CN112689454A - Method for manufacturing shielding material - Google Patents
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- CN112689454A CN112689454A CN202011542028.XA CN202011542028A CN112689454A CN 112689454 A CN112689454 A CN 112689454A CN 202011542028 A CN202011542028 A CN 202011542028A CN 112689454 A CN112689454 A CN 112689454A
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- polyamic acid
- shielding material
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- dianhydride
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- 239000000463 material Substances 0.000 title claims abstract description 28
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 title claims abstract description 7
- 229920001721 polyimide Polymers 0.000 claims abstract description 43
- 239000004642 Polyimide Substances 0.000 claims abstract description 41
- 229920005575 poly(amic acid) Polymers 0.000 claims abstract description 37
- 229910052751 metal Inorganic materials 0.000 claims abstract description 28
- 239000002184 metal Substances 0.000 claims abstract description 28
- 239000011888 foil Substances 0.000 claims abstract description 25
- 150000004985 diamines Chemical class 0.000 claims description 23
- 239000002798 polar solvent Substances 0.000 claims description 21
- 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 description 19
- 239000000203 mixture Substances 0.000 claims description 15
- 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 14
- REYJJPSVUYRZGE-UHFFFAOYSA-N Octadecylamine Chemical compound CCCCCCCCCCCCCCCCCCN REYJJPSVUYRZGE-UHFFFAOYSA-N 0.000 claims description 14
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 10
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 10
- 239000011248 coating agent Substances 0.000 claims description 9
- 238000000576 coating method Methods 0.000 claims description 9
- GEYOCULIXLDCMW-UHFFFAOYSA-N 1,2-phenylenediamine Chemical compound NC1=CC=CC=C1N GEYOCULIXLDCMW-UHFFFAOYSA-N 0.000 claims description 8
- VLDPXPPHXDGHEW-UHFFFAOYSA-N 1-chloro-2-dichlorophosphoryloxybenzene Chemical compound ClC1=CC=CC=C1OP(Cl)(Cl)=O VLDPXPPHXDGHEW-UHFFFAOYSA-N 0.000 claims description 8
- 230000009477 glass transition Effects 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 238000002360 preparation method Methods 0.000 claims description 5
- JVERADGGGBYHNP-UHFFFAOYSA-N 5-phenylbenzene-1,2,3,4-tetracarboxylic acid Chemical compound OC(=O)C1=C(C(O)=O)C(C(=O)O)=CC(C=2C=CC=CC=2)=C1C(O)=O JVERADGGGBYHNP-UHFFFAOYSA-N 0.000 claims description 4
- XROLBZOMVNMIFN-UHFFFAOYSA-N 1-(1-benzofuran-4-yl)propan-2-amine Chemical compound CC(N)CC1=CC=CC2=C1C=CO2 XROLBZOMVNMIFN-UHFFFAOYSA-N 0.000 claims description 3
- WUPRYUDHUFLKFL-UHFFFAOYSA-N 4-[3-(4-aminophenoxy)phenoxy]aniline Chemical compound C1=CC(N)=CC=C1OC1=CC=CC(OC=2C=CC(N)=CC=2)=C1 WUPRYUDHUFLKFL-UHFFFAOYSA-N 0.000 claims description 3
- 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 claims description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 3
- 239000000956 alloy Substances 0.000 claims description 3
- 229910045601 alloy Inorganic materials 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
- 239000010949 copper Substances 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 239000003086 colorant Substances 0.000 abstract description 2
- 239000010410 layer Substances 0.000 description 41
- 230000007774 longterm Effects 0.000 description 6
- 239000002131 composite material Substances 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 239000002344 surface layer Substances 0.000 description 3
- 230000005855 radiation Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000005670 electromagnetic radiation Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
Abstract
The invention discloses a method for manufacturing a shielding material, which is structurally characterized in that a polyamic acid solution A is coated on one surface of a metal foil, then imidization is carried out, so that a first polyimide layer A is obtained, a polyamic acid solution B is coated on the other surface of the metal foil, and then imidization is carried out, so that a second polyimide layer B is obtained. The shielding material obtained by the invention has the characteristics of insulativity, shielding resistance, high temperature resistance, lightness and thinness, and can be made into materials with different colors and different functions.
Description
Technical Field
The invention relates to a polyimide film, in particular to a method for manufacturing a shielding material.
