method is a method of excluding chemical catalysts and inducing an imidization reaction with a heat source such as hot air or an infrared dryer.
  • the thermal imidization method may include the process (c), and the amic acid group present in the gel film is already heat-treated at a variable temperature in the range of 100 to 600 ° C in the process (c). It can be dehydrated, and in detail, the amic acid group present in the gel film can be imidized by heat treatment at 200 to 500 ° C, and more specifically, 300 to 500 ° C.
  • a part of the amic acid (about 0.1 mol% to 10 mol%) may be imidized, and for this, in the process (b), in the range of 50 ° C to 200 ° C,
  • the polyamic acid composition can be dried at variable temperatures, which can also be included in the scope of the thermal imidization method.
  • the polyimide film of the present invention prepared according to the above manufacturing method has a thermal decomposition temperature of 1% by weight of 550 to 620 ° C, a coefficient of thermal expansion (CTE) of 2.0 to 8.0 ppm / ° C, and a glass transition temperature of 400 ° C or more.
  • CTE coefficient of thermal expansion
  • Elongation is 13% or more
  • tensile strength is 270 MPa or more
  • the thickness may be 10 to 20 ⁇ m.
  • the polyimide film of the present invention may have a glass transition temperature of 417 ° C or higher.
  • a polyimide film may be prepared using a dehydrating agent and an imidizing agent according to methods known in the art.
  • the present invention also provides an electronic device including the polyimide film, which may be an electronic device including a flexible circuit board or a display substrate.
  • the polyimide precursor composition according to the present invention includes a crosslinkable dianhydride-based compound containing at least one triple bond in a molecular structure, and thus triple bonds included in different polyamic acid chains during heat treatment for imidization
  • One or more crosslinks may be formed by a radical reaction between them, thereby improving heat resistance and mechanical properties of the polyimide film.
  • the polyimide precursor composition according to the present invention improves heat resistance and mechanical properties during heat treatment for imidization, it is possible to keep the viscosity of the polyimide precursor composition low, thereby significantly improving process handling. .
  • an antioxidant having a 5% by weight decomposition temperature of 380 ° C. or higher included in the polyimide precursor composition has low volatility and excellent thermal stability, so that it is not decomposed or volatilized during the manufacturing process of the polyimide film, and the amide in the polyimide precursor composition The oxidation of the imide group of the group or polyimide film can be prevented, and accordingly, the change in physical properties of the polyimide film can be minimized.
  • the polyimide film has an advantage of satisfying the heat resistance and mechanical properties required for the display substrate.
  • NMP NMP was introduced and the temperature of the reactor was set to 30 ° C, followed by p-PDA as a diamine monomer and BPDA as a dianhydride monomer, and p- It was confirmed that 1 mol of EBPA was added to 100 mol of PDA to completely dissolve it.
  • the compound of Formula 2-1 having a 5 wt% decomposition temperature of about 402 ° C. as an antioxidant is added to the polyamic acid solution and stirred sufficiently until the reaction is completed to obtain a total solid content.
  • NMP is added so that the content is about 15% by weight and the viscosity is about 3,700 cP, and the molar ratio of diamine monomer, dianhydride monomer, and crosslinkable dianhydride compound is 100: 99: 1, and 100 parts by weight of solids
  • a polyimide precursor composition containing 0.5 parts by weight of an antioxidant was prepared.
  • Air bubbles were removed from the polyimide precursor composition through high-speed rotation of 1,500 rpm or more. Thereafter, the defoamed polyimide precursor composition was applied to a glass substrate using a spin coater. Then, under a nitrogen atmosphere and dried at a temperature of 120 ° C. for 30 minutes, a gel film was prepared. Cooling at a rate of 2 ° C / min yielded a polyimide film.
  • the thickness of the prepared polyimide film was 15 ⁇ m.
  • the thickness of the prepared polyimide film was measured using an Anritsu Corporation film thickness tester (Electric Film thickness tester).
