CN1283548A - Nickel-coated polyimide foil and its preparing process - Google Patents
Nickel-coated polyimide foil and its preparing process Download PDFInfo
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- CN1283548A CN1283548A CN 00114628 CN00114628A CN1283548A CN 1283548 A CN1283548 A CN 1283548A CN 00114628 CN00114628 CN 00114628 CN 00114628 A CN00114628 A CN 00114628A CN 1283548 A CN1283548 A CN 1283548A
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- nickel
- foil
- coated polyimide
- kapton
- coated
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- Manufacturing Of Printed Wiring (AREA)
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Abstract
A Ni-coated polyimide foil used as the substrate of flexible printed circuit board is made up by sticking the Ni foil onto polyimide film by adhesive. Its avantages include high stripping strength higher than 1.7 kgl/am, good soldering durability, not layering in tin bath at 260 deg.C for min, high cricking and folding strength, and high electric conductivity.
Description
The present invention relates to electronic component commercial printing circuit-board industry used base material and preparation, specially refer to a kind of new type polyimide and cover nickel foil and preparation thereof.
When making flexible print circuit (FPC) base material, modal method is bonding with Kapton and Copper Foil, as described various polyimide copper clad lamination adhesive of ZL95109152 and manufacture method thereof.Along with the fast development of FPC industry, brought into use the wiring board of nickel-coated polyimide foil processing in some field.Compare with polyimide copper clad lamination, flexibility, the electric conductivity of nickel-coated polyimide foil are better, and the nickel-coated polyimide foil of exploitation function admirable is the needs of printed circuit base material development.
Flexible print circuit base material--the nickel-coated polyimide foil that the purpose of this invention is to provide a kind of flexibility, conducts electricity very well provides a kind of this method of covering nickel foil for preparing simultaneously.
Realize the nickel-coated polyimide foil of above-mentioned purpose, form by Kapton and the nickel foil that is bonded on the film, characteristics are the testing standard built-up circuit figures according to GB/T13557-92 and IPC-TM-650, record its peel strength more than or equal to 1.70Kg/cm, anti-tin-welding is not stratified, non-foaming after 60 seconds in 260 ℃ of tin baths, folding resistance does not rupture more than 400 times, sheet resistance 1.0 * 10
5M Ω, volume resistance 1.0 * 10
6M Ω m.
Above-mentioned Kapton is a commercially available product, be aromatic series pyromellitic acid dianhydride and 4, the H type film that 4 '-diaminodiphenyl ether forms through polycondensation, film forming, stretching, cyclisation in polar solvent, BPDA and 4, the S type film that 4 '-diaminodiphenyl ether is made or compound dianhydride and 4, the X type film of 4 '-diaminodiphenyl ether.
Above-mentioned nickel foil is commercially available electrolysis or calendering nickel foil.
Preparation method's step of this nickel-coated polyimide foil is:
1. the even coated with adhesive of the one side of Kapton, the thick 0.010～0.050mm of its glue;
2. the nickel foil single face carries out roughening treatment;
3. the one side of Kapton coating adhesive is superimposed with the alligatoring face of nickel foil, places the composite pressure machine at 150 ℃～190 ℃, 20～50Kg/cm
2Following hot-press solidifying 40～120 minutes promptly makes described nickel-coated polyimide foil.
The adhesive that uses in this nickel-coated polyimide foil is a multi-component copolymer acrylate adhesive, promptly is that number of patent application is the adhesive described in 00114627.This adhesive initially contains polynary acrylic comonomers a, cross-linking modified monomer b, organic solvent c, reaction initiator d, it is formed weight ratio and is:
a．???????????100
b．???????????0．5～20
c．???????????50～500
d．???????????0．05～5
Preferable composition weight ratio is;
a．???????????100
b．???????????3～8
c．???????????150～300
d．???????????0．1～0．8
Above-mentioned acrylate co-monomers is methacrylic acid C
1～C
8Arrcostab, acrylic acid C
1～C
8The mixture of one or more in Arrcostab, styrene, acrylonitrile, the vinylacetate.
