CN107936275A - A kind of Kapton of flexibility water white transparency and preparation method thereof - Google Patents
A kind of Kapton of flexibility water white transparency and preparation method thereof Download PDFInfo
- Publication number
- CN107936275A CN107936275A CN201711327732.1A CN201711327732A CN107936275A CN 107936275 A CN107936275 A CN 107936275A CN 201711327732 A CN201711327732 A CN 201711327732A CN 107936275 A CN107936275 A CN 107936275A
- Authority
- CN
- China
- Prior art keywords
- preparation
- glue
- kapton
- white transparency
- film
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 229920003223 poly(pyromellitimide-1,4-diphenyl ether) Polymers 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 229920001721 polyimide Polymers 0.000 claims abstract description 54
- 239000003292 glue Substances 0.000 claims abstract description 42
- 239000009719 polyimide resin Substances 0.000 claims abstract description 22
- 239000004642 Polyimide Substances 0.000 claims abstract description 20
- 229920005575 poly(amic acid) Polymers 0.000 claims abstract description 16
- 239000011521 glass Substances 0.000 claims abstract description 15
- 239000011347 resin Substances 0.000 claims abstract description 11
- 229920005989 resin Polymers 0.000 claims abstract description 11
- 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 10
- 150000004985 diamines Chemical class 0.000 claims abstract description 10
- 239000000126 substance Substances 0.000 claims abstract description 8
- 239000003054 catalyst Substances 0.000 claims abstract description 7
- 239000012024 dehydrating agents Substances 0.000 claims abstract description 7
- 239000002904 solvent Substances 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- 238000010276 construction Methods 0.000 claims abstract description 5
- 150000003949 imides Chemical class 0.000 claims abstract description 5
- 239000002131 composite material Substances 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 24
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical group CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 12
- 239000010410 layer Substances 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 10
- 238000005240 physical vapour deposition Methods 0.000 claims description 10
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical group CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 8
- LGRFSURHDFAFJT-UHFFFAOYSA-N Phthalic anhydride Natural products C1=CC=C2C(=O)OC(=O)C2=C1 LGRFSURHDFAFJT-UHFFFAOYSA-N 0.000 claims description 7
- KMOUUZVZFBCRAM-OLQVQODUSA-N (3as,7ar)-3a,4,7,7a-tetrahydro-2-benzofuran-1,3-dione Chemical compound C1C=CC[C@@H]2C(=O)OC(=O)[C@@H]21 KMOUUZVZFBCRAM-OLQVQODUSA-N 0.000 claims description 6
- 239000004952 Polyamide Substances 0.000 claims description 6
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 6
- 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 description 6
- JHIWVOJDXOSYLW-UHFFFAOYSA-N butyl 2,2-difluorocyclopropane-1-carboxylate Chemical group CCCCOC(=O)C1CC1(F)F JHIWVOJDXOSYLW-UHFFFAOYSA-N 0.000 claims description 6
- 239000003153 chemical reaction reagent Substances 0.000 claims description 6
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 6
- 239000002798 polar solvent Substances 0.000 claims description 6
- 229920002647 polyamide Polymers 0.000 claims description 6
- FYSNRJHAOHDILO-UHFFFAOYSA-N thionyl chloride Chemical compound ClS(Cl)=O FYSNRJHAOHDILO-UHFFFAOYSA-N 0.000 claims description 6
- QAEDZJGFFMLHHQ-UHFFFAOYSA-N trifluoroacetic anhydride Chemical compound FC(F)(F)C(=O)OC(=O)C(F)(F)F QAEDZJGFFMLHHQ-UHFFFAOYSA-N 0.000 claims description 6
- 238000010792 warming Methods 0.000 claims description 6
- 238000005229 chemical vapour deposition Methods 0.000 claims description 5
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 5
- 239000011787 zinc oxide Substances 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 4
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 4
- 229910052731 fluorine Inorganic materials 0.000 claims description 4
- 239000011737 fluorine Substances 0.000 claims description 4
- 229910021389 graphene Inorganic materials 0.000 claims description 4
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 4
