CN1733469A - 柔性金属箔-聚酰亚胺层压材料及其制备方法 - Google Patents
柔性金属箔-聚酰亚胺层压材料及其制备方法 Download PDFInfo
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- CN1733469A CN1733469A CNA2005100697859A CN200510069785A CN1733469A CN 1733469 A CN1733469 A CN 1733469A CN A2005100697859 A CNA2005100697859 A CN A2005100697859A CN 200510069785 A CN200510069785 A CN 200510069785A CN 1733469 A CN1733469 A CN 1733469A
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- polyamic acid
- metal foil
- thickness
- kapton
- metal forming
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- 229910052751 metal Inorganic materials 0.000 title claims abstract description 42
- 239000002184 metal Substances 0.000 title claims abstract description 42
- 229920001721 polyimide Polymers 0.000 title claims abstract description 29
- 239000004642 Polyimide Substances 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims abstract description 24
- 229920005575 poly(amic acid) Polymers 0.000 claims abstract description 56
- 239000000853 adhesive Substances 0.000 claims abstract description 29
- 230000001070 adhesive effect Effects 0.000 claims abstract description 29
- 239000000203 mixture Substances 0.000 claims abstract description 27
- CBCKQZAAMUWICA-UHFFFAOYSA-N 1,4-phenylenediamine Chemical compound NC1=CC=C(N)C=C1 CBCKQZAAMUWICA-UHFFFAOYSA-N 0.000 claims abstract description 13
- -1 3,4,3',4'-biphenyltetracarboxylic anhydride Chemical class 0.000 claims abstract description 13
- HLBLWEWZXPIGSM-UHFFFAOYSA-N 4-Aminophenyl ether Chemical compound C1=CC(N)=CC=C1OC1=CC=C(N)C=C1 HLBLWEWZXPIGSM-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229920003223 poly(pyromellitimide-1,4-diphenyl ether) Polymers 0.000 claims description 21
- 239000002648 laminated material Substances 0.000 claims description 11
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 9
- 239000011889 copper foil Substances 0.000 claims description 7
- 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 7
- 239000011888 foil Substances 0.000 abstract description 2
- 239000007795 chemical reaction product Substances 0.000 abstract 3
- VLDPXPPHXDGHEW-UHFFFAOYSA-N 1-chloro-2-dichlorophosphoryloxybenzene Chemical compound ClC1=CC=CC=C1OP(Cl)(Cl)=O VLDPXPPHXDGHEW-UHFFFAOYSA-N 0.000 abstract 1
- 239000012790 adhesive layer Substances 0.000 abstract 1
- 239000002966 varnish Substances 0.000 description 20
- 238000006243 chemical reaction Methods 0.000 description 17
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- 238000000576 coating method Methods 0.000 description 12
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- 238000005259 measurement Methods 0.000 description 8
