CN101338040B - Method for preparing porous conductive coating on plastic surface - Google Patents
Method for preparing porous conductive coating on plastic surface Download PDFInfo
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- CN101338040B CN101338040B CN2008100715969A CN200810071596A CN101338040B CN 101338040 B CN101338040 B CN 101338040B CN 2008100715969 A CN2008100715969 A CN 2008100715969A CN 200810071596 A CN200810071596 A CN 200810071596A CN 101338040 B CN101338040 B CN 101338040B
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- acetate
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- frosting
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Abstract
A method for preparing a porous conductive coating on a plastic surface relates to a method for plastic surface treatment, in particular to a preparation method for obtaining a layer of porous conductive coating on a plastic surface. The porous conductive coating can provide a good substrate for the conventional electroplating (galvanic plating) and ion plating and a method for preparing a porous conductive coating on a plastic surface. Resin is added in an organic solvent, is added with a dispersant and non solvent materials after dissolution, and is added with nano-conductive material particles and leveling agents to mix evenly and then nanometer modified polymer latex is prepared; the plastic surface is activated by sulphuric acid and acetic acid or sodium hydroxide after being cleaned and de-oiled, and is dried to reserve; the nanometer modified polymer latex is sprayed on the dried plastic surface to be dried and activated by the mixed acid of sulphuric acid, hydrochloric acid and acetic acid, namely, a layer of porous conductive coating is prepared on the plastic surface.
Description
Technical field
The present invention relates to the method that a kind of frosting is handled, especially relate to a kind of preparation method at frosting acquisition one deck porous conductive coating, this porous conductive coating can plate (water plating) for traditional electrical and vacuum plating provides a good base material.
Background technology
In short supply along with limited resources such as metallic substance replaces the demand of metal constantly to increase with plastics.Yet when utilizing the engineering plastics of difference in functionality, all be faced with an important difficult problem: how on plastic basis material, to form one deck tie coat, be connected base material and metal level, to guarantee good surface appearance and bonding force.
In order to plate the layer of metal layer at frosting, need handle frosting, the method that frosting commonly used is handled has: electroplate in (water plating) in tradition, adopt chemical roughen, sensitization, activation and electroless copper or nickel plating to handle frosting, its surface treatment method pollutes greatly, operation is many, and the plastics of handling are had selection.Zhao Yiyun utilizes ultrasonic wave amplitude according to ABS in publication number is the Chinese invention patent application of CN1157340, obtains porous surface structure.It is in the Japanese patent application of JP2006206933 that Japan's horizontal well goes out at publication number, when adopting injection moulding, add filler in ABS, reach etching ABS surface by a washing divinyl material (filler) then, forming a layer thickness is 10 μ m or littler porous layer.
More than 2 kinds of methods replace chemical roughens, but can only be of limited application, but also need carry out sensitization, activation and electroless copper at the ABS material.Wang Guixiang (Wang Guixiang, Han Jiajun, Li Ning, Li Deyu. Direct Electroplating on Plastics Surface [J], electroplate and finish, 2005,27 (2) 20～23) " Direct Electroplating on Plastics Surface ", Atotech company (Middeke H J.Plating on plastics partV-direct plating[J], electroplate and covering with paint, 2005,24 (5) 32～37.) the absorption carbon black obtained conductive layer after Futuron technology and U.S. human relations doffer (seeing patent RE37765) utilized alligatoring, more than these methods, all need chemical roughen technology, itself do not make frosting form porous coating, obtain vesicular structure but rely on chemical roughen, to guarantee bonding force.
