CN113293373A - Polyimide film with surface covered with metal pattern layer and preparation method thereof - Google Patents
Polyimide film with surface covered with metal pattern layer and preparation method thereof Download PDFInfo
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- CN113293373A CN113293373A CN202010110495.9A CN202010110495A CN113293373A CN 113293373 A CN113293373 A CN 113293373A CN 202010110495 A CN202010110495 A CN 202010110495A CN 113293373 A CN113293373 A CN 113293373A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C26/00—Coating not provided for in groups C23C2/00 - C23C24/00
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/12—Chemical modification
- C08J7/123—Treatment by wave energy or particle radiation
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
- C21D9/0068—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for particular articles not mentioned below
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/02—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/14—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of noble metals or alloys based thereon
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2379/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2361/00 - C08J2377/00
- C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08J2379/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
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- Polymers & Plastics (AREA)
- Manufacturing Of Printed Wiring (AREA)
Abstract
A polyimide film with a metal pattern layer covered on the surface is prepared by the following steps: firstly preparing strong alkaline glue solution, printing the strong alkaline glue solution on the surface of a polyimide film according to a designed pattern, keeping the pattern for a certain time, etching to generate polyamic acid salt, then soaking the polyimide film in a soluble metal salt solution for ion exchange to obtain the polyimide film with metal ions loaded on the surface, then soaking the polyimide film in a reducing agent solution to reduce the metal ions into metal, and finally performing slow heat treatment to ensure that the polyamic acid salt forms polyimide again to obtain the polyimide film with the surface covered with a metal pattern layer. The method is suitable for polyimide films of all systems, can realize metal patterning in any shape, has excellent interface bonding performance, excellent conductivity and environmental friendliness, and has good industrial prospect.
Description
Technical Field
The invention belongs to the field of polymer matrix composite materials, and relates to a polyimide film with a metal pattern layer covered on the surface and a preparation method thereof.
Background
The Flexible Printed Circuit (FPC) is a highly reliable and Flexible Printed Circuit made of Polyimide (PI) or polyester film as a substrate, and has the characteristics of high wiring density, light weight, thin thickness and good bending property. Patterning of metal layers is a crucial step in the production of flexible printed circuit boards.
The patterning techniques that are mainly used at present are photolithography and inkjet printing. The photoetching method is mainly applied to preparing copper metal patterns and comprises nine steps of gluing, exposing, developing, baking and the like, and although the obtained copper metal patterns have high resolution, the steps are complicated and the pollution is serious; the ink jet printing technology is fast in forming, and only needs to print the metal ink precursor on the surface of the film and then carry out simple post-treatment, but the conductive pattern obtained by the method has poor resolution and poor adhesion with the base material, so that the use value of the conductive pattern is greatly limited. Therefore, finding a simple and effective method for patterning a metal on a polyimide surface is the focus of research in this field.
Therefore, the invention provides a method for growing a metal pattern on the surface of a polyimide film in situ. The method utilizes the characteristic that an imide ring in polyimide is easy to be subjected to alkaline hydrolysis, a strong alkaline glue solution is used for printing a pattern on the surface of a polyimide film for etching to form a layer of pattern of polyamic acid salt, carboxyl and water-soluble metal salt are subjected to ion exchange reaction, metal ions are introduced into the etched pattern, then the metal ions are reduced through a chemical reducing agent, and finally the etched pattern is subjected to heat treatment to form polyimide through ring closure again, so that the polyimide film with the metal pattern growing on the surface in situ is obtained.
Disclosure of Invention
The invention aims to solve the defects of the prior art and provides the method for growing the metal pattern on the surface of the polyimide film in situ, which has excellent interface bonding performance and conductivity, high utilization rate of metal ions, environmental friendliness and easy popularization and industrial production.
A polyimide film with a surface covered with a metal pattern layer, wherein the thickness of the polyimide layer is 20-200 μm, and the thickness of the metal pattern layer is 100-800 nm.
Further, the thickness of the polyimide layer is preferably 25 to 150 μm, particularly preferably 30 to 100 μm; the thickness of the metal pattern layer is preferably 150-700nm, and particularly preferably 200-650 nm.