  • Example 1 a polyimide film was prepared in the same manner as in Example 1, except that the viscosity of the monomer, additive, and polyimide precursor composition was changed as shown in Table 1 below.
  • Example 1 a polyimide film was prepared in the same manner as in Example 1, except that instead of the compound of Formula 2-1 as an antioxidant, a compound of Formula A having a 5 wt% decomposition temperature of about 377 ° C was added. .
  • Example 1 a polyimide film was prepared in the same manner as in Example 1, except that instead of the compound of Formula 2-1 as an antioxidant, a compound of Formula B having a 5 wt% decomposition temperature of about 338 ° C. was added. .
  • Example 1 100 99 - One Formula 2-1 0.5 3,700
  • Example 2 100 99 - One Formula 2-1 One 3,700
  • Example 3 100 95 - 5 Formula 2-1 0.5 3,700
  • Example 4 100 90 - 10 Formula 2-1 0.5 3,700
  • Example 5 100 99 - One Formula 2-1 0.1 3,700
  • Example 6 100 99 - One Formula 2-1 2 3,700
  • Example 7 100 95 - 5 Formula 2-1 One 3,700
  • Example 8 100 50 49 One Formula 2-1 One 3,600
  • Example 9 100 50 45 5 Formula 2-1 One 3,600
  • Example 10 100 99.5 - 0.5 Formula 2-1 0.5 3,700
  • Example 11 100 88 - 12 Formula 2-1 0.5 3,700
  • Example 12 100 99 - One Formula 2-1 2.1 3,700
  • Example 13 100 99 - One Formula 2-1 2.5 3,700
  • a TA thermomechanical analyzer Q400 model was used, and the polyimide film was cut to a width of 2 mm and a length of 10 mm, and then subjected to a tension of 0.05 N under a nitrogen atmosphere, at a rate of 10 ° C./min, 500 at room temperature. After the temperature was raised to °C, while cooling again at a rate of 10 °C / min was measured the slope of the section from 100 °C to 350 °C.
  • thermogravimetric analysis Q50 model was used, and the polyimide film was heated to 150 ° C. at a rate of 10 min / ° C. under a nitrogen atmosphere to maintain isotherm for 30 minutes to remove moisture. Thereafter, the temperature was raised to 600 ° C at a rate of 10 ° C / min, and the temperature at which 1% weight loss occurred was measured.
  • the polyimide film was cut to a width of 4 mm and a length of 20 mm, and then heated at a rate of 5 ° C./min under a nitrogen atmosphere and a temperature range of 550 ° C. at room temperature.
  • the glass transition temperature was measured under conditions. The glass transition temperature was determined as the maximum peak of tan ⁇ calculated according to the ratio of storage modulus and loss modulus.
  • Example 1 8 565 430 18 302
  • Example 2 6 568 441 22 350
  • Example 5 7 560 410 16 290
  • Example 6 555 420 15 280
  • Example 7 5.1 573 446 23
  • Example 8 3 568 435 16 298
  • Example 9 2.5 568 440 18 305
  • Example 10 10 555 414 16 293
  • Example 11 5.5 560 416 15 283
  • Example 12 15 553 415 14 273
  • Example 13 551 410 13 270
  • Example 14 10 550 410 13 271 Comparative Example 1 12 545 380 13 268 Comparative Example 2 20 557 398 10 260 Comparative Example 3 25 540 368 10 268 Comparative Example 4 8.5 547 382 10 256 Comparative Example 5 13 555 390 8 245 Comparative Example 6 15 538 370 7 250 Comparative Example 7

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Abstract

La présente invention concerne une composition de précurseur de polyimide contenant : une solution d'acide polyamique préparée par polymérisation d'au moins un monomère dianhydride et d'au moins un monomère diamine dans un solvant organique; et un antioxydant ayant une température de décomposition de 5 % en poids supérieure ou égale à 380 °C, le monomère dianhydride comprenant un composé à base de dianhydride réticulable, et le composé à base de dianhydride réticulable comprenant au moins une triple liaison dans sa structure moléculaire.
PCT/KR2019/014506 2018-11-14 2019-10-30 Composition de précurseur de polyimide contenant un composé à base de dianhydride réticulable et un antioxydant, et film de polyimide produit à partir de celle-ci WO2020101225A1 (fr)

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KR1020180139864A KR102004660B1 (ko) 2018-11-14 2018-11-14 가교성 디안하이드라이드계 화합물 및 산화방지제를 포함하는 폴리이미드 전구체 조성물, 이로부터 제조된 폴리이미드 필름

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PCT/KR2019/014506 WO2020101225A1 (fr) 2018-11-14 2019-10-30 Composition de précurseur de polyimide contenant un composé à base de dianhydride réticulable et un antioxydant, et film de polyimide produit à partir de celle-ci

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