- 239000012299 nitrogen atmosphere Substances 0.000 description 8
- 238000003756 stirring Methods 0.000 description 7
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 6
- 238000003475 lamination Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 239000004020 conductor Substances 0.000 description 5
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- 229910052757 nitrogen Inorganic materials 0.000 description 4
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- 229910000679 solder Inorganic materials 0.000 description 4
- LFBALUPVVFCEPA-UHFFFAOYSA-N 4-(3,4-dicarboxyphenyl)phthalic acid Chemical compound C1=C(C(O)=O)C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)C(C(O)=O)=C1 LFBALUPVVFCEPA-UHFFFAOYSA-N 0.000 description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- 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 description 3
- 230000008901 benefit Effects 0.000 description 3
- WFKAJVHLWXSISD-UHFFFAOYSA-N isobutyramide Chemical compound CC(C)C(N)=O WFKAJVHLWXSISD-UHFFFAOYSA-N 0.000 description 3
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- WZCQRUWWHSTZEM-UHFFFAOYSA-N 1,3-phenylenediamine Chemical compound NC1=CC=CC(N)=C1 WZCQRUWWHSTZEM-UHFFFAOYSA-N 0.000 description 2
- YEJRWHAVMIAJKC-UHFFFAOYSA-N 4-Butyrolactone Chemical compound O=C1CCCO1 YEJRWHAVMIAJKC-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
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- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 2
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 239000004952 Polyamide Substances 0.000 description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 2
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- AMXOYNBUYSYVKV-UHFFFAOYSA-M lithium bromide Chemical compound [Li+].[Br-] AMXOYNBUYSYVKV-UHFFFAOYSA-M 0.000 description 2
- 229940018564 m-phenylenediamine Drugs 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
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- GEYOCULIXLDCMW-UHFFFAOYSA-N 1,2-phenylenediamine Chemical compound NC1=CC=CC=C1N GEYOCULIXLDCMW-UHFFFAOYSA-N 0.000 description 1
- VQVIHDPBMFABCQ-UHFFFAOYSA-N 5-(1,3-dioxo-2-benzofuran-5-carbonyl)-2-benzofuran-1,3-dione Chemical compound C1=C2C(=O)OC(=O)C2=CC(C(C=2C=C3C(=O)OC(=O)C3=CC=2)=O)=C1 VQVIHDPBMFABCQ-UHFFFAOYSA-N 0.000 description 1
- 229910000975 Carbon steel Inorganic materials 0.000 description 1
- 206010013786 Dry skin Diseases 0.000 description 1
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- 150000008065 acid anhydrides Chemical class 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 150000004982 aromatic amines Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229930188620 butyrolactone Natural products 0.000 description 1