- 239000000758 substrate Substances 0.000 claims description 4
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 4
- 229910001887 tin oxide Inorganic materials 0.000 claims description 4
- PZJJKWKADRNWSW-UHFFFAOYSA-N trimethoxysilicon Chemical compound CO[Si](OC)OC PZJJKWKADRNWSW-UHFFFAOYSA-N 0.000 claims description 4
- SGRJLTOOQLQDRH-UHFFFAOYSA-N 2-[[2,4-dicarboxybutyl(hydroxy)phosphoryl]methyl]pentanedioic acid Chemical compound OC(=O)CCC(C(O)=O)CP(O)(=O)CC(C(O)=O)CCC(O)=O SGRJLTOOQLQDRH-UHFFFAOYSA-N 0.000 claims description 3
- ODJQKYXPKWQWNK-UHFFFAOYSA-N 3,3'-Thiobispropanoic acid Chemical compound OC(=O)CCSCCC(O)=O ODJQKYXPKWQWNK-UHFFFAOYSA-N 0.000 claims description 3
- LJMPOXUWPWEILS-UHFFFAOYSA-N 3a,4,4a,7a,8,8a-hexahydrofuro[3,4-f][2]benzofuran-1,3,5,7-tetrone Chemical compound C1C2C(=O)OC(=O)C2CC2C(=O)OC(=O)C21 LJMPOXUWPWEILS-UHFFFAOYSA-N 0.000 claims description 3
- QQGYZOYWNCKGEK-UHFFFAOYSA-N 5-[(1,3-dioxo-2-benzofuran-5-yl)oxy]-2-benzofuran-1,3-dione Chemical compound C1=C2C(=O)OC(=O)C2=CC(OC=2C=C3C(=O)OC(C3=CC=2)=O)=C1 QQGYZOYWNCKGEK-UHFFFAOYSA-N 0.000 claims description 3
- BBTGUNMUUYNPLH-UHFFFAOYSA-N 5-[4-[(1,3-dioxo-2-benzofuran-5-yl)oxy]phenoxy]-2-benzofuran-1,3-dione Chemical compound C1=C2C(=O)OC(=O)C2=CC(OC2=CC=C(C=C2)OC=2C=C3C(=O)OC(C3=CC=2)=O)=C1 BBTGUNMUUYNPLH-UHFFFAOYSA-N 0.000 claims description 3
- WVOLTBSCXRRQFR-SJORKVTESA-N Cannabidiolic acid Natural products OC1=C(C(O)=O)C(CCCCC)=CC(O)=C1[C@@H]1[C@@H](C(C)=C)CCC(C)=C1 WVOLTBSCXRRQFR-SJORKVTESA-N 0.000 claims description 3
- UEEJHVSXFDXPFK-UHFFFAOYSA-N N-dimethylaminoethanol Chemical class CN(C)CCO UEEJHVSXFDXPFK-UHFFFAOYSA-N 0.000 claims description 3
- WVOLTBSCXRRQFR-DLBZAZTESA-M cannabidiolate Chemical compound OC1=C(C([O-])=O)C(CCCCC)=CC(O)=C1[C@H]1[C@H](C(C)=C)CCC(C)=C1 WVOLTBSCXRRQFR-DLBZAZTESA-M 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- GRGRGLVMGTVCNZ-UHFFFAOYSA-N dmmda Chemical compound COC1=CC(CC(C)N)=C(OC)C2=C1OCO2 GRGRGLVMGTVCNZ-UHFFFAOYSA-N 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- ANSXAPJVJOKRDJ-UHFFFAOYSA-N furo[3,4-f][2]benzofuran-1,3,5,7-tetrone Chemical compound C1=C2C(=O)OC(=O)C2=CC2=C1C(=O)OC2=O ANSXAPJVJOKRDJ-UHFFFAOYSA-N 0.000 claims description 3
- 102000006602 glyceraldehyde-3-phosphate dehydrogenase Human genes 0.000 claims description 3
- 108020004445 glyceraldehyde-3-phosphate dehydrogenase Proteins 0.000 claims description 3
- AWJUIBRHMBBTKR-UHFFFAOYSA-N isoquinoline Chemical compound C1=NC=CC2=CC=CC=C21 AWJUIBRHMBBTKR-UHFFFAOYSA-N 0.000 claims description 3
- VMXAIJCDNKFKPO-UHFFFAOYSA-N n-ethynylaniline Chemical compound C#CNC1=CC=CC=C1 VMXAIJCDNKFKPO-UHFFFAOYSA-N 0.000 claims description 3
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 3
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 2
- 150000002466 imines Chemical class 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- 239000004408 titanium dioxide Substances 0.000 claims description 2
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims 3
- -1 Alkynes phthalic anhydride Chemical class 0.000 claims 1
- 150000001263 acyl chlorides Chemical class 0.000 claims 1
- 230000003139 buffering effect Effects 0.000 claims 1
- RHZWSUVWRRXEJF-UHFFFAOYSA-N indium tin Chemical compound [In].[Sn] RHZWSUVWRRXEJF-UHFFFAOYSA-N 0.000 claims 1
- 230000003647 oxidation Effects 0.000 claims 1
- 238000007254 oxidation reaction Methods 0.000 claims 1
- 239000002344 surface layer Substances 0.000 claims 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 13
- 239000001301 oxygen Substances 0.000 abstract description 13
- 229910052760 oxygen Inorganic materials 0.000 abstract description 13
- 230000005540 biological transmission Effects 0.000 abstract description 11
- 238000002834 transmittance Methods 0.000 abstract description 5
- 239000003960 organic solvent Substances 0.000 abstract description 4
- 238000010438 heat treatment Methods 0.000 abstract description 3
- 239000010408 film Substances 0.000 description 18
- 238000009835 boiling Methods 0.000 description 4
- 238000004544 sputter deposition Methods 0.000 description 4
- NDWKKKBYNUUHKJ-UHFFFAOYSA-N C(C1=CC=CC=C1)(=O)OC(C1=CC=CC=C1)=O.C1(=CC=CC=C1)C#C Chemical compound C(C1=CC=CC=C1)(=O)OC(C1=CC=CC=C1)=O.C1(=CC=CC=C1)C#C NDWKKKBYNUUHKJ-UHFFFAOYSA-N 0.000 description 3
