CN101746103A - Method for preparing laminated polyimide metal foil - Google Patents
Method for preparing laminated polyimide metal foil Download PDFInfo
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- CN101746103A CN101746103A CN200810218376A CN200810218376A CN101746103A CN 101746103 A CN101746103 A CN 101746103A CN 200810218376 A CN200810218376 A CN 200810218376A CN 200810218376 A CN200810218376 A CN 200810218376A CN 101746103 A CN101746103 A CN 101746103A
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- kapton
- acid
- metal foil
- metal forming
- hot pressing
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Abstract
The invention provides a method for preparing laminated polyimide metal foil, comprising the following steps: (a) modifying the surface of a polyimide film so that polyamic acid being formed on the surface of the polyimide film and (b) hot pressing metal foil and the polyimide film whose surface is modified and modifying the polyimide film which is hot pressed together with the metal foil with imide to obtain the laminated polyimide metal foil. The method for preparing the laminated polyimide metal foil is simple, and the metal foil can be well adhered to the polyimide film.
Description
[technical field]
The present invention relates to preparing laminated polyimide metal foil, no glue preparing laminated polyimide metal foil particularly simple in structure, that the interlayer adhesion is good.
[background technology]
In recent years, be accompanied by lightweight, miniaturization, the densification of electronic product, the needs of various printed base plates are increased, wherein particularly growing to the needs of the flexible printed circuit substrate of in restriceted envelope, fixing a large amount of circuit.
At present in flexible print circuit (FPC) base material of producing, the modal adhesive that is to use has three layers of product of glue type with what Kapton and metal forming bonding were laminated with, and adhesive generally adopts TPI described in the prior art at present.But, make technology very complicated owing to adopted TPI.
Along with the fast development of electronics industry, the outward appearance and the performance of electronic product also to be had higher requirement, it is first-selected that short, little, light, thin, beautiful and other excellent properties also become.And FPC industry is in order to satisfy this requirement, begin also to occur that thickness is thinner, the two-layer product of the better gum-free of performance, for example polyimide resin is dissolved in and forms polyimide solution in the solvent, again polyimide solution is coated on the metal forming, heating removes to desolvate and carries out imidizate then, can obtain gum-free polyimide metal foil lamilated body.But because the composition that dissolves in solvent of Thermocurable polyimide film seldom, so adopt the adhesive force of gum-free lamilated body Kapton that this method obtains at last and metal forming relatively poor, metal forming easily comes off.
[summary of the invention]
The present invention is directed to defectives such as the above-mentioned complex process that exists in the prior art, poor adhesive force, proposed a kind of preparing laminated polyimide metal foil, comprise following steps:
(a) the Kapton surface modification makes the Kapton surface form polyamic acid;
(b) Kapton after the surface modification and metal forming hot pressing, to metal forming hot pressing after Kapton carry out imidizate and handle, obtain the polyimide metal foil lamilated body.
Preparing laminated polyimide metal foil provided by the present invention need not adopt adhesive between Kapton and the metal forming, and technology is simple; In addition, by Kapton is carried out surface modification, make that the adhesive force of metal forming and Kapton is very good.
[specific embodiment]
The invention provides a kind of preparing laminated polyimide metal foil, comprise following steps:
(a) the Kapton surface modification makes the Kapton surface form polyamic acid;
(b) Kapton after the surface modification and metal forming hot pressing, to metal forming hot pressing after Kapton carry out imidizate and handle, obtain the polyimide metal foil lamilated body.
The material of Kapton of the present invention is not particularly limited, and preferably adopts the Thermocurable polyimide film.Described Thermocurable polyimide is the condensation polymer that is reacted in polar solvent and obtained by acid dianhydride, diamines.Wherein, the molar ratio of described acid dianhydride and diamines is preferably 0.95～1.05: 1, more preferably 0.985～1: 1.
Described acid dianhydride is the various acid dianhydrides that those skilled in the art use always, preferably comprises the acid dianhydride shown in the following general formula (1).In the general formula (1), A is the group shown in following general formula (2) or (3).
In the preference of the acid dianhydride shown in the general formula (1), comprise pyromellitic acid dianhydride and biphenyl tetracarboxylic dianhydride etc.
The various diamines that described diamines is used always for those skilled in the art, the present invention does not have specific (special) requirements, for example can be selected from 3,3 '-DADPS, 3,4 '-DADPS, 4,4 '-DADPS, 3,3 '-diaminourea benzophenone, 3,4 '-diaminourea benzophenone, 4,4 '-diaminourea benzophenone, 3,3 '-MDA, 3,4 '-MDA, 4,4 '-MDA, 1, two (4-amino-benzene oxygen) benzene, 1 of 3-, two (4-amino-benzene oxygen) benzene of 4-.