- 239000010962 carbon steel Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 150000001896 cresols Chemical class 0.000 description 1
- SBZXBUIDTXKZTM-UHFFFAOYSA-N diglyme Chemical compound COCCOCCOC SBZXBUIDTXKZTM-UHFFFAOYSA-N 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 239000003480 eluent Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 229920001973 fluoroelastomer Polymers 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
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- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
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- 150000002989 phenols Chemical class 0.000 description 1
- 238000009832 plasma treatment Methods 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
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- 230000001681 protective effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- APSBXTVYXVQYAB-UHFFFAOYSA-M sodium docusate Chemical compound [Na+].CCCCC(CC)COC(=O)CC(S([O-])(=O)=O)C(=O)OCC(CC)CCCC APSBXTVYXVQYAB-UHFFFAOYSA-M 0.000 description 1
- HXJUTPCZVOIRIF-UHFFFAOYSA-N sulfolane Chemical compound O=S1(=O)CCCC1 HXJUTPCZVOIRIF-UHFFFAOYSA-N 0.000 description 1
- 238000010301 surface-oxidation reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
Classifications
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- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
- B32B7/04—Interconnection of layers
- B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
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- E—FIXED CONSTRUCTIONS
- E01—CONSTRUCTION OF ROADS, RAILWAYS, OR BRIDGES
- E01D—CONSTRUCTION OF BRIDGES, ELEVATED ROADWAYS OR VIADUCTS; ASSEMBLY OF BRIDGES
- E01D21/00—Methods or apparatus specially adapted for erecting or assembling bridges
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B15/08—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B27/28—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42
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- B32B27/34—Layered products comprising a layer of synthetic resin comprising polyamides
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K1/00—Printed circuits
- H05K1/02—Details
- H05K1/03—Use of materials for the substrate
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- H05K1/0346—Organic insulating material consisting of one material containing N
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B2307/30—Properties of the layers or laminate having particular thermal properties
- B32B2307/306—Resistant to heat
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B2307/70—Other properties
