CN101654001B - Metallized film, preparation method thereof and circuit board containing same - Google Patents
Metallized film, preparation method thereof and circuit board containing same Download PDFInfo
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- CN101654001B CN101654001B CN200810141986.9A CN200810141986A CN101654001B CN 101654001 B CN101654001 B CN 101654001B CN 200810141986 A CN200810141986 A CN 200810141986A CN 101654001 B CN101654001 B CN 101654001B
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Abstract
The invention discloses a metallized film, which comprises a polymer bottom layer and a metal layer on the bottom layer, and is characterized in that the polymer bottom layer is a porous polyimide film. The invention also discloses a preparation method of the metallized film. The metallized film prepared by the method disclosed by the invention is not processed by a strong acid or a strong base, the porous polyimide film as the bottom layer is intact, and the peeling strength of the metal layer on the porous polyimide film is high. A circuit board prepared by adopting the metallized film has the advantages of thin thickness, excellent heat resistance and good product stability.
Description
[technical field]
The present invention relates to a kind of metalized film and preparation method thereof and the wiring board containing this metalized film, especially a kind of surface film having metallic circuit and preparation method thereof and the wiring board containing this film.
[background technology]
In recent years, along with the continuous progress of microelectric technique, electronic device is towards miniaturization, high power and highly integrated future development.This development trend certainly will cause the insulation between each parts of inside of electronic component and resistance to heat problem more outstanding.
The insulation of polyimides and heat resistance are very excellent, and simultaneously it also has good thermal stability, can the advantages such as high temperature resistant and low temperature, good mechanical property, thermal coefficient of expansion be low.So polyimides has vast application prospect at microelectronic.
On Kapton, form line pattern by photoetching, exposure, development in prior art, but the method is polluted greatly, operates inconvenience, length consuming time, is unfavorable for the production that becomes more meticulous.
A kind of method of Kapton laser induced selective chemical plating is disclosed in CN1772948.By Kapton is first carried out the Kapton that dissimulated electricity silver ion is made in modification, then the Kapton laser focusing of dissimulated electricity silver ion is carried out selective radiation, then after dilute acid pretreatment and high-temperature heating, carry out chemical plating can obtain the Kapton patterned chemical deposit of micron order on the surface.The method is implemented simply, it is little to pollute, figure can control by computer in real time, selective height.But carrying out modification to Kapton is carry out in strong base solution, very easily causes the hydrolysis of Kapton and damages film, and the chemical deposit prepared by the method for this disclosure of the invention is lower in the peel strength on Kapton surface.The wiring board stability prepared by the method is not high.
[summary of the invention]
For overcoming the low problem of the peel strength of metal level on bottom, the invention discloses a kind of metalized film, in this metalized film, polyimide film is complete not impaired, more stable, and surface metal-layer is high as the peel strength on the porous polyimide film of bottom.
The invention discloses a kind of metalized film, comprise the metal level on polymer base coat and described bottom, it is characterized in that: described polymer base coat is porous polyimide film.
Described porous polyimide film thickness is 0.01-2mm, and average pore size is 0.01-40um, and porosity is 30-80%.
The invention also discloses the preparation method of above-mentioned metalized film, comprising:
A, porous polyimide film to be contacted with the solution of metal complex, obtain modified polyimide film;
Modified polyimide film described in b, illumination, obtains metalized film precursor;
C, on described metalized film precursor, form metal level, obtain metalized film.
Modified polyimide film can also be kept 60-120min by method disclosed by the invention before above-mentioned illumination at 149-156 DEG C.
The invention also discloses a kind of wiring board, comprise internal layer circuit plate and the first layers of copper and the second layers of copper that are distributed in described internal layer circuit plate both sides, it is characterized in that: described internal layer circuit plate is above-mentioned metalized film.
In metalized film prepared by method disclosed by the invention, owing to not adopting strong acid or highly basic process, the porous polyimide film as bottom stands intact, and the peel strength of metal level on porous polyimide film is high.In addition, this method is implemented simply, it is little to pollute, figure can be controlled in real time by computer, selective height.