- 150000004075 acetic anhydrides Chemical class 0.000 description 3
- 238000013019 agitation Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- MRNHPUHPBOKKQT-UHFFFAOYSA-N indium;tin;hydrate Chemical compound O.[In].[Sn] MRNHPUHPBOKKQT-UHFFFAOYSA-N 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- GTACSIONMHMRPD-UHFFFAOYSA-N 2-[4-[2-(benzenesulfonamido)ethylsulfanyl]-2,6-difluorophenoxy]acetamide Chemical compound C1=C(F)C(OCC(=O)N)=C(F)C=C1SCCNS(=O)(=O)C1=CC=CC=C1 GTACSIONMHMRPD-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 101710130081 Aspergillopepsin-1 Proteins 0.000 description 2
- VGCXGMAHQTYDJK-UHFFFAOYSA-N Chloroacetyl chloride Chemical compound ClCC(Cl)=O VGCXGMAHQTYDJK-UHFFFAOYSA-N 0.000 description 2
- 102100031007 Cytosolic non-specific dipeptidase Human genes 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000010954 inorganic particle Substances 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 238000004506 ultrasonic cleaning Methods 0.000 description 2
- 240000000907 Musa textilis Species 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- UQNCVOXEVRELFR-UHFFFAOYSA-N aminopropylone Chemical compound O=C1C(NC(=O)C(N(C)C)C)=C(C)N(C)N1C1=CC=CC=C1 UQNCVOXEVRELFR-UHFFFAOYSA-N 0.000 description 1
- 229950002372 aminopropylone Drugs 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 239000012769 display material Substances 0.000 description 1
- 238000004100 electronic packaging Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000001301 ethoxy group Chemical group [H]C([H])([H])C([H])([H])O* 0.000 description 1
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 229910052909 inorganic silicate Inorganic materials 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000009738 saturating Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Classifications
-
- 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
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/042—Coating with two or more layers, where at least one layer of a composition contains a polymer binder
- C08J7/0423—Coating with two or more layers, where at least one layer of a composition contains a polymer binder with at least one layer of inorganic material and at least one layer of a composition containing a polymer binder
-
- 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
-
- 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
- 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
- C08G73/1017—Preparatory processes from tetracarboxylic acids or derivatives and diamines containing chain terminating or branching agents in the form of (mono)amine
-
- 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
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/048—Forming gas barrier coatings
-
- 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
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/06—Coating with compositions not containing macromolecular substances
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2379/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2361/00 - C08J2377/00
- C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08J2379/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2479/00—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 C08J2461/00 - C08J2477/00
- C08J2479/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08J2479/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/549—Organic PV cells
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
- Laminated Bodies (AREA)
Abstract
A kind of Kapton of flexibility water white transparency and preparation method thereof, belongs to Kapton field, solves the problems, such as that existing Kapton oxygen and water vapor transmittance are low, thermal coefficient of expansion is excessive.The present invention includes：Diamine and dianhydride dissolving are generated into polyamic acid glue in organic solvent, add dehydrating agent and catalyst completes chemical imidization reaction generation polyimides glue, it is separated out in a solvent and is dried to obtain polyimide resin, it is dissolved in organic solvent and obtains polyimide resin glue, coated on a glass after vacuum defoamation is carried out to it, cool down again after heating flexible water white transparency Kapton；Processing one layer of cushion of generation is carried out to its surface；A strata imide resin glue, the flexible transparent polyimide film for the composite construction that cools down again after heating, obtains are coated with the surface of cushion.The present invention has low oxygen transmission rate, low water vapor transmittance, low thermal coefficient of expansion and high visible light transmissivity.