The various polar solvents that described polar solvent is used always for those skilled in the art for example can be N-methyl pyrrolidone, dimethyl formamide, dimethylacetylamide, methyl-sulfoxide, oxolane.Kapton of the present invention also can adopt and be purchased product, for example Apical and Kapton.
The thickness of Kapton of the present invention is not particularly limited, can be according to suitably selected preferred 12-25 micron by the purposes of the polyimide metal foil lamilated body of its manufacturing.
According to method provided by the present invention, adopt the mode of various surface modifications commonly used to make the Kapton surface form polyamic acid to Kapton.The preferred elder generation that adopts makes at least a portion generation hydrolysis of the imide of film surface by the etching Kapton among the present invention, makes film surface form polyamic acid by ion-exchange again.Among the present invention, the surface modification of Kapton does not preferably change the thickness of this Kapton, does not change thickness and is meant the variation that does not take place more than 1 micron.The face of described etched Kapton can be a face or two faces of film.
Described etched mode is conventionally known to one of skill in the art, for example can adopt alkali treatment or plasma treatment.Preferred employing alkali treatment among the present invention.
Described alkali treatment is carried out alkali treatment for adopting alkaline solution to Kapton, for example can also can carry out the alkaline solution spraying by modes such as injection or sprays to this Kapton for Kapton is soaked in the alkaline solution.Described alkaline solution is the known various alkaline solutions of art technology, for example can be the aqueous solution of IA family or IIA family element hydrogen oxide.Preferred NaOH or the KOH solution of adopting among the present invention.
The alkali treatment condition is not particularly limited, but the thickness of long time treatment Kapton meeting attenuation under excessive temperature, the condition of described alkali treatment is under the preferable case: the concentration of alkaline solution is 0.1～5mol/L, is preferably 0.5～2mol/L; The temperature of alkaline solution is 10～90 ℃, is preferably 20～80 ℃; The time of alkali treatment is 5～50 minutes, is preferably 15～35 minutes.
Described ion-exchange is technology known in those skilled in the art, and the Kapton after promptly adopting aqueous acid to etching carries out acid treatment.Formed one deck imide salts through the Kapton surface after the etching; In the ion exchange process, the imide salts and the aqueous acid on Kapton surface react, and metal ion is made the Kapton surface generate polyamic acid by the hydrogen ion exchange.
The various acid that the acid that described acid treatment is adopted is used always for those skilled in the art for example can be selected from sulfuric acid, formic acid, hydrochloric acid, propionic acid or the nitric acid one or more.Because the imide salts that the Kapton surface forms after the etching is very thin, so the concentration of described acid should not be too high during acid treatment.Under the preferable case, be benchmark with described aqueous acid, the percent by volume of described acid is 0.1～10%.More preferably under the situation, the temperature of described acid is 10～50 ℃, and the acid treatment time is 1～60 minute.
According to method provided by the present invention, with the Kapton after the surface modification and metal forming hot pressing and the Kapton after the hot pressing is carried out imidizate handle, can obtain the polyimide metal foil lamilated body.
The various metals that the metal of described formation metal forming is used always for those skilled in the art, the present invention is not particularly limited, and for example can be selected from copper, zinc, chromium, nickel, aluminium, stainless steel, iron, gold, silver, titanium and/or its alloy.Because the polyimide metal foil lamilated body is applied to printed circuit board (PCB), metal forming forms electronic circuit at last, the therefore preferred high metal of conductance, for example Copper Foil of adopting.The thickness of described metal forming preferably adopts the 9-36 micron without limits, more preferably the 12-18 micron.
In order to improve cohesive force, can also carry out roughening to the surface of metal forming handles, for example can perhaps implement chemistry or mechanical surface roughening processing to metal forming to metal foil surface nickel plating, copper facing-kirsite with aluminum alcoholate, aluminium chelate compound, silane coupler, triazine thiol class, benzotriazole, acetylene series alcohols, levulinic ketone, pyrocatechol, adjacent benzoquinones class, tannin class, hydroxyquinoline class etc.