The wiring board adopting metalized film disclosed by the invention to obtain can give full play to the feature of polyimide film, makes the thickness of product thin, and Good Heat-resistance, good stability.
[accompanying drawing explanation]
The porous polyimide film that Fig. 1 adopts for embodiment 1;
Fig. 2 is each layer schematic diagram of multilayer circuit board disclosed by the invention.
In figure: 1, the first layers of copper; 2, the second layers of copper; 3, metalized film; 4, semi-solid preparation layer; 5, metal level; 6, porous polyimide film.
[detailed description of the invention]
The invention discloses a kind of metalized film, comprise the metal level on polymer base coat and described bottom, it is characterized in that: described polymer base coat is porous polyimide film.
Porous polyimide film disclosed in this invention refers to the polyimide film containing plural cavernous structure, and described cavernous structure can be through hole or non through hole.Described through hole refers to the hole running through monolithic films.
Concrete, described porous polyimide film thickness is 0.01-2mm, and average pore size is 0.01-40um, and porosity is 30-80%.Under preferable case, described porous polyimide film thickness is 0.1-1mm, average pore size 0.01-5um, and porosity is 60-80%.Described porous polyimide film can be commercially available, as the porous polyimide film that Ube Industries Ltd. (Ube Industries) Co., Ltd. produces; Also can make by oneself, as by the solution film forming containing polyimides, pore-forming substance and solvent, and remove pore-forming substance at lower than polyimides glass temperature, concrete grammar has been conventionally known to one of skill in the art, does not repeat them here.
High by the peel strength of the metalized film adopting porous polyimide film preparation disclosed by the invention, and the thermal shock peel strength of the wiring board prepared by this metalized film is compared in prior art, have also been obtained large increase.
Described metal layer thickness is 0.005-0.1mm; Under preferable case, described metal layer thickness is 0.025-0.07mm.When described polymer base coat and metal layer thickness are in above-mentioned scope, peel strength higher between porous polyimide film and metal level can be obtained, the requirement to electronic device microminiaturization can be adapted to again.The thickness of metal level adopts thickness of coating tester (U.S. KOCOUR Model:6000) to record according to the method described in GB/T4955-2005.
Described metal level is one or more in copper coating, nickel coating, silvering, palladium coating, platinum coating and gold plate.Under preferable case, described metal level is one or more in copper coating, nickel coating, silvering.
The invention also discloses the preparation method of described metalized film, comprising:
A, porous polyimide film to be contacted with the solution of metal complex, obtain modified polyimide film;
Modified polyimide film described in b, illumination, obtains metalized film precursor;
C, on described metalized film precursor, form metal level, obtain metalized film.
Average pore size and the porosity of described porous polyimide film illustrate above, do not repeat them here.
The described method contacted with the solution of metal complex by porous polyimide film can for conventional various methods, as porous polyimide film is immersed in metal complex solution in 1-10min.
Described metal complex is one or more and 4-carboxyl phenoxy acetic acid, diamino-acetic acid, saccharin, lysine plus threonine, rutin sophorin, kilnitamin, salicylaldoxime, hydrated sulfuric acid four ammonia, pyrithione, shitosan, oxine, amide-type tripodal ligand, taurine schiff base, hydroxy propyl rutin, 2 in copper, aluminium, Au Ag Pt Pd and nickel, one or more complexs formed in 2 '-bipyridyl, citric acid, 2,4-Nitroimidazoles, large ring cyano group or indole-3-monoprop; The concentration of metal complex solution is 0.1-10mol/l, is preferably 0.5-3mol/l.
Inventor finds, when the concentration of metal complex solution is in above-mentioned scope, contact with thickness, average pore size and the porosity porous polyimide film in aforementioned range, be conducive to metal complex in porous polyimide film surface attachment, after illumination, the metal active centres obtained can at porous polyimide film surface more stable existence, makes the peel strength of metal level on the metalized film that obtains larger.When the concentration of metal complex solution and thickness, average pore size and porosity are in respective preferable range, form the effect cooperatively interacted between the metal active centres energy that metal complex and illumination obtain and micropore, be more conducive to the raising of the peel strength of metal level on metalized film.