Described cross-linking modified monomer is meant methacrylic acid, acrylic acid, methacrylic acid β-C
2～C
8Hydroxy ester, propenoic acid beta-C
2～C
8In hydroxy ester, GMA, glycidyl acrylate, Methacrylamide, acrylamide, NMA, the hydroxyacrylamide two or more contains the mixture of different crosslinked groups.
Described organic solvent is one or more a mixture of toluene, dimethylbenzene, ethyl acetate, butyl acetate, dichloroethanes, trichloroethanes, chloroform, acetone, MEK, cyclohexanone.
Described reaction initiator is 2-(tert-butyl group azo) isobutyronitrile of azo-compound class, 2,2 '-ABVN, 2, the mixture of one or more of the dilauroyl peroxide of 2 '-azodiisobutyronitrile and organic peroxide class, dibenzoyl peroxide, peroxide acetic acid butyl ester, cumyl peroxide, di-tert-butyl peroxide.
The preparation method of this multi-component copolymer acrylate adhesive is: selected acrylate co-monomers, cross-linking modified monomer, reaction initiator, organic solvent are added in the reactor that has heater, agitating device, reflux and thermometer in proportion mix; Stir and heat up, feed nitrogen during the reaction beginning to shorten the reaction initiation time, the control reaction temperature was reacted 5～16 hours between 60 ℃～120 ℃; Cooling discharging is 15%～35% with solvent dilution to solid content then, promptly gets required multi-component copolymer acrylate adhesive.
Embodiments of the invention:
Embodiment 1.
Get the thick Kapton of 0.050mm, evenly coat aforementioned multi-component copolymer acrylate adhesive in its one side, the thick 0.020mm of glue, superimposed with the alligatoring electrolysis nickel foil that 0.035mm is thick, place the composite pressure machine at 170 ℃, 40kg/cm
2Hot-press solidifying was made flexible print circuit base material nickel-coated polyimide foil after 60 minutes under the condition.Testing standard by GB/T13557-92 and IPC-TM-650 is made circuitous pattern, records peel strength, soldering resistance, folding resistance and electrical property etc., the results are shown in Table 1.
Embodiment 2.
Get the thick Kapton of 0.025mm, evenly coat aforementioned multi-component copolymer acrylate adhesive in its one side, the thick 0.010mm of glue, superimposed with the alligatoring electrolysis nickel foil that 0.035mm is thick, place the composite pressure machine at 150 ℃, 50kg/cm
2Hot-press solidifying was made flexible print circuit base material nickel-coated polyimide foil after 90 minutes under the condition.With the identical method production standard specimen of embodiment 1, test result sees Table 1.
Embodiment 3.
Get the thick Kapton of 0.040mm, evenly coat aforementioned multi-component copolymer acrylate adhesive in its one side, the thick 0.015mm of glue, superimposed with the thick alligatoring of 0.035mm calendering nickel foil, in the composite pressure machine in 190 ℃, 20kg/cm
2Following hot-press solidifying was made nickel-coated polyimide foil after 120 minutes.Make the standard testing sample by embodiment 1 identical method, test result sees Table 1.
Embodiment 4.
Get the thick Kapton of 0.025mm, evenly coat aforementioned multi-component copolymer acrylate adhesive in its one side, the thick 0.020mm of glue, superimposed with the alligatoring calendering nickel foil that 0.020mm is thick, place the composite pressure machine at 170 ℃, 30kg/cm
2Following hot-press solidifying was made nickel-coated polyimide foil after 60 minutes.Press the identical method production standard specimen of embodiment 1, test result sees Table 1.
Embodiment 5.