Further, the metal of the metal pattern layer is silver, copper, or the like; the pattern shape of the metal pattern layer is any printable pattern.
A preparation method of a polyimide film with a metal pattern layer covered on the surface is characterized by comprising the following steps:
A. carrying out plasma treatment on a Polyimide (PI) film, and printing strong alkaline glue solution on the surface of the polyimide film to obtain the polyimide film with a surface loaded with a modified pattern;
B. soaking the polyimide film with the surface loaded with the modified pattern obtained in the step A in a soluble metal salt solution for ion exchange to obtain a polyimide film with the surface loaded with metal ions;
C. soaking the polyimide film loaded with metal ions on the surface obtained in the step B in a reducing agent solution for reduction to obtain the polyimide film loaded with metal patterns on the surface;
D. and D, carrying out heat treatment on the polyimide film with the metal pattern loaded on the surface obtained in the step C in an inert atmosphere to obtain the polyimide film with the metal pattern loaded on the surface with high adhesiveness.
Further, repeating steps B and C before the heat treatment to increase the thickness of the metal layer; the number of repetitions is preferably from 2 to 15.
Wherein, the polyimide film is washed with deionized water and ethanol before the plasma treatment in the step A. Plasma treatment process: the polyimide film is placed in a cavity of a plasma processing device, the input voltage is 110-.
Wherein, the concentration of the strong alkaline glue solution is 2-8M, preferably 2.5-6.5M; the strong alkaline solution is KOH, NaOH solution, etc. The strong alkaline glue solution is dissolved with a cellulose thickener or a polyoxyethylene thickener, and the content is 2-7 wt%, preferably 2.5-5.5 wt%. Keeping for 30-60min after printing, cleaning, and drying.
The monomer of the PI film can be any one of binary anhydride and diamine.
Wherein the soluble metal salt solution in the step B is an aqueous solution of any water-soluble metal salt or a complex solution thereof, and the concentration of the soluble metal salt solution is 0.01-0.3M, preferably 0.05-0.25M; the time of ion exchange is 10-30min, preferably 12-25 min; and cleaning and drying after ion exchange.
Wherein, the reducing agent solution in the step C is dimethylamine borane (DMAB) or ascorbic acid, and the concentration of the dimethylamine borane is 0.01-0.2M, preferably 0.05-0.15M; the time for reducing treatment of the reducing agent solution is 5-30min, preferably 10-20 min; and cleaning and drying after reduction.
Wherein, the heat treatment procedure in the step E is that the temperature is raised to 140 ℃ at the speed of less than or equal to 3 ℃/min and then is kept for 1-2h at the normal temperature, and then the temperature is raised to 210 ℃ at the speed of less than or equal to 3 ℃/min and is kept for 1-3 h; the heating rate is preferably 0.5-2.8 deg.C/min.
Compared with the prior art, the method has the following technical characteristics and beneficial effects:
1. the method directly prints the strong alkaline glue solution pattern on the surface of the polyimide film, and has the advantages of simple preparation process, quick forming, less pollution, high utilization rate of the alkaline glue solution and lower cost.
2. The metal patterned polyimide film prepared by the method has the advantages of compact and uniform metal layer, excellent conductivity and excellent interface adhesion, and meets the actual application requirements.
3. The metal salt solution used by the method can be repeatedly used, has low cost and high utilization rate of metal ions, and is easy to popularize industrial production.
Drawings
FIG. 1: scanning Electron Microscope (SEM) photographs of the silver pattern on the surface of the film obtained in example 1 were magnified by 50K.
FIG. 2: scanning Electron Microscope (SEM) cross-sectional photographs of the silver pattern on the surface of the film obtained in example 1 were magnified 33K.
FIG. 3: a digital photograph of the silver pattern on the surface of the film obtained in example 1.
The specific implementation mode is as follows:
the invention is further described with reference to specific examples. It should be noted that the following examples are only for illustrating the present invention and are not to be construed as limiting the technical solutions described in the present invention, and all the technical solutions and modifications thereof which do not depart from the present invention should be covered within the scope of the claims of the present invention.