Above-mentioned metal complex obtains by self-control, as: 4-carboxyl phenoxy acetic acid is dissolved in DMF (DMF) solution, copper nitrate solution slowly instills in above-mentioned 4-carboxyl phenoxy acetic acid solution again, after stirring at room temperature 30min, separatory, can obtain the complex solution of Cu.Although containing hydrogen ion and nitrate ion in this solution, because content is very low, and at described temperature and time of contact, the hydrogen ion in solution and nitrate ion can not have an impact to the porous polyimide film that the present invention adopts.
Before described illumination, first modified polyimide film is kept 60-120min at 149-156 DEG C under preferable case.By carrying out illumination again after above-mentioned process, be conducive to the deposition of metal active centres on porous polyimide film surface, thus improve the peel strength of metalized film.
Described illumination modified polyimide film method is: adopt wavelength to be that 300-1200nm, Q are frequently for the laser of 3-40kHz irradiates described modified polyimide film 10-120s.By induced with laser, impel metal complex to decomposite metal simple-substance particle and become the spike forming metal level.The DPY series semiconductor pumping Nd:YAG laser marking system that described irradiation is produced by Shenzhen City Tete Laser Technology Co., Ltd. carries out.
When making line pattern, by the course of programme-control light source, carrying out elective irradiation, obtaining the spike of the metal level forming grain pattern.
In the present invention, according to the metallized needs of single or double, the one or both sides of modified polyimide film can also be irradiated.Be: first modified polyimide film is irradiated under these conditions then modified polyimide film is overturn, with another side just to light source, irradiate under these conditions the method that the two sides of modified polyimide film is all irradiated.
The method that described metalized film precursor is formed metal level is chemical plating or plating.The method of described plating and chemical plating has been conventionally known to one of skill in the art.As at 50 DEG C, above-mentioned metalized film precursor is placed in plating solution and carries out electroless copper 20min or above-mentioned metalized film precursor is placed in plating solution being negative electrode with metalized film precursor, being that anode carries out electro-coppering 30min with copper electrode.Above-mentioned metalized film can be obtained.Described plating solution is sulfate or the nitrate of copper, aluminium etc.
The invention also discloses a kind of wiring board, comprise internal layer circuit plate and the first layers of copper and the second layers of copper that are distributed in described internal layer circuit plate both sides, it is characterized in that: described internal layer circuit plate is above-mentioned metalized film.
The preparation method of above-mentioned wiring board is known in this field, as: the first layers of copper (Zhuhai Totking Electron Technology Co., Ltd.), prepreg (positive extensive region, Shanghai-Hong Bang adhesive tape), metalized film, prepreg (positive extensive region, Shanghai-Hong Bang adhesive tape) and the second layers of copper (Zhuhai Totking Electron Technology Co., Ltd.) are stacked together, put into multilayer line laminating machine (Shanghai rich can company) pressing, then through hole.
Pressing condition is known in this field, as in laminating machine, in 160-180 DEG C, pressure is 25-50kg/cm
2under condition, hot pressing 60min, obtains multi-layer sheet; Then above-mentioned multi-layer sheet is placed 1h at 160 DEG C.
Be method well known in the art to upper through-hole approaches, as: first use circuit board etching machine (Beijing Hao Wei Creative Technology Ltd.) to scribe whole circuitous pattern in the first layers of copper; Whole first layers of copper plate face is pasted, with part beyond masking aperture again with the diaphragm of band gum; Use circuit board etching machine drill hole subsequently, after completing, multi-layer sheet is placed in vacuum adsorption table; With providing rubber flap evenly to scrape crowded conductive paste (Li Xing Electron Material Co., Ltd of Shenzhen) at random on the first layers of copper plate face, make in its access aperture.Meanwhile, vacuum adsorption force more makes conductive paste flow in hole, finally causes only on hole wall, leaving one deck conductive paste.After coated with conductive cream, the diaphragm being used for sheltering is taken off, circuit board is placed in 130 DEG C of hot-blast ovens and heats 60min, conductive paste is solidified, obtain the hole wall being covered with silver coating, achieve hole electricity conduction.Obtain wiring board of the present invention.