Get the thick Kapton of 0.050mm, evenly coat aforementioned multi-component copolymer acrylate adhesive in its one side, the thick 0.030mm of glue, superimposed with the calendering nickel foil that 0.020mm is thick, place the composite pressure machine at 170 ℃, 40kg/cm
2Following hot-press solidifying was made nickel-coated polyimide foil after 40 minutes.Press the identical method production standard specimen of embodiment 1, test result sees Table 1.
Comparative Examples 1.
Get methacrylic acid 5 grams, butyl acrylate 70 grams, acrylonitrile 30, peroxide acetic acid butyl ester 0.8 gram, butyl acetate: mixed solvent 300 grams of MEK=2: 1 mix, heating reflux reaction is 10 hours in having the 500ml three-necked bottle of agitator, condenser, thermometer, and cooling back adds 5 gram epoxy resin E-51 (Chinese Wuxi resin processing plant produce) and obtains adhesive.The gained adhesive is evenly coated on the thick Kapton of 0.050mm, the thick 0.020mm of glue, superimposed with the alligatoring electrolytic copper foil that 0.035mm is thick, place the composite pressure machine at 170 ℃, 40kg/cm
2Following hot-press solidifying made the coated polyimide Copper Foil after 90 minutes.Press the identical method production standard specimen of embodiment 1, test result sees Table 1.
Data from table 1 as can be seen, the nickel-coated polyimide foil of embodiment 1～5 is better than peel strength height, the electric conductivity of the coated polyimide Copper Foil of Comparative Examples 1, folding resistance is better.Table 1
| Test event | Test condition | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Comparative Examples 1 | Method of testing |
| Peel strength (kg/cm) | Normality | 1．82 | ?1．78 | ?1．77 | ?1．86 | ?1．86 | ?1．63 | The 3.1st of GB/T13557 |
| Handle after 30 minutes for 125 ℃ | 1．81 | ?1．76 | ?1．76 | ?1．84 | ?1．81 | ?1．58 | The 3.2nd of GB/T13557 | |
| After 200 ℃ of thermal shocks are handled | 1．75 | ?1．71 | ?1．70 | ?1．76 | ?1．73 | ?1．52 | The 3.3rd of GB/T13557 | |
| After trichloro-ethylene soaks 3 minutes | 1．75 | ?1．70 | ?1．68 | ?1．74 | ?1．70 | ?1．48 | The 3.4th of GB/T13557 | |
| Anti-tin-welding (second) | In 260 ℃ of tin baths | ＞60 | ?＞60 | ?＞60 | ?＞60 | ?＞60 | ?＞60 | IPC-TM-650-2.4B (method A) |
| Volume resistance (M Ω m) | After constant humid heat treatment is recovered | 2．8× ?10 6 | 3．1× ?10 6 | 2．6× ?10 6 | 4．4× ?10 6 | 2．5× ?10 6 | 2．5× ?10 6 | GB4722 the 5th chapter |
| Sheet resistance (M Ω) | After constant humid heat treatment is recovered | 3．3× ?10 5 | 2．7× ?10 5 | 3．5× ?10 5 | 3．2× ?10 5 | 2．7× ?10 5 | 1．9× ?10 5 | GB4722 the 6th chapter |
| Dielectric constant (maximum) | After constant humid heat treatment is recovered | 3．5 | ?3．7 | ?3．3 | 3．2 | 3．4 | 3．4 | GB4722 the 9th chapter |
| Dielectric loss angle tangent (maximum) | After constant humid heat treatment is recovered | 0．035 | ?0．033 | ?0．032 | ?0．037 | ?0．035 | ?0．036 | GB4722 the 9th chapter |
| Perpendicular layers is to electrical strength (KV/mm minimum of a value) | 112 | ?107 | ?109 | ?102 | ?113 | ?107 | The GB4722 Chapter 11 | |
| Chemical proofing | 2NNaOH/10 minute | No change | No change | No change | No change | No change | No change | IPC-TM-650- ????2．3．2A |
| 2NHCl solution/10 minute | No change | No change | No change | No change | No change | No change | ||
| Folding resistance | ?413 | ?448 | ?531 | ?548 | ?524 | ?115 | GB4722 the 4th chapter |
Claims (5)
1. nickel-coated polyimide foil, form by Kapton and the nickel foil that is bonded on this film, it is characterized in that this nickel-coated polyimide foil makes circuitous pattern according to the testing standard of GB/T13557-92 and IPC-TM-650 and record peel strength more than or equal to 1.70Kg/cm; Anti-tin-welding is not stratified, non-foaming in 260 ℃ of tin baths, after 60 seconds; Folding resistance does not rupture more than 400 times; Sheet resistance 1.0 * 10
5M Ω; Volume resistance 1.0 * 10
6M Ω m.