Description
Technical field
The invention belongs to Kapton technical field, and in particular to a kind of Kapton of flexibility water white transparency
And preparation method thereof.
Background technology
Kapton is a kind of thermal stability, mechanical performance, the material that optical property is excellent and dielectric constant is low,
It has been widely used in flexible printed circuit board (FPC), Electronic Packaging, optical waveguide (Optical Waveguide), liquid crystal
Show in the fields such as alignment film and the fluid channel element (Microfluidic Device) of device (LCD).Flexible water white transparency in recent years
Kapton is as display material, touch module material, solar cell material, gas separation membrane, biology sensor
Material and flexible electronics etc. are paid high attention to.
At present, the oxygen and steam for the flexible transparent polyimide film prepared using existing preparation process are passed through
Rate is higher, and thermal coefficient of expansion is larger, so as to limit application of such film in electronics and biological field.In order to make polyamides
Imines film has relatively low oxygen and water vapor transmittance, low thermal coefficient of expansion, existing to use organosilicate or inorganic mostly
Particle carries out scattered hydridization during polyamic acid or polyimide solution is prepared and handles, inorganic silicon in this processing method
Hydrochlorate or inorganic particle are not easy to disperse in polyamic acid or polyimide solution, it may occur that reunite, additive amount is limited, and inorganic
Silicate or inorganic particle cannot be evenly distributed on film same layer and form effective barrier, influence film light transmission rate and thermal expansion
Coefficient.
The content of the invention
In order to solve, Kapton oxygen and water vapor transmittance prepared existing for existing preparation method are low, heat is swollen
The problem of swollen coefficient is excessive, the present invention provide a kind of Kapton of flexible water white transparency and preparation method thereof.
The present invention is as follows for technical scheme applied to solve the technical problem：
A kind of preparation method of the Kapton of flexible water white transparency of the present invention, comprises the following steps：
Step 1: according to molar ratio it is 1 by diamine and dianhydride:It is molten that 0.95~1.05 ratio is dissolved in aprotonic polar
In agent, when uniform stirring 10~20 is small after add end-capping reagent, continue stirring 3~8 it is small when generate polyamic acid glue；
Step 2: add dehydrating agent and catalyst completion chemical imidization reaction, reaction 10~20 to polyamic acid glue
Hour generation polyimides glue；
Step 3: polyimides glue is separated out drying in deionized water or ethanol, polyimide resin is obtained；
Polyimide resin glue is obtained Step 4: polyimide resin is dissolved in aprotic polar solvent；
Step 5: by polyimide resin glue carry out vacuum defoamation 1~10 it is small when after, be coated uniformly on glass plate,
It is put into baking oven and is warming up to 150~300 DEG C, when oven temperature is down to 25 DEG C, takes out glass plate, obtain flexible water white transparency
Kapton；
Step 6: processing generation a layer thickness is carried out to flexible transparent polyimide film surface less than 150nm's
Cushion；
Step 7: being coated with a strata imide resin glue on the surface of cushion, be put into baking oven and be warming up to 150~
300 DEG C, when oven temperature is down to 25 DEG C, obtain the flexible transparent polyimide film of composite construction.