Background
Polyimide films are increasingly used in the electrical industry due to their excellent low temperature resistance (cold resistance), high temperature resistance, and dielectric insulation, especially in the fields of electromagnetic radiation such as electronic computers, communication satellites, high voltage power transmission networks, and some medical devices. However, the existing polyimide with the electromagnetic shielding function generally has the problems of uneven filler dispersion, serious agglomeration and easy falling, so that the electrical conductivity and magnetism of the composite film are poor, the mechanical property of the composite film is influenced, and the further development and application of the composite film in the electronic field are limited.
Disclosure of Invention
The present invention is directed to a method for manufacturing a shielding material to solve the above-mentioned disadvantages of the prior art.
In order to achieve the above object, the present invention provides a method for manufacturing a shielding material, comprising the steps of:
firstly, putting diamine into a reaction kettle, dissolving the diamine with a polar solvent, adding dianhydride with an equal molar ratio (molar ratio: 1:1) into the reaction kettle in batches, and stirring to prepare the needed polyamic acid solution A, wherein the polar solvent accounts for 70-90% by mass;
and step two, taking a metal foil with the thickness of 6-100 microns, coating a layer of polyamic acid solution A on the metal foil, putting the metal foil into a first tunnel furnace for baking and curing, wherein the gradient temperature is 80 ℃/1-10min, 120 ℃/1-10min, 160 ℃/1-10min, 200 ℃/1-10min, 250 ℃/1-10min and 320 ℃/1-10min, complete imidization of the polyamic acid is completed, and a first polyimide layer A with the thickness of 5-25 microns is formed, and the first polyimide layer A resists high temperature for 60 seconds and has the temperature of 500 ℃. The glass transition temperature of the imidized material of the polyamic acid solution A is 280-320 ℃.
The metal foil is one of aluminum, alloy or copper.
The diamine in the preparation of the polyamic acid solution A is one or more of octadecyl amine (ODA), 4-diaminodiphenylmethane (MDA) and phenylenediamine (PPD);
the dianhydride is one or more of pyromellitic dianhydride (PMDA), biphenyl tetracarboxylic dianhydride (BPDA), 3',4,4' -Benzophenone Tetracarboxylic Dianhydride (BTDA) and 4,4' -oxydiphthalic anhydride (ODPA).
The polar solvent is one or more of Dimethylacetamide (DMAC) and N-methylpyrrolidone (NMP).
The invention also discloses a manufacturing method of the shielding material, which comprises the following steps:
firstly, putting diamine into a reaction kettle, dissolving the diamine with a polar solvent, adding dianhydride with an equal molar ratio (molar ratio: 1:1) into the reaction kettle in batches, and stirring to prepare the needed polyamic acid solution A, wherein the polar solvent accounts for 70-90% by mass; the glass transition temperature of the imidized material of the polyamic acid solution A is 280-320 ℃.
Step two, taking a metal foil with the thickness of 6-100 microns, coating a layer of polyamic acid solution A on the metal foil, putting the metal foil into a first tunnel furnace for baking and curing, wherein the gradient temperature is 80 ℃/1-10min, 120 ℃/1-10min, 160 ℃/1-10min, 200 ℃/1-10min, 250 ℃/1-10min and 320 ℃/1-10min, complete imidization of polyamic acid is completed, and a first polyimide layer A with the thickness of 5-25 microns is formed, and the first polyimide layer A resists high temperature for 60 seconds and has the temperature of 500 ℃;
putting a diamine mixture into a reaction kettle, dissolving the diamine mixture by using a polar solvent, adding a dianhydride mixture into the reaction kettle in batches at an equal molar ratio, and stirring to prepare a needed polyamic acid solution B, wherein the diamine mixture consists of 1, 3-bis (4-aminophenoxy) benzene (1, 3, 4-APB) and Octadecylamine (ODA) at a molar ratio of 7:3, the dianhydride mixture consists of 3,3',4,4' -benzophenonetetracarboxylic dianhydride (BTDA) and 4,4' -oxydiphthalic anhydride (ODPA) at a molar ratio of 2:8, and the polar solvent accounts for 70-90% by mass; and finally, coating a layer of polyamic acid solution B on the other surface of the metal foil, then, integrally entering a second tunnel furnace for baking and curing, wherein the gradient temperature is 80 ℃/1-10min, 120 ℃/1-10min, 160 ℃/1-10min, 200 ℃/1-10min and 220 ℃/1-10min, the thorough imidization of the polyamic acid is completed, a second polyimide layer B with the thickness of 5-10 microns is formed, and the second polyimide layer B resists high temperature for 60 seconds and has the temperature of 360 ℃. The glass transition temperature of the second polyimide layer B is 180 to 220 ℃. The polar solvent is one or more of Dimethylacetamide (DMAC) and N-methylpyrrolidone (NMP).