There are many utilizations to be coated with electrically conducting coating both at home and abroad and carry out Direct Electroplating, people such as Guo Zhongcheng in 2007 utilize in publication number is the Chinese patent application of CN1944718 conductive silver, copper are added in acrylic resin, the Resins, epoxy, the electrically conducting coating of preparation is coated on the non-metallic substrate surface, thereby the acquisition conductive layer carries out electro-coppering, nickel, chromium then.Xu Jin was in the Chinese patent application of CN1080670 at publication number entirely in 1992, applied one deck anticorrosive adhesive earlier on on-metallic article, was coated with conductive layer again, carried out electro-coppering then.Japanese slope Ben Jiahong was in the Chinese patent application of CN1109924 at publication number in 1994, utilized binding agent that conductive carbon black is sticked to the plastic basis material surface, carried out electro-coppering then.More than these methods, the bonding force that all lacks between and the electroplated metal layer guarantees, all is to attract by hydrogen bond, does not form chemical bond or the physics anchor closes, this all influences the bonding force of whole plated film.
Vacuum plating is by sputter or evaporation coating direct deposition layer of metal layer on plastic basis material, but its bonding force needs plasma etching to guarantee, its suitability is limited, can only be at several thermoplasticss, and can not repair the defective of base material.
Summary of the invention
The objective of the invention is to deficiency, a kind of method for preparing porous conductive coating at frosting is provided at above-mentioned prior art existence.
The present invention includes following steps:
1) resin is added in the organic solvent, the dissolving back adds dispersion agent and non-solvent class material, adds nanometer conductive material particle and flow agent again, makes nano modification polymer (being called for short SNP) emulsion after mixing;
2) frosting is cleaned oil removing after, with sulfuric acid and acetate, or sodium hydroxide activates, the oven dry back is standby;
3) the nano modification macromolecule emulsion with step 1) preparation is sprayed on step 2) on the frosting after the oven dry, the oven dry back activates with the nitration mixture of sulfuric acid, hydrochloric acid and acetate, promptly prepares one deck porous conductive coating on frosting.
Resin can be ABS, polystyrene, polycarbonate, polyvinyl chloride, at least a in the acrylic resin etc.Organic solvent can be at least a in ethyl acetate, butylacetate, pentyl acetate, acetone, tetrahydrofuran (THF), butanone (MEK), heptanone, N-N-methyl-2-2-pyrrolidone N-, 2-Butoxyethyl acetate, 1-Methoxy-2-propyl acetate and the isophorone etc.Dispersion agent can be at least a in cetyl trimethylammonium bromide, fluorine octyl group sulphonyl (fluorocarbon surfactant), polyvinylpyrrolidone, the polymine etc.Non-solvent class material can be at least a in water, ethanol, propyl alcohol, the butanols etc.The nanometer conductive material particle can be at least a in nanometer silver, nanometer copper, carbon nanotube, nanometer carbon black, nanometer nickel, the ITO particles such as (nano indium tin metal oxides).Flow agent can be a kind of in silane coupling agent that polydimethylsiloxane, model are KH560, polyether modified silicon oil etc.Press mass ratio, the content of each raw material is organic solvent: non-solvent class material: portions of resin nanometer conductive material particle: dispersion agent: flow agent=1: (0.1～0.01): (0.4～0.1): (0.2～0.01): (0.01～0.001): (0.01～0.001).
In step 2) in, vitriolic concentration is preferably 1～6mol/L, acetate is preferably pure acetate, by volume, best sulfuric acid: acetate=4: 1, concentration sodium hydroxide is preferably 8～15mol/L, and the activatory time is preferably 1～10min, the temperature of oven dry is preferably 50 ℃, and the time of oven dry is preferably 20min.
In step 3), the temperature of oven dry is preferably 70～90 ℃, the time of oven dry is preferably 30～60min, vitriolic concentration is preferably 1mol/L, and the concentration of hydrochloric acid is preferably 1mol/L, the best pure acetate of acetate, by volume, the proportioning of sulfuric acid, hydrochloric acid and acetate is preferably sulfuric acid: hydrochloric acid: acetate=2: 1: 3, the activatory time is preferably 1～5min, is generally 5～20 μ m at the thickness of the prepared porous conductive coating of frosting.