About without limits, for example can be lamination methods with the method for Kapton and metal forming hot pressing.The method of described lamination methods for sandwiching Kapton and metal forming and fit between roller and roller is so lamination methods can be described as roll-in again.To the material of described roller without limits, for example can be metallic roll or rubber rollers.Wherein, described metallic roll can be used steel material or stainless steel material, the preferred roller that adopts the surface to carry out processing such as chromium plating; Described rubber rollers preferably adopts the surface to have stable on heating silicon rubber, fluorubber.The temperature of described hot pressing is preferably 150～300 ℃.Mode of heating also can utilize radiation heating mode, induction heating mode etc. except the conduction mode of heating.Applied pressure has no particular limits during described hot pressing, and preferred line pressure is 30～100kg/cm.To being not particularly limited pressing time.
According to method provided by the present invention, the Kapton after the hot pressing is continued heating, make the polyamic acid generation imidizate (claiming hot imidization again) of film surface, can obtain the polyimide metal foil lamilated body.Heating furnace or autoclave that heater can adopt those skilled in the art to use always.In order to prevent that metal forming from oxidation taking place when the high temperature acid imide, described imidizate is handled and is carried out under inert gas atmosphere under the preferable case, for example carries out imidizate in nitrogen atmosphere.Heating means can adopt the method for continuous heating film or be positioned in the heating furnace in that film is twisted on the mandrel.The various mode of heatings that mode of heating is used always for those skilled in the art for example can be the mode of heating of conduction heating, radiation heating or both and usefulness.Under the preferable case, the temperature of described imidizate is 200～500 ℃, and the time of imidizate is 0.5～5 hour.
Adopt the polyimide metal foil lamilated body of method preparation provided by the invention, the adaptation excellence of metal forming and Kapton, the peel strength height of metal forming.Therefore, the polyimide metal foil lamilated body of the present invention's preparation is suitable to the circuit material substrate.
The present invention is further illustrated below by embodiment.The raw material that is adopted in the embodiment of the invention all is available commercially.
Embodiment 1
Kapton (Kapton) is immersed in the NaOH solution of 1mol/L, the temperature of NaOH solution is 50 ℃, and soak time is 20 minutes.Use washed with de-ionized water after the taking-up.Be immersed in percent by volume then and be in 5% the dilute hydrochloric acid solution, soaking temperature is 30 ℃, and soak time is 30 minutes.Use washed with de-ionized water after the taking-up.The Copper Foil of 12 micron thickness is immersed in the 3-sulfydryl propyl trimethoxy silicane of 5 quality %, and soak time is 5 minutes, takes out to use washed with de-ionized water, and drying obtains the Copper Foil of surface roughening.To fit through the Kapton and the above-mentioned Copper Foil that obtains of surface modification then, (Nishimura Machinery Co. Ltd.) carries out pressing to it, and pressing-in temp is 250 ℃, and pressure is 50kg/cm to adopt test roll-type laminator.Put into heating furnace after the pressing, carry out imidizate under the nitrogen atmosphere, adopt trapezoidal continuous intensification during imidizate: 300 ℃ are incubated 30 minutes down, and 350 ℃ are incubated 1 hour down.
By said method, the polyimide metal foil lamilated body that makes is designated as A1.
Embodiment 2
Kapton (Kapton) is immersed in the NaOH solution of 0.5mol/L, the temperature of NaOH solution is 80 ℃, and soak time is 50 minutes.Use washed with de-ionized water after the taking-up.Be immersed in percent by volume then and be in 0.1% the dilute nitric acid solution, soaking temperature is 50 ℃, and soak time is 60 minutes.The taking-up washed with de-ionized water.To directly fit through the Copper Foil behind the Kapton of surface modification and 12 microns, (Nishimura Machinery Co. Ltd.) carries out pressing to it, and pressing-in temp is 230 ℃, and pressure is 70kg/cm to adopt test roll-type laminator then.Put into heating furnace after the pressing, carry out imidizate under the nitrogen atmosphere, adopt trapezoidal continuous intensification during imidizate: 300 ℃ are incubated 30 minutes, and 350 degree are incubated 1 hour down.By said method, the polyimide metal foil lamilated body that makes is designated as A2.
Embodiment 3
Kapton (Kapton) is immersed in the NaOH solution of 2mol/L, the temperature of NaOH solution is 20 ℃, and soak time is 10 minutes.Use washed with de-ionized water after the taking-up.Be immersed in percent by volume then and be in 10% the dilute hydrochloric acid solution, soaking temperature is 15 ℃, and soak time is 10 minutes.The taking-up washed with de-ionized water.The Copper Foil of 12 micron thickness is immersed in N-phenyl-3-TSL 8330 of 1 quality %, and soak time is 5 minutes, takes out to use washed with de-ionized water, and drying obtains the Copper Foil of surface roughening.To fit through the Kapton and the above-mentioned Copper Foil that obtains of surface modification then, (Nishimura Machinery Co. Ltd.) carries out pressing to it, and pressing-in temp is 200 ℃, and pressure is 100kg/cm to adopt test roll-type laminator.Twist in after the pressing on the mandrel, put into heating furnace then, carry out imidizate, 300 ℃ are incubated 30 minutes, and 350 degree are incubated 1 hour down.