- B32B2307/74—Oxygen absorber
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- E—FIXED CONSTRUCTIONS
- E01—CONSTRUCTION OF ROADS, RAILWAYS, OR BRIDGES
- E01D—CONSTRUCTION OF BRIDGES, ELEVATED ROADWAYS OR VIADUCTS; ASSEMBLY OF BRIDGES
- E01D19/00—Structural or constructional details of bridges
- E01D19/10—Railings; Protectors against smoke or gases, e.g. of locomotives; Maintenance travellers; Fastening of pipes or cables to bridges
- E01D19/106—Movable inspection or maintenance platforms, e.g. travelling scaffolding or vehicles specially designed to provide access to the undersides of bridges
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- E—FIXED CONSTRUCTIONS
- E04—BUILDING
- E04G—SCAFFOLDING; FORMS; SHUTTERING; BUILDING IMPLEMENTS OR AIDS, OR THEIR USE; HANDLING BUILDING MATERIALS ON THE SITE; REPAIRING, BREAKING-UP OR OTHER WORK ON EXISTING BUILDINGS
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- E—FIXED CONSTRUCTIONS
- E04—BUILDING
- E04G—SCAFFOLDING; FORMS; SHUTTERING; BUILDING IMPLEMENTS OR AIDS, OR THEIR USE; HANDLING BUILDING MATERIALS ON THE SITE; REPAIRING, BREAKING-UP OR OTHER WORK ON EXISTING BUILDINGS
- E04G3/00—Scaffolds essentially supported by building constructions, e.g. adjustable in height
- E04G3/28—Mobile scaffolds; Scaffolds with mobile platforms
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K2201/00—Indexing scheme relating to printed circuits covered by H05K1/00
- H05K2201/01—Dielectrics
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- H05K2201/0145—Polyester, e.g. polyethylene terephthalate [PET], polyethylene naphthalate [PEN]
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K2201/00—Indexing scheme relating to printed circuits covered by H05K1/00
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- H05K2201/0137—Materials
- H05K2201/0154—Polyimide
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K2201/00—Indexing scheme relating to printed circuits covered by H05K1/00
- H05K2201/03—Conductive materials
- H05K2201/0332—Structure of the conductor
- H05K2201/0335—Layered conductors or foils
- H05K2201/0355—Metal foils
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/38—Improvement of the adhesion between the insulating substrate and the metal
- H05K3/386—Improvement of the adhesion between the insulating substrate and the metal by the use of an organic polymeric bonding layer, e.g. adhesive
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- 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
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
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- Y10T428/31678—Of metal
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Landscapes