Wiring board disclosed by the invention, due to the employing of internal layer circuit plate is metalized film provided by the invention, and can give full play to the advantage of polyimide film, this wiring board performance is operationally more stable, and the peel strength after heat-shock is still higher.
Below by embodiment, the present invention is further illustrated.
Embodiment 1
The present embodiment is for illustration of metalized film disclosed by the invention and preparation method thereof.
1, metal complex is prepared
The 4-carboxyl phenoxy acetic acid of 5mol is dissolved in the N of 500ml, in dinethylformamide, be that the copper nitrate solution of 10mol/l under agitation slowly instills in above-mentioned solution again by 500ml concentration, stirring at room temperature 30min, can obtain the complex solution that concentration is the Cu of 5mol/l.
2, modified polyimide film is prepared
Porous polyimide film (UBE Industries Ltd., thickness is 1.5mm, and average pore size is 10um, and porosity is 50%) is immersed in 5min in the solution of above-mentioned metal complex.
3, metalized film precursor is prepared
Laser is adopted to irradiate above-mentioned modified polyimide film.Optical maser wavelength is 1064nm, Q is 20kHz frequently, and laser irradiation time is 60s.
4, metalized film is prepared
The copper sulfate bath that above-mentioned metalized film precursor is placed in 16g/l is carried out electroless copper 15min.Take out, drying obtains metalized film A1.Recording metal layer thickness on A1 is 0.02mm.
Embodiment 2
The present embodiment is for illustration of metalized film disclosed by the invention and preparation method thereof.
1, metal complex is prepared
Be dissolved in the DMF of 800ml by the diamino-acetic acid of 2mol, then be that the liquor argenti nitratis ophthalmicus of 10mol/l under agitation slowly instills in above-mentioned solution by 200ml concentration, stirring at room temperature 30min, can obtain the complex solution that concentration is the Ag of 2mol/l.
2, modified polyimide film is prepared
Porous polyimide film (UBE Industries Ltd., thickness is 0.8mm, and average pore size is 1um, and porosity is 70%) is immersed in 8min in the solution of above-mentioned metal complex.
3, metalized film precursor is prepared
Laser is adopted to irradiate above-mentioned modified polyimide film.Optical maser wavelength is 1064nm, Q is 30kHz frequently, and laser irradiation time is 90s.
4, metalized film is prepared
The silver nitrate plating solution that above-mentioned metalized film precursor is placed in 16g/l is carried out electroless copper 40min.Take out, drying obtains metalized film A2.Recording metal layer thickness on A2 is 0.05mm.
Embodiment 3
The present embodiment is for illustration of metalized film disclosed by the invention and preparation method thereof.
1, metal complex is prepared
The saccharin of 1mol is dissolved in the N of 750ml, in dinethylformamide solution, be that the copper nitrate solution of 4mol/l under agitation slowly instills in above-mentioned solution again by 250ml concentration, stirring at room temperature 30min, can obtain the complex solution that concentration is the Cu of 1mol/l.
2, modified polyimide film is prepared
Porous polyimide film (UBE Industries Ltd., thickness is 0.5mm, and average pore size is 3um, and porosity is 60%) is immersed in 6min in the solution of above-mentioned metal complex.
3, metalized film precursor is prepared
Modified polyimide film is kept 90min at 150 DEG C.
Laser is adopted to irradiate above-mentioned modified polyimide film.Optical maser wavelength is 1064nm, Q is 30kHz frequently, and laser irradiation time is 80s.
4, metalized film is prepared
The copper sulfate bath that above-mentioned metalized film precursor is placed in 16g/l is carried out electroless copper 30min.Take out, drying obtains metalized film A3.Recording metal layer thickness on A3 is 0.03mm.