By said method, the polyimide metal foil lamilated body that makes is designated as A3.
Embodiment 4
Kapton (Kapton) is immersed in the NaOH solution of 3mol/L, the temperature of NaOH solution is 85 ℃, and soak time is 10 minutes.Use washed with de-ionized water after the taking-up.Be immersed in percent by volume then and be in 10% the dilute hydrochloric acid solution, soaking temperature is 15 ℃, and soak time is 10 minutes.The taking-up washed with de-ionized water.The aluminium foil of 15 micron thickness is immersed in N-phenyl-3-TSL 8330 of 3 quality %, and soak time is 10 minutes, takes out to use washed with de-ionized water, and drying obtains the Copper Foil of surface roughening.To fit through the Kapton and the above-mentioned Copper Foil that obtains of surface modification then, (Nishimura Machinery Co. Ltd.) carries out pressing to it, and pressing-in temp is 150 ℃, and pressure is 100kg/cm to adopt test roll-type laminator.Twist in after the pressing on the mandrel, put into heating furnace then, carry out imidizate, 300 ℃ are incubated 30 minutes, and 350 degree are incubated 1 hour down.
By said method, the polyimide metal foil lamilated body that makes is designated as A4.
Comparative Examples 1
Adopt pyromellitic acid anhydride and 4,4 '-diaminodiphenyl ether makes polyamic acid solution in DMAc, this polyamic acid solution is coated on the Copper Foil again, and heating removes to desolvate carries out imidizate.The polyimide metal foil lamilated body that makes is designated as D1.
Comparative Examples 2
Adopt the method identical with embodiment 1 to prepare the polyimide metal foil lamilated body, difference is: apply the thick TPI binding agent of one deck 1um on the Kapton surface, and do not carry out surface modification.Then with Copper Foil pressing, imidizate.The polyimide metal foil lamilated body that makes is designated as D2.
Performance test:
Adopt Copper Foil peel strength tester (YX-BL, Dongguan City Chang'an AsiaSat precision instrument Co., Ltd) manufactures and designs by 2.4.8 in the IPC-TM-650 test methods manual and 2.4.9, be equipped with Japanese digital pull and push dynamometer table, measure the peel strength of embodiment and comparative example A1～A4 and D1～D2 metal forming.Its test condition: peeling rate is 10-100mm/min; Peel angle is 90 °; Operating voltage is 220VAC, 50HZ; Test result is as shown in table 1 below.
Table 1 peel strength test result
| Sample | Polyimides thickness (μ m) | Metal foil thickness (μ m) | Peel strength (N/cm) |
| ??A1 | ??12.5 | ??12 | ??7.6 |
| ??A2 | ??12.5 | ??12 | ??7.2 |
| ??A3 | ??12.5 | ??12 | ??7.0 |
| ??A4 | ??12.5 | ??15 | ??6.9 |
| ??D1 | ??12.5 | ??12 | ??6.8 |
| ??D2 | ??12.5 | ??12 | ??5.0 |
As can be seen from Table 1, the polyimide metal foil lamilated body that adopts method provided by the invention to make, the adaptation of metal forming and Kapton is very excellent, and the peel strength of metal forming is very high, and the adhesive force of metal forming and Kapton is very good.
From the result of A1～A4 and D1 more as can be seen, the polyimide metal foil lamilated body that adopts preparation method provided by the present invention to obtain, the peel strength of its metal forming can reach the peel strength requirement of the two-layer resultant metal paper tinsel of gum-free that the method for direct employing polyamic acid hydrostomia on metal forming at present commonly used obtain, even higher.In addition, adopt preparation method provided by the invention, can form dual platen in the two sides of Kapton pressing metal forming simultaneously, and adopt the hydrostomia method of prior art once can only form single sided board,, then need repetitive operation, complex process if will form dual platen.
Claims (11)
1. preparing laminated polyimide metal foil comprises following steps:
(a) the Kapton surface modification makes the Kapton surface form polyamic acid;
(b) Kapton after the surface modification and metal forming hot pressing, to metal forming hot pressing after Kapton carry out imidizate and handle, obtain the polyimide metal foil lamilated body.