2. nickel-coated polyimide foil as claimed in claim 1, it is characterized in that Kapton is aromatic series pyromellitic acid dianhydride and 4, H type film, BPDA and 4 that 4 '-diaminodiphenyl ether is made, the X type film that make the S type film that 4 '-diaminodiphenyl ether is made or compound dianhydride and 4,4 '-diaminodiphenyl ether.
3. nickel-coated polyimide foil as claimed in claim 1 is characterized in that nickel foil is electrolysis or calendering nickel foil.
4. the preparation method of the described nickel-coated polyimide foil of claim 1 is characterized in that step is:
1. at the even coated with adhesive of one side of Kapton, the thick 0.010～0.050mm of its glue
2. the nickel foil single face carries out roughening treatment;
3. the one side of Kapton coating adhesive is superimposed with the one side of nickel foil alligatoring, places the composite pressure machine at 150 ℃～190 ℃, 20～50Kg/cm
2Following hot-press solidifying 40～120 minutes promptly makes described nickel-coated polyimide foil;
5. preparation method as claimed in claim 4, the adhesive that it is characterized in that on the Kapton being coated with is a multi-component copolymer acrylate adhesive.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB001146289A CN1151921C (en) | 2000-06-13 | 2000-06-13 | Nickel-coated polyimide foil and its preparing process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB001146289A CN1151921C (en) | 2000-06-13 | 2000-06-13 | Nickel-coated polyimide foil and its preparing process |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1283548A true CN1283548A (en) | 2001-02-14 |
| CN1151921C CN1151921C (en) | 2004-06-02 |
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ID=4584279
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB001146289A Expired - Lifetime CN1151921C (en) | 2000-06-13 | 2000-06-13 | Nickel-coated polyimide foil and its preparing process |
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| Country | Link |
|---|---|
| CN (1) | CN1151921C (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112778563A (en) * | 2021-01-25 | 2021-05-11 | 深圳和力纳米科技有限公司 | Polyimide film and preparation method thereof |
-
2000
- 2000-06-13 CN CNB001146289A patent/CN1151921C/en not_active Expired - Lifetime
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112778563A (en) * | 2021-01-25 | 2021-05-11 | 深圳和力纳米科技有限公司 | Polyimide film and preparation method thereof |
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| Publication number | Publication date |
|---|---|
| CN1151921C (en) | 2004-06-02 |
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Address after: No. 30 Guan Shan Road, Hongshan District, Hubei, Wuhan Patentee after: Huashuo Technology Co., Ltd. Address before: No. 30 Guan Shan Road, Hongshan District, Hubei, Wuhan Patentee before: Hubei Research Institute of Chemistry |
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Denomination of invention: Nickel-coated polyimide foil and its preparing process Effective date of registration: 20100907 Granted publication date: 20040602 Pledgee: Bank of Hankou, Limited by Share Ltd, Optics Valley branch Pledgor: Huashuo Technology Co., Ltd. Registration number: 2010990000869 |
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Date of cancellation: 20151106 Granted publication date: 20040602 Pledgee: Bank of Hankou Limited by Share Ltd Optics Valley branch Pledgor: Huashuo Technology Co., Ltd. Registration number: 2010990000869 |
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