The present invention adopts organic solvent, the dissolving macromolecule resin, obtain organic polymer solution, then to wherein adding dispersion agent and non-solvent class material, add the nanometer conductive material particle again, flow agent, generate one deck function film with the template construction from part, this layer film has other physicalies such as nano aperture structure and metallicity conductivity, can obtain regular nanometer micropore by preparation porous conductive coating on engineering plastic, simultaneously when follow-up plasma surface modification, can introduce active function groups easily, thereby improve the bonding force between modified layer and engineering plastic substrate surface and the subsequent deposition layer.This modified layer also possesses electroconductibility, thereby provides assurance for the structural controllability of subsequent deposition layer.Can make plastic part be applied to tradition by this technology and electroplate fields such as (water) and vacuum plating.The present invention has also widened the use range of engineering plastic material in addition.
The present invention adopts and is painted on frosting, has simplified traditional plating (water plating) technology, makes it save operations such as alligatoring, sensitization, electroless copper, has shortened flow process, has improved efficient, has reduced pollution; Also for vacuum plating provides one deck tie coat, the range of application of vacuum plating is enlarged simultaneously, satisfied multifarious requirement, also provide the foundation simultaneously for vacuum plating obtains specular appearance.
This shows, the present invention not only make engineering plastic surface have the nano aperture structure (100～2000nm) and the metallicity conductivity, and the coating by vesicular structure, the mechanical anchor that increases between porous layer and the metal level closes, and promotes bonding force.In addition, by conductivity, operations such as the alligatoring of energy substituted chemistry, sensitization, activation and electroless copper are simplified technology, reduce and pollute.Have the levelling leveling ability owing to coating simultaneously, the tiny defective in energy repairing plastic surface, thus be that vacuum plating obtains a good surface appearance and bonding force.
Embodiment
Embodiment 1: electroplate (water plating) sour copper on the ABS goods
Organic solvent (adopt acetoneand ethyl acetate, by volume, acetone: ethyl acetate=10: 1) be 45g;
Non-solvent material (water) is 2g;
Resin (ABS) is 2.5g;
Conductive particle (nanometer silver and nanometer copper, mass ratio 2: 1) is 4g;
Flow agent (polydimethylsiloxane) is 0.1g;
Dispersion agent (polyvinylpyrrolidone) is 0.1g.
Disperse, mix with magnetic stirrer according to the above-mentioned raw materials ratio, be mixed with the nano modification macromolecule emulsion, the electroplating technology flow process is: ABS workpiece, electrochemical deoiling, diluted acid (dilute sulphuric acid of 3mol/L and pure acetate is (4: 1) by volume) activation 5min, 50 ℃ of oven dry 20min, dipping nano modification macromolecule emulsion, 70 ℃ of oven dry 30min, nitration mixture activation 5min, the washing secondary, electroplating acid copper 30min.
Embodiment 2: go up PVD copper facing at unsaturated polyester (BMC)
Organic solvent (adopt ethyl acetate, butanone and N-N-methyl-2-2-pyrrolidone N-, by volume, ethyl acetate: butanone: N-N-methyl-2-2-pyrrolidone N-=10: 1: 1) be 45g;
Non-solvent material (ethanol) is 5g;
(ABS and acrylic resin are pressed mass ratio to resin, ABS: acrylic resin=10: 1) be 6g;
(nanometer silver and nanometer copper are pressed mass ratio, nanometer silver: nanometer copper=1: 3) be 5g to conductive particle;
Flow agent (polyether modified silicon oil and KH560 silane coupling agent, volume ratio is: 1: 1) is 0.1g;
Dispersion agent (polymine) is 0.1g;
Disperse, mix with magnetic stirrer according to the above-mentioned raw materials ratio, be mixed with nano modification polymer (SNP) emulsion, the technique for vacuum coating flow process is: BMC workpiece, electrochemical deoiling, highly basic activation 10min, 50 ℃ of oven dry 20min, spraying nano modification macromolecule emulsion, 90 ℃ of oven dry 30min, nitration mixture activation 5min, washing, 50 ℃ of oven dry 20min, the copper facing of PVD vacuum.