Comparative example 1
This comparative example is for illustration of metalized film of the prior art and preparation method thereof.
Metalized film D1 is prepared according to method disclosed in patent CN1772948 embodiment 1.
Embodiment 5
The present embodiment is for illustration of wiring board disclosed by the invention.
Obtained to first layers of copper, prepreg, embodiment 1 metalized film A1, prepreg and the second layers of copper are stacked together, put into multilayer line laminating machine (Shanghai rich can company) pressing, then through hole, obtain wiring board X1.
Pressing condition is: in 170 DEG C, pressure is 30kg/cm
2under condition, hot pressing 60min, obtains multi-layer sheet; Then above-mentioned multi-layer sheet is placed 1h at 160 DEG C.
Embodiment 6
The present embodiment is for illustration of wiring board disclosed by the invention.
Wiring board X2 is prepared according to the method for embodiment 5, unlike, the A1 in the metalized film A2 replacement embodiment 5 adopting embodiment 2 obtained.
Embodiment 7
The present embodiment is for illustration of wiring board disclosed by the invention.
Wiring board X3 is prepared according to the method for embodiment 5, unlike, the A1 in the metalized film A3 replacement embodiment 5 adopting embodiment 3 obtained.
Comparative example 2
This comparative example is for illustration of wiring board of the prior art.
Wiring board XD1 is prepared according to the method for embodiment 5, unlike, the A1 in the metalized film D1 replacement embodiment 5 adopting comparative example 1 obtained.
Performance test
1, peel strength test is carried out to above-mentioned obtained metalized film A1, A2, A3 and D1:
Test according to the method described in GBT13557-1992.
2, thermal shock peel strength test is carried out to above-mentioned obtained metalized film X1, X2, X3 and XD1:
Test according to the method described in GBT13557-1992.
Test result is in table 1.
Table 1
| Sample | A1 | A2 | A3 | D1 |
| Peel strength/N/mm | 2.13 | 3.02 | 2.85 | 0.11 |
| Sample | X1 | X2 | X3 | XD1 |
| Thermal shock peel strength/N/mm | 1.35 | 2.14 | 1.99 | Foaming comes off |
The test result of analytical table 1 is known, compared to prior art, the wiring board (X1-X3) of metalized film disclosed by the invention (A1-A3) and this metalized film of employing, its peel strength and thermal shock peel strength are obtained for obvious raising.
The test result of contrast A1-A3, when the thickness of the concentration of metal complex and porous polyimide film, average pore size and porosity are in preferable range of the present invention, peel strength and the thermal shock peel strength of metalized film (A2 and A3) and corresponding wiring board (X2 and X3) are higher.And as can be seen from the test result of A2 and A3, before carrying out illumination, at 149-156 DEG C, kept by modified polyimide film 60-120min very favourable to the performance improving metalized film and wiring board further.
Claims (13)
1. a metalized film, comprise the metal level on polymer base coat and described bottom, it is characterized in that: described polymer base coat is porous polyimide film, described porous polyimide film thickness is 0.01-2mm, average pore size is 0.01-40um, and porosity is 30-80%.
2. metalized film according to claim 1, is characterized in that: described porous polyimide film thickness is 0.1-1mm, average pore size 0.01-5um, and porosity is 60-80%.
3. metalized film according to claim 1, is characterized in that: described metal layer thickness is 0.005-0.1mm.
4. according to the metalized film in claim 1-3 described in any one, it is characterized in that: described metal level is one or more in copper coating, nickel coating, silvering, palladium coating, platinum coating and gold plate.
5. a preparation method for metalized film, comprising:
A, porous polyimide film to be contacted with the solution of metal complex, obtain modified polyimide film;
Modified polyimide film described in b, illumination, obtains metalized film precursor;
C, on described metalized film precursor, form metal level, obtain metalized film.
6. preparation method according to claim 5, is characterized in that, described porous polyimide film thickness is 0.01-2mm, and average pore size is 0.01-40um, and porosity is 30-80%.