The shielding material is structurally characterized in that a polyamic acid solution A is coated on one surface of a metal foil, and then imidization is carried out, so that a first polyimide layer A is obtained, wherein the first polyimide layer A can resist high temperature for 60 seconds, the temperature is 500 ℃, and the whole long-term temperature resistance is over 260 ℃.
The other shielding material obtained by the invention has the structure that one side of a metal foil is coated with a polyamic acid solution A, and then imidization is carried out, so that a first polyimide layer A is obtained, wherein the first polyimide layer A can resist high temperature for 60 seconds, the temperature is 500 ℃, and the whole long-term temperature resistance is more than 260 ℃. And then coating a polyamic acid solution B on the other surface, and imidizing to obtain a second polyimide layer B, wherein the second polyimide layer B resists high temperature for 60 seconds, the temperature is 360 ℃, and the overall long-term temperature resistance is over 160 ℃.
The two shielding materials have the characteristics of insulativity, shielding resistance, high temperature resistance, thinness, secondary adhesion with PI and metal surface layers, and can be made into materials with different colors and different functions. The specific performance indexes are as follows:
1. insulating property: the polyimide of the first polyimide layer A and the polyimide of the second polyimide layer B have the capacity of resisting more than 1000 volts, and the thicker the film layer is, the higher the voltage resistance is, the better the insulativity is;
2. shielding prevention: the thickness of the metal foil is 6-100 microns, the shielding performance is mainly realized through the metal foil, and the lowest shielding efficiency reaches more than 85dB (10 Mhz-3 Ghz);
3. high temperature resistance: the first polyimide layer A can resist high temperature for 60 seconds, 500 ℃ and over 260 ℃ for a long time, and has the characteristics of high insulation, chemical stability, radiation resistance, self-extinguishing and the like; the second polyimide layer B can resist high temperature for 60 seconds, the temperature is 360 ℃, the whole long-term temperature resistance is above 160 ℃, and meanwhile, the second polyimide layer B can be bonded with the PI and metal surface layers again at 320 ℃ under certain pressure;
4. light and thin: the overall thickness is 20-110 microns.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1:
the manufacturing method of the shielding material provided by the embodiment comprises the following steps:
firstly, putting diamine into a reaction kettle, dissolving the diamine with a polar solvent, adding dianhydride with an equal molar ratio (molar ratio: 1:1) into the reaction kettle in batches, and stirring to prepare the needed polyamic acid solution A, wherein the polar solvent accounts for 70-90% by mass; the glass transition temperature of the imidized material of the polyamic acid solution A is 280-320 ℃.
And step two, taking a metal foil with the thickness of 6-100 microns, coating a layer of polyamic acid solution A on one side of the metal foil, baking and curing the whole in a first tunnel furnace, wherein the gradient temperature is 80 ℃/1-10min, 120 ℃/1-10min, 160 ℃/1-10min, 200 ℃/1-10min, 250 ℃/1-10min and 320 ℃/1-10min, and complete imidization of the polyamic acid is completed to form a first polyimide layer A with the thickness of 5-25 microns, and the first polyimide layer A can resist high temperature for 60 seconds and has the temperature of 500 ℃.
The metal foil is one of aluminum, alloy or copper.
The diamine in the preparation of the polyamic acid solution A is one or more of octadecyl amine (ODA), 4-diaminodiphenylmethane (MDA) and phenylenediamine (PPD);
the dianhydride is one or more of pyromellitic dianhydride (PMDA), biphenyl tetracarboxylic dianhydride (BPDA), 3',4,4' -Benzophenone Tetracarboxylic Dianhydride (BTDA) and 4,4' -oxydiphthalic anhydride (ODPA).
The polar solvent is one or more of Dimethylacetamide (DMAC) and N-methylpyrrolidone (NMP).
Through tests, the first polyimide layer A can resist high temperature for 60 seconds, the temperature is 500 ℃, and the whole long-term temperature resistance is over 260 ℃; the first polyimide layer A has the capacity of resisting more than 1000 volts, and the thicker the film layer is, the higher the voltage resistance is, the better the insulativity is; and the minimum shielding effectiveness reaches more than 85 dB.