Embodiment 3: electroplate (water plating) nickel at nylon PA6
Organic solvent (adopt butylacetate, heptanone and N-N-methyl-2-2-pyrrolidone N-, by volume, butylacetate: heptanone: N-N-methyl-2-2-pyrrolidone N-=10: 1: 1) be 45g;
Non-solvent class material (water) is 1g;
(ABS and acrylic resin are pressed mass ratio to resin, ABS: acrylic resin=3: 0.2) be 3g;
(nanometer silver and carbon nanotube are pressed mass ratio to conductive particle, nanometer silver: carbon nanotube=2: 1) be 3g;
Flow agent (polyether modified silicon oil) is 0.1g;
Dispersion agent (polymine) is 0.1g.
Disperse, mix with magnetic stirrer according to the above-mentioned raw materials ratio, be mixed with nano modification polymer (SNP) emulsion, the electroplating technology flow process is: nylon workpiece, electrochemical deoiling, diluted acid (dilute sulphuric acid of 6mol/L and pure acetate is (4: 1) by volume) activation 5min, 50 ℃ of oven dry 20min, spraying nano modification macromolecule emulsion, 70 ℃ of oven dry, nitration mixture activation 5min, washing is electroplated sour ketone, electronickelling.
Embodiment 4: electroplate (water plating) nickel (PBT) at polybutylene terephthalate
Organic solvent (adopt acetone, butylacetate, tetrahydrofuran (THF), by volume, acetone: butylacetate: tetrahydrofuran (THF)=5: 1: 8) be 45g;
Non-solvent class material (water) is 2g;
Resin (ABS and polycarbonate, mass ratio is: 5: 1) is 2.5g;
Conductive particle (nanometer silver and nanometer carbon black, mass ratio is: 4: 1) is 2g;
Flow agent (polydimethylsiloxane) is 0.1g;
Dispersion agent (polymine) is 0.1g.
Disperse, mix with magnetic stirrer according to the above-mentioned raw materials ratio, be mixed with nano modification polymer (SNP) emulsion, the electroplating technology flow process is: PBT workpiece, electrochemical deoiling, diluted acid (dilute sulphuric acid of 6mol/L and pure acetate is (4: 1) by volume) activation 5min, 50 ℃ of oven dry 20min, spraying nano modification macromolecule emulsion, 70 ℃ of oven dry, nitration mixture activation 5min, washing, electroplating acid copper, electronickelling
Embodiment 5: polyvinyl chloride PVD chromium plating
Organic solvent (adopt pentyl acetate, butanone and 2-Butoxyethyl acetate, volume ratio is 5: 5: 1) is 45g;
Non-solvent class material: propyl alcohol, 2g
Resin: polyvinyl chloride, 4g
Nanometer conductive material particle: nanometer carbon black, carbon nanotube, mass ratio 2: 1,4g
Flow agent: polydimethylsiloxane
Dispersion agent: cetyl trimethylammonium bromide and polyvinylpyrrolidone
Disperse, mix with magnetic stirrer according to the above-mentioned raw materials ratio, be mixed with nano modification polymer (SNP) emulsion, the electroplating technology flow process is: polyvinyl chloride workpiece, electrochemical deoiling, diluted acid (dilute sulphuric acid of 6mol/L and pure acetate is (4: 1) by volume) activation 5min, 50 ℃ of oven dry 20min, spraying nano modification macromolecule emulsion, 70 ℃ of oven dry, nitration mixture activation 5min, washing, vacuum copper facing, vacuum chromium-coated.