As preferred embodiment, the diamine be selected from TFDB, HFBAPP, 6FODA, DMMDA, ODA, APB,
One or more in BAPB, PPD, PBDA, GAPD.
As preferred embodiment, the dianhydride be selected from 6FDA, CBDA, HQDPA, BPDA, TDPA, ODPA, PMDA,
One or more in HPMDA, HBPDA.
As preferred embodiment, the end-capping reagent is selected from phthalic anhydride (PA), maleic anhydride (MA), phenylacetylene benzoic anhydride
(PEPA), tetrahydrophthalic anhydride (THPA), acetylenylaniline (APA), to (trimethoxy silicon substrate) aniline (APTS), three ethoxy of aminopropyl
One or more in base silane (APTES).
As preferred embodiment, the aprotic polar solvent is one kind in DMF, DMAc, NMP, DMSo, THF
It is or a variety of.
As preferred embodiment, the gross mass of the diamine and dianhydride account for polyamic acid glue gross mass 10~
20%.
As preferred embodiment, the dehydrating agent is acetic anhydride, trifluoroacetic anhydride, chloroacetic chloride or thionyl chloride.
As preferred embodiment, the catalyst is triethylamine, pyridine, N-N dimethylethanolamines, tert .-butylpyridine
Or isoquinolin.
As preferred embodiment, in step 6, processing institute is carried out to flexible transparent polyimide film surface
The method of use is in sol-gal process, chemical vapor deposition, physical vapour deposition (PVD), magnetron sputtering method, hydrothermal synthesis method
It is one or more.
As preferred embodiment, the cushioning layer material is selected from silica, tin indium oxide, fluorine doped tin oxide, oxygen
Change the one or more in zinc, titanium dioxide, graphene.
The present invention also protects a kind of a kind of Kapton of the flexible water white transparency prepared using above-mentioned preparation method,
Soluble resin is first prepared using chemical imidization method, then soluble resin is deployed into polyamides Asia in organic solvent again
Amine glue is coated film.
The beneficial effects of the invention are as follows：The present invention is directed primarily to a kind of flexible colourless with high visible light transmissivity
The preparation method of bright Kapton, the Kapton for the flexible water white transparency that this method obtains are saturating with low oxygen
Rate and water vapor transmittance are crossed, while there is relatively low thermal coefficient of expansion, extends answering for flexible transparent polyimide film
Use field.
Flexible transparent polyimide film prepared by the present invention has sandwich construction, such as：ABA、ABABA、
ABACA, ABCA etc..Cushion preparation method can be sol-gal process, chemical vapor deposition (CVD), physical vapour deposition (PVD)
(PVD), the methods of magnetron sputtering method, hydrothermal synthesis method in one or more, cushioning layer material is selected from silica (SiO2)、
Tin indium oxide (ITO), fluorine doped tin oxide (FTO), zinc oxide (ZnO2), titanium dioxide (TiO2), one kind in graphene or more
Kind, the buffer layer thickness of acquisition is less than 150nm.
Embodiment
A kind of Kapton of flexible water white transparency of the present invention, is prepared solvable using chemical imidization method first
Soluble resin, is then deployed into polyimides glue again and is coated film by property resin in organic solvent.
Present invention also offers a kind of preparation method of the Kapton of flexible water white transparency, particular by following
Step is realized：
Step 1: according to molar ratio it is 1 by diamine and dianhydride:0.95~1.05 ratio, is dissolved in aprotonic polar
In solvent (one or more in DMF, DMAc, NMP, DMSo, THF, be not limited in this), when uniform stirring 10~20 is small after plus
Enter end-capping reagent (phthalic anhydride, maleic anhydride, phenylacetylene benzoic anhydride, tetrahydrophthalic anhydride, acetylenylaniline, to (trimethoxy silicon substrate) aniline, ammonia
One or more in propyl-triethoxysilicane, are not limited in this), continue to generate polyamic acid glue when stirring 3~8 is small,
The gross mass of diamine and dianhydride monomer accounts for the 10~20% of polyamic acid glue gross mass.