Example 1:
A. after the polyimide film of the PMDA-ODA system is cleaned by deionized water and ethanol, the polyimide film is subjected to plasma treatment, and the process of the plasma treatment comprises the following steps: the polyimide film is placed in a cavity of plasma processing equipment, the input voltage is 120V, the filament current is 200mA, the vacuum degree is 10Pa, the processing power is 160W, the processing gas is oxygen, and the processing time is 60 s. Printing a KOH solution with the concentration of 3M and the content of sodium carboxymethylcellulose (CMC) of 3 wt% prepared in advance on the surface of a PI film, keeping for 45min, cleaning and drying to obtain a polyimide film with a surface loaded with a modified pattern;
B. soaking the polyimide film with the surface loaded with the modified pattern obtained in the step A in 0.2M AgNO3Keeping the solution for 15min for ion exchange, taking out, cleaning and drying to obtain polyimide with silver ions loaded on the surfaceA film;
C. b, soaking the polyimide film loaded with silver ions on the surface obtained in the step B in 0.1M DMAB solution for 15min to reduce the silver ions on the surface, taking out, cleaning and drying to obtain the polyimide film loaded with silver patterns on the surface;
D. repeating the step B and the step C for 8 times to obtain a polyimide film with a silver metal pattern loaded on the surface;
E. and D, heating the polyimide film loaded with the thickened silver pattern on the surface obtained in the step D from the normal temperature to 135 ℃ at the speed of 2.5 ℃/min in the nitrogen atmosphere, keeping for 1.5h, heating to 200 ℃ at the speed of 2.5 ℃/min, and keeping for 2h to obtain the polyimide film loaded with the high-adhesion silver pattern on the surface.
Example 2:
A. after the polyimide film of the PMDA-ODA system is cleaned by deionized water and ethanol, the polyimide film is subjected to plasma treatment, and the process of the plasma treatment comprises the following steps: the polyimide film is placed in a cavity of plasma processing equipment, the input voltage is 120V, the filament current is 200mA, the vacuum degree is 10Pa, the processing power is 160W, the processing gas is oxygen, and the processing time is 60 s. Printing a KOH solution with the concentration of 5M and the content of sodium carboxymethylcellulose (CMC) of 3 wt% prepared in advance on the surface of a PI film, keeping for 45min, cleaning and drying to obtain a polyimide film with a surface loaded with a modified pattern;
B. soaking the polyimide film with the surface loaded with the modified pattern obtained in the step A in 0.2M silver ammonia solution for 15min for ion exchange, taking out, cleaning and drying to obtain the polyimide film with the surface loaded with silver ions;
C. b, soaking the polyimide film loaded with silver ions on the surface obtained in the step B in 0.1M DMAB solution for 15min to reduce the silver ions on the surface, taking out, cleaning and drying to obtain the polyimide film loaded with silver patterns on the surface;
D. repeating the step B and the step C for 8 times to obtain a polyimide film with a thickened silver pattern loaded on the surface;
E. and D, heating the polyimide film loaded with the thickened silver pattern on the surface obtained in the step D from the normal temperature to 135 ℃ at the speed of 2.5 ℃/min in the nitrogen atmosphere, keeping for 1.5h, heating to 200 ℃ at the speed of 2.5 ℃/min, and keeping for 2h to obtain the polyimide film loaded with the high-adhesion silver pattern on the surface.
Example 3:
A. after the polyimide film of the PMDA-ODA system is cleaned by deionized water and ethanol, the polyimide film is subjected to plasma treatment, and the process of the plasma treatment comprises the following steps: the polyimide film is placed in a cavity of plasma processing equipment, the input voltage is 120V, the filament current is 200mA, the vacuum degree is 10Pa, the processing power is 160W, the processing gas is oxygen, and the processing time is 60 s. Printing a KOH solution with the concentration of 5M and the content of sodium carboxymethylcellulose (CMC) of 3 wt% prepared in advance on the surface of a PI film, keeping for 45min, cleaning and drying to obtain a polyimide film with a surface loaded with a modified pattern;
B. soaking the polyimide film with the surface loaded with the modified pattern obtained in the step A in 0.2M AgNO3Keeping the solution for 10min for ion exchange, taking out, cleaning and drying to obtain a polyimide film with the surface loaded with silver ions;
C. b, soaking the polyimide film loaded with the silver ions on the surface, which is obtained in the step B, in 0.1M DMAB solution for 15min to reduce the silver ions on the surface, taking out the polyimide film, cleaning and drying the polyimide film to obtain the polyimide film loaded with the copper patterns on the surface;
D. repeating the step B and the step C for 8 times to obtain a polyimide film with a thickened silver pattern loaded on the surface;
E. and D, heating the polyimide film loaded with the thickened copper pattern on the surface obtained in the step D from the normal temperature to 135 ℃ at the speed of 2.5 ℃/min in the nitrogen atmosphere, keeping for 1.5h, heating to 200 ℃ at the speed of 2.5 ℃/min, and keeping for 2h to obtain the polyimide film loaded with the high-adhesion silver pattern on the surface.