- Engineering & Computer Science (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Architecture (AREA)
- Civil Engineering (AREA)
- Structural Engineering (AREA)
- Laminated Bodies (AREA)
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Abstract
一种柔性金属箔-聚酰亚胺层压材料,其通过居间的粘合剂层将聚酰亚胺薄膜连接到金属箔上而制备。粘合剂为聚酰胺酸混合物,包括:(A)3,4,3′,4′-联苯基四羧酸酐与对苯二胺的反应产物,(B)3,4,3′,4′-联苯基四羧酸酐与4,4′-二氨基二苯醚的反应产物,和(C)均苯四酸二酐与4,4′-二氨基二苯醚的反应产物,其中(A+B)/C的重量比为75/25-25/75。该方法简单、价廉,并且在保持聚酰亚胺抗热性的同时得到具有改善的剥离强度和抗卷曲性的柔性金属箔-聚酰亚胺层压材料。
Description
技术领域
本发明涉及用于电子元件,尤其是用于印刷电路板的柔性金属箔-聚酰亚胺层压材料,及其制备方法。
背景技术
JP-A62-212140中公开了一种制备柔性基体的方法(标记为方法1),其中将聚酰亚胺前体树脂溶液直接涂覆在导体上,然后干燥和固化。方法1中没有使用任何粘合剂,然而却具备了降低的卷曲性和改善的抗热性的优点。尽管具备了上述优点,由于使用了特定类型的聚酰亚胺前体,部分卷曲和较差粘合强度的问题会更突出。JP-A 2-180682、JP-A 2-180679、JP-A 1-245586和JP-A2-122697中也公开了一种方法(标记为方法2),其中将聚酰亚胺前体树脂溶液分次地涂复于导体上。
在通过将聚酰亚胺前体树脂溶液涂复于导体上以制备柔性基体的方法中,柔性基体缺乏所谓的“整体性(body)”(或一种刚度),并且如果最终得到的聚酰亚胺层的厚度小于20微米其难于进行处理。因此,该聚酰亚胺前体树脂必须较厚地使用并固化到导体上,以使最终得到的聚酰亚胺层具有20微米或更高的厚度。难于将厚涂层使用均匀,通常将导致厚度不均,亦即涂布失败。在这方面,方法(2)中的分次涂复具有如下倾向:随着使用步骤的数目增加,厚度不均将变得非常显著。此外,方法(2)的分次涂复在整个生产过程中需要消耗大量时间,因为涂复和干燥步骤必须不断重复进行。
发明内容
本发明的一个目标是提供柔性金属箔-聚酰亚胺层压材料,其充分利用了聚酰亚胺树脂所具备的抗热性优点,具有改进的剥离强度和最小化的卷曲度;及其制备方法。
在通过中间粘合层将金属箔连接到聚酰亚胺薄膜上以制备柔性金属箔-聚酰亚胺层压材料时,本发明人试图使用聚酰胺酸作为粘合剂。现已发现,当聚酰胺酸的混合物:(A)3,4,3′,4′-联苯基四羧酸酐与对苯二胺的反应产物、(B)3,4,3′,4′-联苯基四羧酸酐与4,4′-二氨基二苯醚的反应产物和(C)均苯四酸二酐与4,4′-二氨基二苯醚的反应产物,以(A+B)/C的重量比为75/25-25/75作为粘合剂使用时,将会得到充分利用了具有抗热性聚酰亚胺树脂性能的柔性金属箔-聚酰亚胺层压材料。
本发明一方面提供一种柔性金属箔-聚酰亚胺层压材料,其包括金属箔和聚酰亚胺薄膜,其上为二者之间的粘合剂层。粘合剂层通过聚酰胺酸混合物的亚胺化反应得到,该聚酰胺酸混合物包括:
(A)聚酰胺酸,其为3,4,3′,4′-联苯基四羧酸酐与对苯二胺的反应产物,
(B)聚酰胺酸,其为3,4,3′,4′-联苯基四羧酸酐与4,4′-二氨基二苯醚的反应产物,和
(C)聚酰胺酸,其为均苯四酸二酐与4,4-二氨基二苯醚的反应产物,其中(A+B)/C的重量比为75/25-25/75。
本发明另一方面提供一种制备柔性金属箔-聚酰亚胺层压材料的方法,其包括通过位于其间的粘合剂层将金属箔粘结到聚酰亚胺薄膜上,其中使用上述聚酰胺酸混合物作为粘合剂。该层压材料优选按照下述方法制备:将粘合剂使用于金属箔上,并将聚酰亚胺薄膜粘结到金属箔上,以使粘合剂层位于两者之间。
在优选实施方案中,聚酰胺酸混合物含有A/B重量比为10/90-90/10的聚酰胺酸(A)和(B)。典型地,金属箔为厚度至少为9μm的铜箔,聚酰亚胺薄膜具有至少12μm的厚度,并且粘合剂层具有高达10μm的厚度。
本发明的层压材料制备方法简便、廉价,并且得到具有所有聚酰亚胺特性的柔性金属箔-聚酰亚胺层压材料,其在维持聚酰亚胺的抗热性的同时,具备了改良的剥离强度和抗卷曲性。
具体实施方式
本发明的柔性金属箔-聚酰亚胺层压材料为金属箔和聚酰亚胺薄膜的叠层物,粘合剂层位于其间。此处使用的粘合剂为聚酰胺酸混合物,其包括:
(A)聚酰胺酸,其为3,4,3′,4′-联苯基四羧酸酐与对苯二胺的反应产物,
(B)聚酰胺酸,其为3,4,3′,4′-联苯基四羧酸酐与4,4′-二氨基二苯醚的反应产物,和
(C)聚酰胺酸,其为均苯四酸二酐与4,4’-二氨基二苯醚的反应产物,其中(A+B)/C的重量比为75/25-25/75。粘合剂层通过聚酰胺酸混合物的亚胺化反应得到。
用作粘合剂的聚酰胺酸混合物含有三种不同的聚酰胺酸(A)、(B)和(C),其以如下比例存在:(A+B)/C的重量比为75/25-25/75,优选70/30-30/70,更优选60/40-40/60。如果(A+B)/C的混和比超过75/25,则相对于金属箔的剥离强度将变弱。如果(A+B)/C的混和比低于25/75,则粘合剂层本身易于卷曲,而这在处理中是不希望的。
在优选实施方案中,聚酰胺酸混合物含有聚酰胺酸(A)和(B),其中A/B重量比为10/90-90/10,更优选的是15/85-85/15,十分优选的是20/80-80/20。如果A/B重量比超过90/10,剥离强度呈降低趋势。如果A/B重量比低于10/90,粘合剂层可能在尺寸稳定性上降级。