The one kind of diamine in TFDB, HFBAPP, 6FODA, DMMDA, ODA, APB, BAPB, PPD, PBDA, GAPD
Or it is a variety of, it is not limited in this.
The one kind or more of dianhydride in 6FDA, CBDA, HQDPA, BPDA, TDPA, ODPA, PMDA, HPMDA, HBPDA
Kind, it is not limited in this.
End-capping reagent is selected from phthalic anhydride (PA), maleic anhydride (MA), phenylacetylene benzoic anhydride (PEPA), tetrahydrophthalic anhydride (THPA), acetylene
Base aniline (APA), to one kind or more in (trimethoxy silicon substrate) aniline (APTS), aminopropyl triethoxysilane (APTES)
Kind, not limited to this.
Step 2: adding suitable dehydrating agent and catalyst to the polyamic acid glue of generation, it is anti-to complete chemical imidization
Should, when reaction 10~20 is small, generate polyimides glue.
Dehydrating agent is acetic anhydride, trifluoroacetic anhydride, chloroacetic chloride or thionyl chloride, is not limited in this.
Catalyst is triethylamine, pyridine, N-N dimethylethanolamines, tert .-butylpyridine or isoquinolin, is not limited in this.
Step 3: polyimides glue is separated out drying in solvent (deionized water or ethanol, be not limited in this), obtain
Polyimide resin.
Step 4: polyimide resin is dissolved in aprotic polar solvent (one in DMF, DMAc, NMP, DMSo, THF
Kind or it is a variety of, be not limited in this) in obtain polyimide resin glue.
Step 5: by polyimide resin glue carry out vacuum defoamation 1~10 it is small when after, be coated uniformly on cleaning glass
On plate, it is put into baking oven Program and is warming up to 150~300 DEG C, when oven temperature is down to 25 DEG C of environment temperature, takes out glass plate,
Obtain the Kapton of flexible water white transparency.
Step 6: the Kapton surface of above-mentioned acquisition flexibility water white transparency is passed through into sol-gal process, chemical gas
At one or more in the methods of mutually depositing (CVD), physical vapour deposition (PVD) (PVD), magnetron sputtering method, hydrothermal synthesis method
Reason, generation a layer thickness are not more than the cushion of 150nm；Cushioning layer material is selected from silica (SiO2), tin indium oxide
(ITO), fluorine doped tin oxide (FTO), zinc oxide (ZnO2), titanium dioxide (TiO2), the one or more in graphene.
Step 7: being coated with a strata imide resin glue on the surface of cushion, it is put into baking oven Program and is warming up to
150~300 DEG C, when oven temperature is down to 25 DEG C of environment temperature, the flexible transparent polyimide for obtaining composite construction is thin
Film.
It is characteristic of the invention that there is the flexible transparent polyimide film prepared low oxygen and steam to pass through
Rate, low thermal coefficient of expansion, and there is high visible light transmissivity, extend flexible transparent polyimide film application neck
Domain.
Comparative example 1
8.778 grams of TFDB are dissolved into the DMF of 98ml at room temperature, mechanical agitation is being stirred after TFDB is completely dissolved
Mix and add 7.306 grams of 6FDA and 3.226 gram of BPDA under state into above-mentioned solution, generate solid content 15wt%'s when stirring 12 is small
Polyamic acid glue, 11.182g acetic anhydrides and 5.591g triethylamines are added into polyamic acid glue solution, when stirring 12 is small after
Generate polyimide solution.
It is dry by the polyimide solution formed Precipitation in ethanol, obtain polyimide resin.Take suitable
Polyimide resin is deployed into polyimide resin glue in DMAc.After the polyimide resin glue vacuum defoamation,
It is cast on clean glass plate, is placed on warm table when baking 1 is small at 80 DEG C and treats that solvent vapors away, after film hardening, will scribble thin
The glass plate of film is moved into high temperature oven, and baking oven, from room temperature processing to 250 DEG C, is then turned off height with the programming rate of 5 DEG C/min
Warm baking oven makes temperature naturally ring to 25 DEG C of room temperature, the glass plate for scribbling polyimides is taken out from baking oven, into the water by boiling
To boiling, Kapton is peeled off from glass plate.