Example 2:
the manufacturing method of the shielding material provided by the embodiment comprises the following steps:
firstly, putting diamine into a reaction kettle, dissolving the diamine with a polar solvent, adding dianhydride with an equal molar ratio into the reaction kettle in batches, and stirring to prepare the needed polyamic acid solution A, wherein the polar solvent accounts for 70-90% by mass; the glass transition temperature of the imidized material of the polyamic acid solution A is 280-320 ℃.
Step two, taking a metal foil with the thickness of 6-100 microns, coating a layer of polyamic acid solution A on the metal foil, putting the metal foil into a first tunnel furnace for baking and curing, wherein the gradient temperature is 80 ℃/1-10min, 120 ℃/1-10min, 160 ℃/1-10min, 200 ℃/1-10min, 250 ℃/1-10min and 320 ℃/1-10 min), and the polyamic acid is completely imidized to form a first polyimide layer A with the thickness of 5-25 microns, wherein the first polyimide layer A can resist high temperature for 60 seconds and has the temperature of 500 ℃;
putting a diamine mixture into a reaction kettle, dissolving the diamine mixture by using a polar solvent, adding a dianhydride mixture into the reaction kettle in batches at an equal molar ratio, and stirring to prepare a needed polyamic acid solution B, wherein the diamine mixture consists of 1, 3-bis (4-aminophenoxy) benzene (1, 3, 4-APB) and Octadecylamine (ODA) at a molar ratio of 7:3, the dianhydride mixture consists of 3,3',4,4' -benzophenonetetracarboxylic dianhydride (BTDA) and 4,4' -oxydiphthalic anhydride (ODPA) at a molar ratio of 2:8, and the polar solvent accounts for 70-90% by mass; and finally, coating a layer of polyamic acid solution B on the other surface of the metal foil, then, integrally entering a second tunnel furnace for baking and curing, wherein the gradient temperature is 80 ℃/1-10min, 120 ℃/1-10min, 160 ℃/1-10min, 200 ℃/1-10min and 220 ℃/1-10 min), the thorough imidization of the polyamic acid is completed, and a second polyimide layer B with the thickness of 5-10 microns is formed, and the second polyimide layer B resists high temperature for 60 seconds and has the temperature of 360 ℃. The glass transition temperature of the second polyimide layer B is 180 to 220 ℃.
The diamine in the preparation of the polyamic acid solution A is one or more of octadecyl amine (ODA), 4-diaminodiphenylmethane (MDA) and phenylenediamine (PPD); the dianhydride is one or more of pyromellitic dianhydride (PMDA), biphenyl tetracarboxylic dianhydride (BPDA), 3',4,4' -Benzophenone Tetracarboxylic Dianhydride (BTDA) and 4,4' -oxydiphthalic anhydride (ODPA).
The polar solvent is one or more of Dimethylacetamide (DMAC) and N-methylpyrrolidone (NMP).
Tests show that the first polyimide layer can resist high temperature for 60 seconds, 500 ℃ and over 260 ℃ for a long time, and has the characteristics of high insulation, chemical stability, radiation resistance, self-extinguishing and the like; the second polyimide layer can resist high temperature for 60 seconds, the temperature is 360 ℃, the whole long-term temperature resistance is above 160 ℃, and meanwhile, the second polyimide layer can be bonded with the PI and metal surface layers again at 320 ℃ under certain pressure. The first polyimide layer and the second polyimide layer both have the capacity of resisting more than 1000 volts, and the thicker the film layer is, the higher the voltage resistance is, the better the insulativity is; and the minimum shielding effectiveness reaches more than 85 dB.
Claims (9)
1. A method of manufacturing a shielding material, comprising: the method comprises the following steps:
firstly, putting diamine into a reaction kettle, dissolving the diamine with a polar solvent, adding dianhydride with an equal molar ratio into the reaction kettle in batches, and stirring to prepare the needed polyamic acid solution A, wherein the polar solvent accounts for 70-90% by mass;
and secondly, taking a metal foil with the thickness of 6-100 microns, coating a layer of polyamic acid solution A on one side of the metal foil, and then putting the whole into a first tunnel furnace for baking and curing to complete imidization of the polyamic acid to form a first polyimide layer A with the thickness of 5-25 microns.