聚酰胺酸(A)、(B)和(C)可以使用上述单体通过已知方法制备。在反应中使用溶剂以制备这些聚酰胺酸(A)、(B)和(C)。合适的溶剂的例子包括:二甲基乙酰胺(DMAc)、N-甲基吡咯烷酮(NMP)、二甲基亚砜(DMSO)、硫酸二甲酯、环丁砜、丁内酯、甲酚、苯酚、卤代苯酚、环己酮、二噁烷、四氢呋喃和二甘醇二甲醚,并优选N,N′-二甲基乙酰胺和N-甲基-2-吡咯烷酮。所有反应都可以在任何一种上述溶剂单独使用或其混合物中、于10-40℃的温度和至多30%的反应溶液浓度下进行。优选以0.95∶1.00-1.05∶1.00的摩尔比,更优选在氮气气氛下,使芳香族四羧酸酐与芳香族胺反应。在此反应中,如何溶解和加入起始单体并没有特别限定。
通过使用聚苯乙烯作为标样的凝胶渗透色谱法(GPC)进行测量,聚酰胺酸(A)、(B)和(C)均优选具有10,000-100,000的重均分子量,更优选10,000-50,000。当Mw超过100,000时,反应溶液粘度增大。当Mw低于10,000时,相对于金属箔的粘合力变弱。
已知GPC测量在如下条件下进行:
测量条件:
柱:Shodex KD-80MX2
洗脱液:四氢呋喃/二甲基甲酰胺=1/1(10mM LiBr)
流速:RI
设备:HLC-8020(Toso有限公司)
由三种组分(A)、(B)和(C)混和得到的液体混合物的粘度优选为于25℃时的1,500-4,000mPa·s,更优选于25℃时的2,00o-3,500mPa·s。小于1,500mPa·s或大于4,000mPa·s的粘度将使其难于用于金属箔上。粘度测量时应当注意,使用包括单筒旋转粘度计、作为辅助仪器的校准温度计和具有循环泵的恒温箱(保持在25℃)的体系,并且当样品温度达到25℃时进行测量。
组分(A)、(B)和(C)的混合物通过将聚酰胺酸合成品的反应溶液混合在一起得到,然后作为清漆涂覆到金属箔或聚酰亚胺薄膜上,优选涂覆到金属箔上。清漆优选含有8-15重量%的得自组分(A)、(B)和(C)混合物的固体。当固体含量小于8重量%时,清漆粘度太低而难以使用,通常导致涂层变化。当固体含量大于15重量%时,清漆粘度太高而难于处理。清漆优选施加到这种构造,以使亚胺化反应固化得到的涂层具有10μm或更小的厚度。
此处使用的术语“清漆”等价于聚酰胺酸混合物。
在使用清漆之前,为了改善各种特性可以混合无机物、有机物或纤维。还可以加入添加剂,例如加入抗氧化剂以防止导体氧化,或加入硅烷偶合剂以提高粘合力。
在柔性金属箔-聚酰亚胺层压材料中使用的金属箔的例子包括铜、铝、铁和镍。这些例子中,优选轧制铜箔。此处使用的金属箔优选具有5-100μm的厚度。尤其优选具有至少9μm厚度的轧制铜箔。太薄的金属箔具有低强度(弱整体性),并且在清漆涂布和层压步骤期间容易褶皱,有时需要使用保护装置。
此处使用的聚酰亚胺薄膜应当优选具有较高初始抗张模量,并具有近似于铜的线膨胀系数。更具体的说,初始抗张模量至少为325kg/mm2(ASTM D882),线膨胀系数在100-200℃(TMA)的温度范围内约为1.6×10-5/℃。这种聚酰亚胺薄膜通常为购自Dupont的Kapton和购自Kaneka公司的Apical。聚酰亚胺薄膜优选具有7.5-125μm,更优选至少12μm的厚度。
在层压步骤之前,聚酰亚胺薄膜可以进行预处理,例如在聚酰亚胺薄膜的表面进行等离子处理或蚀刻处理。
在本发明的优选实施方案中,聚酰胺酸混合物或清漆涂覆到金属箔的表面并干燥。在此步骤中使用的设备和方法没有特别限定。可以使用任何涂布没备,包括弧形涂布机(comma coaters)、T模头涂布(T dies)、辊式涂布机、刀涂机、逆向涂布机(reverse coaters)和压边涂敷(lip coaters)。
在本发明的优选实施方案中,聚酰胺酸混合物或清漆涂复到金属箔的表面并干燥以形成粘合剂层,然后通过所需方法,例如辊压处理,在其上对聚酰亚胺薄膜进行层压。辊压处理应当在至少加热轧辊以使其与金属箔接触的同时进行。加热轧辊的方式包括使用热油或蒸汽直接加热轧辊。对于轧辊的材料,可以使用金属轧辊,例如碳钢,和橡胶辊,例如耐热氟橡胶和硅橡胶。虽然辊压处理条件没有特别限定,优选条件包括100-150℃的温度,其低于聚酰胺酸溶剂的沸点,以及5-100kg/cm的线性压力。
层压在干燥(除去溶剂)和亚胺化反应之后进行。可以进行干燥直到除去溶剂,一般为约3-30小时。亚胺化反应在除去溶剂后立即进行,并且可以以常规方法在减压条件下、在足够低氧气浓度条件下(通常至多2体积%)以防止金属箔表面氧化,或者在氮保护气氛下在250-350℃进行约3-20小时。在除去溶剂和亚胺化反应期间,层压材料可以为片形或卷形。如果为卷形,如何缠绕成卷并不重要,例如金属箔可以在内侧或外侧,并且隔层可以位于其中。
在本发明方法中涉及的层压后的除去溶剂和亚胺化反应期间,层压后可能存在剩余的溶剂和亚胺化反应生成的水,这些都将被除去。然后将优选以松卷绕的卷或具有不同间隔材料的隔离层的卷轴形式的层压材料进行热处理。
应当注意,粘合剂层优选具有至多10μm的厚度,更优选3-7μm,特别优选5-6μm。粘合剂层太厚,则在涂布后难于干燥。粘合剂层太薄,则其对金属箔的粘合力较差。
实施例
本发明的实施例与对比实施例一起如下给出,其仅仅用于说明而并非对本发明的限制。
实施例1
聚酰胺酸的合成
(A)将108g对苯二胺加入到3,216g N-甲基-2-吡咯烷酮中,氮气气氛下搅拌溶解。向此溶液中缓慢加入294g 3,4,3′,4′-联苯基四羧酸二酐,以使内部温度不超过10℃。添加完成后,内部温度上升至40℃,在此温度下反应2小时。所得聚酰胺酸通过GPC测量具有42,000的重均分子量。由此得到含12.5重量%聚酰胺酸的反应溶液。
(B)将200g 4,4′-二氨基二苯醚加入到3,952g N-甲基-2-吡咯烷酮中,其在氮气气氛下搅拌溶解。向此溶液中缓慢加入294g 3,4,3′,4′-联苯基四羧酸二酐,以使内部温度不超过10℃。添加完成后,内部温度上升至40℃,在此温度下反应2小时。所得聚酰胺酸通过GPC测量具有48,000的重均分子量。由此得到含12.5重量%聚酰胺酸的反应溶液。
(C)将200g 4,4′-二氨基二苯醚加入到3,152g N,N’-二甲基乙酰胺中,其在氮气气氛下搅拌溶解。向此溶液中缓慢加入194g均苯四酸二酐,以使内部温度不超过15℃。添加完成后,反应在15℃下进行2小时,然后在室温下进行6小时。所得聚酰胺酸通过GPC测量具有36,000的重均分子量。由此得到含12.5重量%聚酰胺酸的反应溶液。
作为粘合剂的聚酰胺酸清漆的制备