OTR oxygen transmission rate, moisture-vapor transmission, light transmission rate and the thermal coefficient of expansion of test gained film, the results are shown in Table 1.
Embodiment 2
8.778 grams of TFDB are dissolved into the DMF of 98ml at room temperature, mechanical agitation is being stirred after TFDB is completely dissolved
Mix and add 7.306 grams of 6FDA and 3.226 gram of BPDA under state into above-mentioned solution, generate solid content 15wt%'s when stirring 12 is small
Polyamic acid glue, 11.182g acetic anhydrides and 5.591g triethylamines are added into polyamic acid glue solution, when stirring 12 is small after
Generate polyimide solution.
It is dry by the polyimide solution formed Precipitation in ethanol, obtain polyimide resin.Take suitable
Polyimide resin is deployed into polyimide resin glue in DMAc.After the polyimide resin glue vacuum defoamation,
It is cast on clean glass plate, is placed on warm table when baking 1 is small at 80 DEG C and treats that solvent vapors away, after film hardening, will scribble thin
The glass plate of film is moved into high temperature oven, and baking oven, from room temperature processing to 250 DEG C, is then turned off height with the programming rate of 5 DEG C/min
Warm baking oven makes temperature naturally ring to 25 DEG C of room temperature, the glass plate for scribbling polyimides is taken out from baking oven, into the water by boiling
To boiling, Kapton is peeled off from glass plate.
Film is put into ultrasonic cleaning in ultrasonic cleaning instrument to dry after twenty minutes, is put into magnetic control sputtering device, uses ITO
Target, vacuum 1*10-3Pa, 200 DEG C of base reservoir temperature, sputtering time takes out after 30 seconds, control buffer layer thickness about 100nm.
It is cast a strata imide resin glue again on the surface of the buffer layer, it is small is placed on heating platform baking 1 at 80 DEG C
When treat that solvent vapors away, after film hardening, move into high temperature oven in, baking oven with the programming rate of 5 DEG C/min from room temperature processing to
250 DEG C, high temperature oven is then turned off, treats that temperature naturally rings to room temperature, is taken out from baking oven, obtains that there is the compound of ABA structures
Film.
OTR oxygen transmission rate, moisture-vapor transmission, light transmission rate and the thermal coefficient of expansion of test gained film, the results are shown in Table 1.
Embodiment 3
8.778 grams of TFDB are dissolved into the DMF of 98ml at room temperature, mechanical agitation is being stirred after TFDB is completely dissolved
Mix the lower polyamides that 7.306 grams of 6FDA and 3.226 gram of BPDA are added into above-mentioned solution, solid content 15wt% is generated when stirring 12 is small
Amino acid glue, 11.182g acetic anhydrides and 5.591g triethylamines are added into polyamic acid glue solution, when stirring 12 is small after generate
Polyimide solution.
Apply membrane process such as embodiment 1.
Cushion prepares SiO using magnetron sputtering method (radio-frequency sputtering)2, preparation condition such as embodiment 2, sputtering power
1.5KW, control buffer layer thickness about 140nm.
OTR oxygen transmission rate, moisture-vapor transmission, light transmission rate and the thermal coefficient of expansion of test gained film, the results are shown in Table 1.
Table 1
| LT (%) | Oxygen (mlT-1·m-2) | Vapor (gT-1·m-2) | CTE(ppm/℃) | |
| Comparative example 1 | 88% | 6.73 | 24.77 | 30 |
| Embodiment 2 | 85% | 1.48 | 2.13 | 19 |
| Embodiment 3 | 87% | 0.75 | 0.52 | 13 |
Using the embodiment 2 and embodiment 3 of the method for the invention, cushion is prepared on the basis of comparative example 1, is obtained
Obtained the compound polyimide film of ABA structures.By test result, this method ensure that film has compared with high visible
On the basis of transmitance, the transmitance of oxygen, steam can be effectively reduced, and obtain relatively low thermal coefficient of expansion, such as table 1
It is shown.