2. The method of manufacturing a shielding material of claim 1, wherein: the metal foil is one of aluminum, alloy or copper.
3. The method of manufacturing a shielding material of claim 1, wherein: the diamine in the preparation of the polyamic acid solution A is one or more of octadecyl amine (ODA), 4-diaminodiphenylmethane (MDA) and phenylenediamine (PPD); the dianhydride is one or more of pyromellitic dianhydride (PMDA), biphenyl tetracarboxylic dianhydride (BPDA), 3',4,4' -Benzophenone Tetracarboxylic Dianhydride (BTDA) and 4,4' -oxydiphthalic anhydride (ODPA).
4. The method of manufacturing a shielding material of claim 1, wherein: the preparation method comprises the third step of putting a diamine mixture into a reaction kettle, dissolving the diamine mixture by using a polar solvent, adding a dianhydride mixture into the reaction kettle in batches at an equal molar ratio, and stirring to prepare the needed polyamic acid solution B, wherein the diamine mixture consists of 1, 3-bis (4-aminophenoxy) benzene (1, 3, 4-APB) and Octadecylamine (ODA) at a molar ratio of 7:3, the dianhydride mixture consists of 3,3',4,4' -Benzophenone Tetracarboxylic Dianhydride (BTDA) and 4,4' -oxydiphthalic anhydride (ODPA) at a molar ratio of 2:8, and the polar solvent accounts for 70-90% by mass; and finally, coating a layer of polyamic acid solution B on the other surface of the metal foil, and then putting the whole into a second tunnel furnace for baking and curing to complete imidization of polyamic acid to form a second polyimide layer B with the thickness of 5-10 microns.
5. The method of manufacturing a shielding material according to claim 1 or 4, wherein: the polar solvent is one or more of Dimethylacetamide (DMAC) and N-methylpyrrolidone (NMP).
6. The method of manufacturing a shielding material of claim 1, wherein: the first polyimide layer a has a glass transition temperature of 280 to 320 ℃.
7. The method of manufacturing a shielding material of claim 1, wherein: the echelon temperature of the first tunnel furnace is 80 ℃/1-10min, 120 ℃/1-10min, 160 ℃/1-10min, 200 ℃/1-10min, 250 ℃/1-10min and 320 ℃/1-10 min.
8. The method of manufacturing a shielding material according to claim 4, wherein: the second polyimide layer B has a glass transition temperature of 180 to 220 ℃.
9. The method of manufacturing a shielding material according to claim 4, wherein: the temperature of the second tunnel furnace is 80 ℃/1-10min, 120 ℃/1-10min, 160 ℃/1-10min, 200 ℃/1-10min and 220 ℃/1-10 min.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114369361A (en) * | 2021-12-31 | 2022-04-19 | 广州惠利电子材料有限公司 | Insulating PI membrane material |
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CN1599538A (en) * | 2003-05-06 | 2005-03-23 | 三菱瓦斯化学株式会社 | Metal plated laminate |
CN1786052A (en) * | 2004-12-07 | 2006-06-14 | 长春人造树脂厂股份有限公司 | Preparation method of polyimide |
WO2011049357A2 (en) * | 2009-10-20 | 2011-04-28 | 주식회사 두산 | Polyamic acid solution, polyimide resin, and flexible copper clad laminate using same |
CN102459466A (en) * | 2009-04-03 | 2012-05-16 | 株式会社斗山 | Polyamic acid solution, polyimide resin and a soft metal-foil laminate employing the same |
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2020
- 2020-12-23 CN CN202011542028.XA patent/CN112689454A/en active Pending
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
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JPH03291986A (en) * | 1990-04-09 | 1991-12-24 | Sumitomo Bakelite Co Ltd | Manufacture of board for flexible printed circuit with cover coating |
CN1599538A (en) * | 2003-05-06 | 2005-03-23 | 三菱瓦斯化学株式会社 | Metal plated laminate |
CN1786052A (en) * | 2004-12-07 | 2006-06-14 | 长春人造树脂厂股份有限公司 | Preparation method of polyimide |
CN102459466A (en) * | 2009-04-03 | 2012-05-16 | 株式会社斗山 | Polyamic acid solution, polyimide resin and a soft metal-foil laminate employing the same |
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CN114369361A (en) * | 2021-12-31 | 2022-04-19 | 广州惠利电子材料有限公司 | Insulating PI membrane material |
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Application publication date: 20210420 |