不加分离而使用上面得到的聚酰胺酸反应溶液(组分A、B和C),称重并混合以使(A+B)/C的重量比为(9+50)/41。具体而言,9g反应溶液(A)、50g反应溶液(B)和41g反应溶液(C)计量加入200-cc烧杯中,在此用玻璃棒充分搅拌20分钟。混合物在300mmHg的减压下保持10分钟以脱气。得到含有12.5重量%混和聚酰胺酸的清漆,并在25℃具有2,600mPa·s的粘度。
层压材料的制备
使用涂布器将上述制备的聚酰胺酸清漆涂敷在30cm×25cm面积的35-μm辊轧铜箔上,达到40μm的湿涂层厚度。涂层在干燥箱中于120℃干燥5分钟。面积为30cm×25cm的25-μm聚酰亚胺薄膜(Kaneka公司的Apical NPI,初始抗张模量420kg/mm2,100-200℃下线膨胀系数约为1.6×10-5/℃)覆盖在清漆涂层上。使用测试辊式层压机(Nishimura Machinery有限公司)在120℃、15kg/cm的压力和4m/min的速率下对材料进行层压。在氮气惰性干燥箱中,层压材料连续地进行热处理,160℃加热4小时,250℃加热1小时,然后350℃加热1小时。所得层压材料包括35μm厚的铜箔和30μm厚的聚酰亚胺层(粘合剂层+聚酰亚胺薄膜)。
层压材料通过如下测试进行检验。
剥离强度
根据JIS C6471,测量其上形成有1m宽的电路图形的样品在50mm/min的牵引速率和180°的剥离角下的剥离强度。
焊料耐热性
样品在360℃浸入在焊锡槽中30秒,然后视觉观察分层或起泡。
卷曲
12cm×12cm的聚酰亚胺薄膜放置在水平平台上。如果薄膜的对边不与平台贴合,测量该分离距离。如果薄膜片非常卷曲并成为翻卷成圆,测量该圆形薄膜的直径并记录于表2。
实施例2-7
除了组分A、B和C以如表1所示的混和比例混和,实施例2-7的操作与实施例1相同。
对比实施例1-3
除了组分A、B和C以如表2所示的混和比例混和,对比实施例1-3的操作与实施例1相同。
对比实施例4
(A)将10.8g间苯二胺加入到321.6g N-甲基-2-吡咯烷酮中,其在氮气气氛下搅拌溶解。向此溶液中缓慢加入29.4g 3,4,3′,4′-联苯基四羧酸二酐,以使内部温度不超过10℃。添加完成后,内部温度上升至40℃,在此温度下反应2小时。所得聚酰胺酸通过GPC测量具有44,000的重均分子量。
(B)将24.3g 2-羟基-4,4′-二氨基苯酰替苯胺加入到452g二甲基乙酰胺中,其在氮气气氛下搅拌溶解。向此溶液中缓慢加入32.2g 3,4,3′,4′-二苯甲酮四羧酸二酐。添加完成后,反应在25℃进行3小时。所得聚酰胺酸通过GPC测量具有24,000的重均分子量。
(C)将19.8g 4,4′-二氨基二苯甲烷加入到392g二甲基乙酰胺中,其在氮气气氛下搅拌溶解。向此溶液中缓慢加入19.4g均苯四酸二酐。添加完成后,反应在25℃进行3小时。所得聚酰胺酸通过GPC测量具有30,000的重均分子量。
上面得到的聚酰胺酸反应溶液(组分A、B和C)称重并混合,以使(A+B)/C的重量比为(9+50)/41。充分混合后,聚酰胺酸混合物在300mmHg的减压下保持10分钟以脱气。得到含有11.5重量%混和聚酰胺酸的清漆,并在25℃具有1,700mPa·s的粘度。
如实施例1所示,使用这种清漆制备层压材料并测试该材料。
表1
实施例 | |||||||
1 | 2 | 3 | 4 | 5 | 6 | 7 | |
A+B,重量% | 9+50 | 4+50 | 42.5+7.5 | 64+11 | 21+4 | 30+25 | 65+5 |
A/B比 | 15/85 | 7/93 | 85/15 | 85.3/14.7 | 84/16 | 54/46 | 94/6 |
C,重量% | 41 | 46 | 50 | 25 | 75 | 45 | 30 |
在混和清漆中的固含量,wt% | 12.5 | 12.5 | 12.5 | 12.5 | 12.5 | 12.5 | 12.5 |
混和清漆的粘度,mPa·s,25℃ | 2,600 | 2,580 | 2,200 | 2,500 | 2,000 | 2,100 | 2,500 |
剥离强度,kg/cm | 1.2 | 0.95 | 1.05 | 1.0 | 1.15 | 1.1 | 1.2 |
焊料耐热性,360℃/30秒 | 完好 | 完好 | 完好 | 完好 | 完好 | 完好 | 完好 |
卷曲,cm | 0.2 | 0.1 | 0.05 | 0 | 0.15 | 0.1 | 0.4 |
表2
对比实施例 | ||||
1 | 2 | 3 | 4 | |
A+B,重量% | 85+15 | 0 | 9.5+0.5 | 9+50 |
A/B比 | 85/15 | 0 | 95/15 | 15/85 |
C,重量% | 0 | 100 | 90 | 41 |
在混和清漆中的固含量,wt% | 12.5 | 12.5 | 12.5 | 11.5 |
混和清漆的粘度,mPa·s,25℃ | 2,700 | 1,800 | 1,900 | 1,700 |
剥离强度,kg/cm | 1.1 | 1.0 | 1.0 | 1.0 |
焊料耐热性,360℃/30秒 | 完好 | 完好 | 完好 | 完好 |
卷曲,cm | 1.5 | 卷曲到2cm直径 | 卷曲到3cm直径 | 卷曲到2cm直径 |
Claims (6)
1.一种柔性金属箔-聚酰亚胺层压材料,其包括金属箔和聚酰亚胺薄膜,两者之间的粘合剂层层叠于薄膜之上,所述粘合剂层通过聚酰胺酸混合物的亚胺化反应得到,该聚酰胺酸混合物包括:
(A)聚酰胺酸,其为3,4,3′,4′-联苯基四羧酸酐与对苯二胺的反应产物,
(B)聚酰胺酸,其为3,4,3′,4′-联苯基四羧酸酐与4,4′-二氨基二苯醚的反应产物,和
(C)聚酰胺酸,其为均苯四酸二酐与4,4′-二氨基二苯醚的反应产物,其中(A+B)/C的重量比为75/25-25/75。
2.权利要求1所述的层压材料,其中所述聚酰胺酸混合物含有A/B重量比为10/90-90/10的聚酰胺酸(A)和(B)。
3.权利要求1所述的层压材料,其中所述金属箔为厚度至少为9μm的铜箔,所述聚酰亚胺薄膜具有至少12μm的厚度,并且所述粘合剂层具有多达10μm的厚度。