2. method according to claim 1 is characterized in that: the mode of described surface modification is first etching, ion-exchange makes the Kapton surface form polyamic acid again.
3. method according to claim 2 is characterized in that: described being etched to carried out alkali treatment to Kapton.
4. method according to claim 3 is characterized in that: described alkali treatment is carried out alkali treatment for adopting alkaline solution to Kapton, and described alkaline solution is the aqueous solution of NaOH or KOH.
5. method according to claim 4 is characterized in that: the concentration of described alkaline solution is 0.1～5mol/L, and temperature is 10～90 ℃; The time of described alkali treatment is 5～50 minutes.
6. method according to claim 2 is characterized in that: described ion-exchange is carried out acid treatment for adopting aqueous acid to Kapton.
7. method according to claim 6 is characterized in that: the acid that described acid treatment is adopted is one or more in sulfuric acid, formic acid, hydrochloric acid, propionic acid or the nitric acid; Described aqueous acid is a benchmark, and the percent by volume of described acid is 0.1～10%.
8. method according to claim 1 is characterized in that, the condition of described hot pressing is: temperature is 150～300 ℃, and pressure is 30-100kg/cm.
9. method according to claim 1 is characterized in that, the condition of described imidizate is: temperature is 200～500 ℃, and the time is 0.5～5 hour.
10. method according to claim 1 is characterized in that: the metal of described formation metal forming is copper, zinc, chromium, nickel, aluminium, stainless steel, iron, gold, silver, titanium and/or its alloy.
11. method according to claim 1 is characterized in that: before also being included in Kapton and metal forming hot pressing metal forming is carried out the surface roughening processing.
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| CN200810218376A CN101746103A (en) | 2008-12-12 | 2008-12-12 | Method for preparing laminated polyimide metal foil |
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| CN200810218376A CN101746103A (en) | 2008-12-12 | 2008-12-12 | Method for preparing laminated polyimide metal foil |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101966766A (en) * | 2010-08-19 | 2011-02-09 | 王建 | Multi-layer metal cold-pressing compounding technology and product thereof |
| CN104842625A (en) * | 2015-05-21 | 2015-08-19 | 成都多吉昌新材料有限公司 | Preparation method of two-layer dielectric adhesive-free flexible copper clad laminate |
| WO2017193487A1 (en) * | 2016-05-13 | 2017-11-16 | 苏州卫鹏机电科技有限公司 | Method for preparing printed circuit board of ultra-thin metal layer |
| CN108358161A (en) * | 2017-12-29 | 2018-08-03 | 西北工业大学 | The preparation method of polyimide nano structure based on PS bead nanometer masks |
| CN114786942A (en) * | 2019-08-06 | 2022-07-22 | 保特利尖端材料股份有限公司 | Aluminum pouch film for secondary battery and method of manufacturing the same |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008004520A1 (en) * | 2006-07-04 | 2008-01-10 | Nippon Steel Chemical Co., Ltd. | Method of modifying surface of polyimide resin layer and process for producing metal-clad laminate |
-
2008
- 2008-12-12 CN CN200810218376A patent/CN101746103A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008004520A1 (en) * | 2006-07-04 | 2008-01-10 | Nippon Steel Chemical Co., Ltd. | Method of modifying surface of polyimide resin layer and process for producing metal-clad laminate |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101966766A (en) * | 2010-08-19 | 2011-02-09 | 王建 | Multi-layer metal cold-pressing compounding technology and product thereof |
| CN104842625A (en) * | 2015-05-21 | 2015-08-19 | 成都多吉昌新材料有限公司 | Preparation method of two-layer dielectric adhesive-free flexible copper clad laminate |
| WO2017193487A1 (en) * | 2016-05-13 | 2017-11-16 | 苏州卫鹏机电科技有限公司 | Method for preparing printed circuit board of ultra-thin metal layer |
| JP2018533191A (en) * | 2016-05-13 | 2018-11-08 | 蘇州衛鵬機電科技有限公司 | Method of manufacturing ultra-thin metal layer printed circuit board |
| US10187999B2 (en) | 2016-05-13 | 2019-01-22 | Suzhou Weipeng Electrical Technology Co., Ltd. | Method for manufacturing an ultra-thin metal layer printed circuit board |
| CN108358161A (en) * | 2017-12-29 | 2018-08-03 | 西北工业大学 | The preparation method of polyimide nano structure based on PS bead nanometer masks |
| CN114786942A (en) * | 2019-08-06 | 2022-07-22 | 保特利尖端材料股份有限公司 | Aluminum pouch film for secondary battery and method of manufacturing the same |
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Application publication date: 20100623 |