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of preparation method of the Kapton of flexibility water white transparency, it is characterised in that comprise the following steps：
Step 1: according to molar ratio it is 1 by diamine and dianhydride:0.95~1.05 ratio is dissolved in aprotic polar solvent
In, when uniform stirring 10~20 is small after add end-capping reagent, continue stirring 3~8 it is small when generate polyamic acid glue；
Step 2: dehydrating agent and catalyst completion chemical imidization reaction are added to polyamic acid glue, when reaction 10~20 is small
Generate polyimides glue；
Step 3: polyimides glue is separated out drying in deionized water or ethanol, polyimide resin is obtained；
Polyimide resin glue is obtained Step 4: polyimide resin is dissolved in aprotic polar solvent；
Step 5: by polyimide resin glue carry out vacuum defoamation 1~10 it is small when after, be coated uniformly on glass plate, be put into
150~300 DEG C are warming up in baking oven, when oven temperature is down to 25 DEG C, glass plate is taken out, obtains the polyamides of flexible water white transparency
Imines film；
Step 6: the buffering that processing generation a layer thickness is less than 150nm is carried out to flexible transparent polyimide film surface
Layer；
Step 7: being coated with a strata imide resin glue on the surface of cushion, it is put into baking oven and is warming up to 150~300
DEG C, when oven temperature is down to 25 DEG C, obtain the flexible transparent polyimide film of composite construction.
2. preparation method according to claim 1, it is characterised in that the diamine be selected from TFDB, HFBAPP, 6FODA,
One or more in DMMDA, ODA, APB, BAPB, PPD, PBDA, GAPD.
3. preparation method according to claim 1, it is characterised in that the dianhydride be selected from 6FDA, CBDA, HQDPA,
One or more in BPDA, TDPA, ODPA, PMDA, HPMDA, HBPDA.
4. preparation method according to claim 1, it is characterised in that the end-capping reagent is selected from phthalic anhydride, maleic anhydride, benzene second
Alkynes phthalic anhydride, tetrahydrophthalic anhydride, acetylenylaniline, to one kind in (trimethoxy silicon substrate) aniline, aminopropyl triethoxysilane or
It is a variety of.
5. preparation method according to claim 1, it is characterised in that the aprotic polar solvent for DMF, DMAc,
One or more in NMP, DMSo, THF.
6. preparation method according to claim 1, it is characterised in that the gross mass of the diamine and dianhydride accounts for polyamide
The 10~20% of sour glue gross mass.
7. preparation method according to claim 1, it is characterised in that the dehydrating agent is acetic anhydride, trifluoroacetic anhydride, second
Acyl chlorides or thionyl chloride；The catalyst is triethylamine, pyridine, N-N dimethylethanolamines, tert .-butylpyridine or isoquinolin.
8. preparation method according to claim 1, it is characterised in that in step 6, to flexible transparent polyimide
Method is selected from sol-gal process, chemical vapor deposition, physical vapour deposition (PVD), magnetron sputtering used by film surface is handled
One or more in method, hydrothermal synthesis method.
9. preparation method according to claim 1, it is characterised in that the cushioning layer material is selected from silica, oxidation
One or more in indium tin, fluorine doped tin oxide, zinc oxide, titanium dioxide, graphene.
10. a kind of polyamides of the flexible water white transparency prepared using the preparation method described in any one in claim 1 to 9 is sub-
Amine film, it is characterised in that soluble resin is first prepared using chemical imidization method, then again by soluble resin organic
Polyimides glue is deployed into solvent and is coated film.
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| CN116284755A (en) * | 2023-04-28 | 2023-06-23 | 华中科技大学 | Degradable polyamide polymer and preparation method and application thereof |
| CN116284755B (en) * | 2023-04-28 | 2024-05-24 | 华中科技大学 | Degradable polyamide polymer and preparation method and application thereof |
| CN118063814A (en) * | 2024-02-03 | 2024-05-24 | 广东中科亚湾科技有限公司 | Two-dimensional polyamide modified polyimide composite material and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN112812353A (en) | 2021-05-18 |
| CN107936275B (en) | 2021-02-26 |
| CN112812353B (en) | 2023-04-28 |
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