Embodiment 6: the copper facing of polystyrene vacuum
Organic solvent (adopt butylacetate, butanone and 1-Methoxy-2-propyl acetate and isophorone, by volume, butylacetate: butanone: 1-Methoxy-2-propyl acetate: isophorone=10: 1: 1: 0.4) be 45g;
Non-solvent class material (butanols) is 1.5g;
(ABS and polystyrene are pressed mass ratio to resin, ABS: polystyrene=1: 1) be 3g;
(nanometer silver and nanometer nickel are pressed mass ratio, nanometer silver: nanometer nickel=4: 1) be 3g to conductive particle;
Flow agent (polyether modified silicon oil) is 0.1g;
Dispersion agent (polymine and fluorine octyl group sulphonyl, volume ratio is 1: 1) is 0.1g.
Disperse, mix with magnetic stirrer according to the above-mentioned raw materials ratio, be mixed with nano modification polymer (SNP) emulsion, the electroplating technology flow process is: polystyrene workpiece, electrochemical deoiling, diluted acid (dilute sulphuric acid of 6mol/L and pure acetate is (4: 1) by volume) activation 5min, 50 ℃ of oven dry 20min, spraying nano modification macromolecule emulsion, 90 ℃ of oven dry, nitration mixture activation 5min, washing, 50 ℃ of oven dry 20min, vacuum copper facing.
Claims (9)
1. one kind prepares the method for porous conductive coating at frosting, it is characterized in that may further comprise the steps:
1) resin is added in the organic solvent, the dissolving back adds dispersion agent and non-solvent class material, add nanometer conductive material particle and flow agent again, make the nano modification macromolecule emulsion after mixing, described non-solvent class material is selected from least a in water, ethanol, propyl alcohol, the butanols, press mass ratio, the content of each raw material is organic solvent: non-solvent class material: portions of resin nanometer conductive material particle: dispersion agent: flow agent=1: (0.1～0.01): (0.4～0.1): (0.2～0.01): (0.01～0.001): (0.01～0.001);
2) frosting is cleaned oil removing after, with sulfuric acid and acetate, or sodium hydroxide activates, the oven dry back is standby;
3) the nano modification macromolecule emulsion with step 1) preparation is sprayed on step 2) on the frosting after the oven dry, the oven dry back activates with the nitration mixture of sulfuric acid, hydrochloric acid and acetate, promptly prepares one deck porous conductive coating on frosting.
2. as claimed in claim 1ly a kind ofly prepare the method for porous conductive coating, it is characterized in that resin is selected from ABS, polystyrene, polycarbonate, polyvinyl chloride, at least a in the acrylic resin at frosting; Organic solvent is selected from least a in ethyl acetate, butylacetate, pentyl acetate, acetone, tetrahydrofuran (THF), butanone, heptanone, N-N-methyl-2-2-pyrrolidone N-, 2-Butoxyethyl acetate, 1-Methoxy-2-propyl acetate and the isophorone.
3. as claimed in claim 1ly a kind ofly prepare the method for porous conductive coating, it is characterized in that dispersion agent is selected from least a in cetyl trimethylammonium bromide, fluorine octyl group sulphonyl, polyvinylpyrrolidone, the polymine at frosting.
4. as claimed in claim 1ly a kind ofly prepare the method for porous conductive coating, it is characterized in that the nanometer conductive material particle is selected from least a in nanometer silver, nanometer copper, carbon nanotube, nanometer carbon black, nanometer nickel, the nano indium tin metal oxide particle at frosting.
5. as claimed in claim 1ly a kind ofly prepare the method for porous conductive coating, it is characterized in that flow agent is selected from a kind of in silane coupling agent that polydimethylsiloxane, model are KH560, the polyether modified silicon oil at frosting.
6. as claimed in claim 1ly a kind ofly prepare the method for porous conductive coating, it is characterized in that in step 2 at frosting) in, vitriolic concentration is 1～6mol/L, acetate is pure acetate, by volume, sulfuric acid: acetate=4: 1; Concentration sodium hydroxide is 8～15mol/L.