4.一种制备柔性金属箔-聚酰亚胺层压材料的方法,包括通过两者之间的粘合剂层将金属箔连接到聚酰亚胺薄膜,所述粘合剂为聚酰胺酸混合物,包括:
(A)聚酰胺酸,其为3,4,3′,4′-联苯基四羧酸酐与对苯二胺的反应产物,
(B)聚酰胺酸,其为3,4,3′,4′-联苯基四羧酸酐与4,4′-二氨基二苯醚的反应产物,和
(C)聚酰胺酸,其为均苯四酸二酐与4,4′-二氨基二苯醚的反应产物,其中(A+B)/C的重量比为75/25-25/75。
5.权利要求4所述的方法,其中所述聚酰胺酸混合物含有A/B重量比为10/90-90/10的聚酰胺酸(A)和(B)。
6.权利要求4所述的方法,其中所述金属箔为厚度至少为9μm的铜箔,所述聚酰亚胺薄膜具有至少12μm的厚度,并且所述粘合剂层具有多达10μm的厚度。
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JP2004039634 | 2004-02-17 | ||
JP2004039634A JP4200376B2 (ja) | 2004-02-17 | 2004-02-17 | フレキシブル金属箔ポリイミド積層板及びその製造方法 |
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US (1) | US20050181223A1 (zh) |
JP (1) | JP4200376B2 (zh) |
KR (1) | KR20060042029A (zh) |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN1958649B (zh) * | 2006-10-26 | 2010-12-01 | 同济大学 | 一种含生色基团的聚酰亚胺薄膜及其制备方法 |
CN110239163A (zh) * | 2019-06-13 | 2019-09-17 | 陈建义 | 一种提高PI膜与Cu箔间粘结性能的柔性印刷电路板基材 |
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JP3952196B2 (ja) * | 2003-06-25 | 2007-08-01 | 信越化学工業株式会社 | フレキシブル金属箔ポリイミド積層板の製造方法 |
WO2005000576A1 (ja) * | 2003-06-25 | 2005-01-06 | Shin-Etsu Chemical Co., Ltd. | フレキシブル金属箔ポリイミド積層板 |
JP2006015681A (ja) * | 2004-07-05 | 2006-01-19 | Shin Etsu Chem Co Ltd | フレキシブル金属箔ポリイミド積層板及びその製造方法 |
JP2006068920A (ja) * | 2004-08-31 | 2006-03-16 | Shin Etsu Chem Co Ltd | フレキシブル銅箔ポリイミド積層板の製造方法 |
JP4766247B2 (ja) * | 2006-01-06 | 2011-09-07 | 信越化学工業株式会社 | フレキシブル金属箔片面ポリイミド積層板の製造方法 |
JP4593509B2 (ja) | 2006-03-31 | 2010-12-08 | 新日鐵化学株式会社 | フレキシブル積層板の製造方法 |
JP2009113475A (ja) * | 2007-10-18 | 2009-05-28 | Shin Etsu Chem Co Ltd | フレキシブル片面ポリイミド銅張積層板の製造方法 |
CN112778563A (zh) * | 2021-01-25 | 2021-05-11 | 深圳和力纳米科技有限公司 | 聚酰亚胺薄膜及其制备方法 |
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-
2004
- 2004-02-17 JP JP2004039634A patent/JP4200376B2/ja not_active Expired - Fee Related
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2005
- 2005-01-28 TW TW94102778A patent/TW200528265A/zh not_active IP Right Cessation
- 2005-02-01 US US11/046,751 patent/US20050181223A1/en not_active Abandoned
- 2005-02-17 KR KR1020050013017A patent/KR20060042029A/ko not_active Application Discontinuation
- 2005-02-17 CN CNA2005100697859A patent/CN1733469A/zh active Pending
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1958649B (zh) * | 2006-10-26 | 2010-12-01 | 同济大学 | 一种含生色基团的聚酰亚胺薄膜及其制备方法 |
CN110239163A (zh) * | 2019-06-13 | 2019-09-17 | 陈建义 | 一种提高PI膜与Cu箔间粘结性能的柔性印刷电路板基材 |
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JP4200376B2 (ja) | 2008-12-24 |
TW200528265A (en) | 2005-09-01 |
KR20060042029A (ko) | 2006-05-12 |
JP2005231051A (ja) | 2005-09-02 |
US20050181223A1 (en) | 2005-08-18 |
TWI331086B (zh) | 2010-10-01 |
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