Example 4:
A. after the polyimide film of the PMDA-ODA system is cleaned by deionized water and ethanol, the polyimide film is subjected to plasma treatment, and the process of the plasma treatment comprises the following steps: the polyimide film is placed in a cavity of plasma processing equipment, the input voltage is 120V, the filament current is 200mA, the vacuum degree is 10Pa, the processing power is 160W, the processing gas is oxygen, and the processing time is 60 s. Printing a KOH solution with the concentration of 5M and the content of sodium carboxymethylcellulose (CMC) of 5 wt% prepared in advance on the surface of a PI film, keeping for 45min, cleaning and drying to obtain a polyimide film with a surface loaded with a modified pattern;
B. soaking the polyimide film with the surface loaded with the modified pattern obtained in the step A in 0.2M AgNO3Keeping the solution for 10min for ion exchange, taking out, cleaning and drying to obtain a polyimide film with the surface loaded with silver ions;
C. b, soaking the polyimide film loaded with silver ions on the surface obtained in the step B in 0.1M DMAB solution for 15min to reduce the silver ions on the surface, taking out, cleaning and drying to obtain the polyimide film loaded with silver patterns on the surface;
D. repeating the step B and the step C for 8 times to obtain a polyimide film with a thickened silver pattern loaded on the surface;
E. and D, heating the polyimide film loaded with the thickened silver pattern on the surface obtained in the step D from the normal temperature to 135 ℃ at the speed of 2.5 ℃/min in the nitrogen atmosphere, keeping for 1.5h, heating to 200 ℃ at the speed of 2.5 ℃/min, and keeping for 2h to obtain the polyimide film loaded with the high-adhesion silver pattern on the surface.
Example 5:
A. after the polyimide film of the PMDA-ODA system is cleaned by deionized water and ethanol, the polyimide film is subjected to plasma treatment, and the process of the plasma treatment comprises the following steps: the polyimide film is placed in a cavity of plasma processing equipment, the input voltage is 120V, the filament current is 200mA, the vacuum degree is 10Pa, the processing power is 160W, the processing gas is oxygen, and the processing time is 60 s. Printing a KOH solution with the concentration of 5M and the content of sodium carboxymethylcellulose (CMC) of 5 wt% prepared in advance on the surface of a PI film, keeping for 45min, cleaning and drying to obtain a polyimide film with a surface loaded with a modified pattern;
B. modifying the surface load obtained in step ASoaking polyimide film of sexual pattern in 0.2M AgNO3Keeping the solution for 10min for ion exchange, taking out, cleaning and drying to obtain a polyimide film with the surface loaded with silver ions;
C. b, soaking the polyimide film loaded with silver ions on the surface obtained in the step B in 0.1M DMAB solution for 15min to reduce the silver ions on the surface, taking out, cleaning and drying to obtain the polyimide film loaded with silver patterns on the surface;
D. repeating the step B and the step C for 5 times to obtain a polyimide film with a thickened silver pattern loaded on the surface;
E. and D, heating the polyimide film loaded with the thickening copper pattern on the surface obtained in the step D from the normal temperature to 135 ℃ at the speed of 2.5 ℃/min in the nitrogen atmosphere, keeping for 2h, heating to 200 ℃ at the speed of 2.5 ℃/min, and keeping for 2h to obtain the polyimide film loaded with the high-adhesiveness copper pattern on the surface.