7. as claimed in claim 1ly a kind ofly prepare the method for porous conductive coating, it is characterized in that in step 2 at frosting) in, the activatory time is 1～10min, and the temperature of oven dry is 50 ℃, and the time of oven dry is 20min.
8. as claimed in claim 1ly a kind ofly prepare the method for porous conductive coating at frosting, it is characterized in that in step 3) the temperature of oven dry is 70～90 ℃, the time of oven dry is 30～60min.
9. a kind of method for preparing porous conductive coating at frosting as claimed in claim 1, it is characterized in that in step 3), vitriolic concentration is 1mol/L, the concentration of hydrochloric acid is 1mol/L, the pure acetate of acetate, by volume, the proportioning of sulfuric acid, hydrochloric acid and acetate is a sulfuric acid: hydrochloric acid: acetate=2: 1: 3, the activatory time is 1～5min.
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| CN2008100715969A CN101338040B (en) | 2008-08-15 | 2008-08-15 | Method for preparing porous conductive coating on plastic surface |
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| CN2008100715969A CN101338040B (en) | 2008-08-15 | 2008-08-15 | Method for preparing porous conductive coating on plastic surface |
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| CN101338040B true CN101338040B (en) | 2011-01-19 |
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102392234A (en) * | 2011-10-17 | 2012-03-28 | 哈尔滨工程大学 | Chemical plating or electro -brush plating pretreatment method for organic non-conducting base material and resin base conductive paint |
| CN102702892A (en) * | 2012-06-14 | 2012-10-03 | 天长市银狐漆业有限公司 | Conducting paint composition and preparation method thereof |
| CN102886894B (en) * | 2012-10-19 | 2015-02-25 | 南宁燎旺车灯有限责任公司 | Method for homogenizing surface of plastic piece by atomization method |
| CN107459667A (en) * | 2017-08-16 | 2017-12-12 | 孝感双华应用科技开发有限公司 | A kind of environmentally friendly film plating process of polyvinyl chloride |
| CN109056020A (en) * | 2018-10-29 | 2018-12-21 | 上海芮远化学科技有限公司 | A kind of method for metallising and electro-plating method of plastic workpiece |
| CN110093645A (en) * | 2019-05-31 | 2019-08-06 | 厦门大学 | Plastic electroplating method |
| CN110551307B (en) * | 2019-08-07 | 2022-04-19 | 湖南松井新材料股份有限公司 | Polishing agent for plastic and method for forming uniform rough surface on plastic surface |
| CN114437603B (en) * | 2022-03-10 | 2023-03-24 | 山东鑫纳超疏新材料有限公司 | Preparation method of durable super-hydrophobic micro-droplet self-cleaning coating based on conductive nanoparticles |
| CN115820039A (en) * | 2022-12-28 | 2023-03-21 | 厦门大学 | Porous conductive ink, preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1103074A (en) * | 1993-09-09 | 1995-05-31 | 通用电气公司 | Synthetic resin sheet comprising a conductive carbon black-containing coating layer |
| CN101036423A (en) * | 2004-08-26 | 2007-09-12 | 富士胶片株式会社 | Method for producing conductive pattern material |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1103074A (en) * | 1993-09-09 | 1995-05-31 | 通用电气公司 | Synthetic resin sheet comprising a conductive carbon black-containing coating layer |
| CN101036423A (en) * | 2004-08-26 | 2007-09-12 | 富士胶片株式会社 | Method for producing conductive pattern material |
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Address after: 361000 Tianfeng Road, Jimei District, Xiamen, Fujian Province, No. 69 Patentee after: Runner (Xiamen) Corp. Address before: 361023 Dongting Road 155-159, Guankou Town, Jimei District, Xiamen City, Fujian Province Patentee before: Xiamen Runner Industrial Corp. |
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