7. the preparation method according to claim 5 or 6, is characterized in that, described is that porous polyimide film is immersed in 1-10min in the solution of metal complex by the method that porous polyimide film contacts with the solution of metal complex.
8. preparation method according to claim 7, is characterized in that, the concentration of metal complex solution is 0.1-10mol/l; Described metal complex is one or more and 4-carboxyl phenoxy acetic acid, diamino-acetic acid, saccharin, lysine plus threonine, rutin sophorin, kilnitamin, salicylaldoxime, hydrated sulfuric acid four ammonia, pyrithione, shitosan, oxine, amide-type tripodal ligand, taurine schiff base, hydroxy propyl rutin, 2 in copper, aluminium, Au Ag Pt Pd and nickel; one or more complexs formed in 2 '-bipyridyl, citric acid, 2,4-Nitroimidazoles, large ring cyano group or indole-3-monoprop.
9. preparation method according to claim 5, is characterized in that, before being also included in described illumination, modified polyimide film is kept 60-120min at 149-156 DEG C.
10. the preparation method according to claim 5 or 9, is characterized in that, described illumination modified polyimide film method is: adopt wavelength to be that 300-1200nm, Q are frequently for the laser of 3-40kHz irradiates described modified polyimide film 10-120s.
11. preparation methods according to claim 5, is characterized in that, the method that described metalized film precursor is formed metal level is chemical plating or plating.
12. 1 kinds of wiring boards, comprise internal layer circuit plate and the first layers of copper and the second layers of copper that are distributed in described internal layer circuit plate both sides, it is characterized in that: described internal layer circuit plate is the metalized film described in claim 1-4.
13. 1 kinds of wiring boards, being comprised internal layer circuit plate and the first layers of copper and the second layers of copper that are distributed in described internal layer circuit plate both sides, it is characterized in that: the metalized film of described internal layer circuit plate for being prepared by the method described in claim 5-11.
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Families Citing this family (7)
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| CN102529223B (en) * | 2010-12-30 | 2014-12-10 | 比亚迪股份有限公司 | Polyimide metal overprinting body and preparation method thereof, and dual-sided metal overprinting body |
| CN104902689A (en) * | 2014-03-05 | 2015-09-09 | 立诚光电股份有限公司 | Method for manufacturing circuit and a ceramic substrate having circuit pattern |
| CN104191804B (en) * | 2014-09-05 | 2016-02-03 | 电子科技大学 | A kind of preparation method of glue-free flexible double face copper |
| CN106337197B (en) * | 2016-09-27 | 2018-12-28 | 东莞中探探针有限公司 | A kind of electric connector electroplating technology |
| CN108754467B (en) * | 2018-06-27 | 2021-01-12 | 深圳市贝加电子材料有限公司 | Ruthenium palladium alloy chemical plating solution and plating method and application thereof |
| CN114729258A (en) * | 2020-02-13 | 2022-07-08 | 昭和电工材料株式会社 | CMP polishing liquid and polishing method |
| CN113278972B (en) * | 2021-04-29 | 2022-02-01 | 中国电子科技集团公司第二十九研究所 | Preparation method of conformal radiation layer |
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| CN1392764A (en) * | 2001-06-18 | 2003-01-22 | 日东电工株式会社 | Method for producing metal foil laminated product and method for producingcircuit board |
| CN1715444A (en) * | 2004-05-27 | 2006-01-04 | 恩通公司 | Method for metallizing plastic surfaces |
| CN1772948A (en) * | 2005-11-17 | 2006-05-17 | 上海交通大学 | Laser induced selective chemical plating process for polyimide film |
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| CN1392764A (en) * | 2001-06-18 | 2003-01-22 | 日东电工株式会社 | Method for producing metal foil laminated product and method for producingcircuit board |
| CN1715444A (en) * | 2004-05-27 | 2006-01-04 | 恩通公司 | Method for metallizing plastic surfaces |
| CN1772948A (en) * | 2005-11-17 | 2006-05-17 | 上海交通大学 | Laser induced selective chemical plating process for polyimide film |
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