TABLE 1 Structure and Performance data for films of examples 1-5
Experimental method for adhesion: the test of the marking of paint films of GB9286-1998 paints and varnishes;
adhesion evaluation criteria:
level 0-smooth edge of the line, there is no paint to drop off at the edge and cross point of the line;
level 1-small pieces of paint fall off at the intersection of the lines, and the total area of fall off is less than 5%;
2, small pieces of paint fall off at the edge and the intersection of the scribing line, and the total falling area is between 5 and 15 percent;
level 3-a piece of paint falls off at the edge and the intersection of the line, and the total area of the falling off is between 15 and 35 percent;
4-a piece of paint falls off at the edge and the intersection of the line, and the total area of the falling off is between 35 and 65 percent;
grade 5-there is a patch of paint falling off at the edge and intersection of the scribe, and the total area of falling off is greater than 65%.
Claims (10)
1. A polyimide film with a surface covered with a metal pattern layer is characterized in that the thickness of the polyimide layer is 20-200 μm, and the thickness of the metal pattern layer is 100-800 nm.
2. The film as claimed in claim 1, wherein the metal of the metal pattern layer is silver, copper, etc.; the pattern shape of the metal pattern layer is any printable pattern.
3. The method for preparing the polyimide film with the surface covered with the metal pattern layer according to claim 1, which comprises the following steps:
A. carrying out plasma treatment on a Polyimide (PI) film, and printing strong alkaline glue solution on the surface of the polyimide film to obtain the polyimide film with a surface loaded with a modified pattern;
B. soaking the polyimide film with the surface loaded with the modified pattern obtained in the step A in a soluble metal salt solution for ion exchange to obtain a polyimide film with the surface loaded with metal ions;
C. soaking the polyimide film loaded with metal ions on the surface obtained in the step B in a reducing agent solution for reduction to obtain the polyimide film loaded with metal patterns on the surface;
D. and D, carrying out heat treatment on the polyimide film with the metal pattern loaded on the surface obtained in the step C in an inert atmosphere to obtain the polyimide film with the metal pattern loaded on the surface with high adhesiveness.
4. The method of claim 3, wherein steps B and C are repeated prior to the heat treatment to increase the thickness of the metal layer; the number of repetitions is preferably from 2 to 15.
5. The method according to claim 3, wherein the polyimide film is washed with deionized water and ethanol before the plasma treatment in step A.
6. The method as claimed in claim 3, wherein the concentration of the strongly alkaline glue solution is 2-8M, and the strongly alkaline solution is KOH, NaOH solution, etc.
7. The method of claim 6, wherein the strongly alkaline glue solution is dissolved with 2-7 wt% of cellulose thickener or polyoxyethylene thickener; keeping for 30-60min after printing.
8. The method of claim 3, wherein the soluble metal salt solution in step B is an aqueous solution of any one water-soluble metal salt or a complex solution thereof, and the concentration of the solution is 0.01-0.3M; the time of ion exchange is 10-30 min.
9. The process of claim 3, wherein the reducing agent solution in step C is dimethylamine borane (DMAB) or ascorbic acid at a concentration of 0.01 to 0.2M; the time for reducing treatment of the reducing agent solution is 5-30 min.
10. The method as defined in claim 3, wherein the heat treatment procedure in step E comprises raising the temperature at room temperature to 140 ℃ at a rate of 3 ℃/min or less, then maintaining the temperature for 1-2h, and then raising the temperature at a rate of 3 ℃/min or less to 190 ℃ at 210 ℃ for 1-3 h; the heating rate is preferably 0.5-2.8 deg.C/min.
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JP2007242689A (en) * | 2006-03-06 | 2007-09-20 | Sharp Corp | Metallic pattern forming method to polyimide surface and manufacturing method of polyimide wiring board having through-hole |
CN102108505A (en) * | 2010-11-01 | 2011-06-29 | 广西师范学院 | Method for directly depositing metal line patterns based on screen printing method |
CN103249255A (en) * | 2013-04-17 | 2013-08-14 | 复旦大学 | Method for directly preparing conducting circuit on resin baseplate |
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Title |
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