CN1912190A - Method for conduction high polymer pattern sedimentation on surface of plastic - Google Patents
Method for conduction high polymer pattern sedimentation on surface of plastic Download PDFInfo
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- CN1912190A CN1912190A CN 200610086146 CN200610086146A CN1912190A CN 1912190 A CN1912190 A CN 1912190A CN 200610086146 CN200610086146 CN 200610086146 CN 200610086146 A CN200610086146 A CN 200610086146A CN 1912190 A CN1912190 A CN 1912190A
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Abstract
The invention relates to a pattering deposition method conducting high polymer on plastic surface. It combines selectivity photochemistry decorating and selectivity area chemical plating to make metal electrode on the plastic surface, adopts electrochemical oxidation to realize pattering deposition of the conducing high polymer on the metal electrode. This can effectively remove residue reagent, improve sample performance, avoid a great number of acid waste water discharging to protect the environment, and ensure the security of the operator.
Description
Technical field
The present invention relates to a kind of treatment process of superpolymer, refer in particular to the method for a kind of conduction high polymer at the frosting pattern sedimentation.
Background technology
In recent years, extensively carrying out and deepen continuously along with conduction high polymer research, the interest of research is not concentrating on problems such as the preparation technology of conduction high polymer, electrical conduction mechanism, workability yet, but turn to cheap, can disposable plastics or papery electrical equipment (as mobile phone, plastic chip etc.).With the exception of this, the conduction high polymer figure equivalence of definite shape is corresponding to a certain specific circuit, can produce response to the hertzian wave of certain frequency, therefore can be used for the field such as false proof of the antitheft and product of supermarket commodity.
The MacDiarmid professor research group of Univ Pennsylvania USA has invented a kind of employing laser printer the bargraphs that computer aided design software (CAD) designs has been printed on the transparent film, method with in-situ polymerization is deposited on polypyrrole on the film then, utilize solvability difference, in toluene, wash with the part of ultrasonic wave with printing ink powder, obtain the conductive pattern that reverses, be called LP (line patterning) method.This is to utilize the conduction high polymer characteristic to carry out the trial first of pattern sedimentation.
But, this method is owing to used chemical oxidization method to prepare polypyrrole, used oxygenant remains in the performance that influences sample in the sample easily, also has a large amount of acid waste water dischargings in addition, cause environmental pollution, and the toluene that is used for dissolving printing ink powder is the very big organic solvent of volatile toxicity.
Summary of the invention
The purpose of this invention is to provide a kind of environmental friendliness, realize the method for conduction high polymer at the frosting pattern sedimentation with electrochemical oxidation process.
The invention provides the method for conduction high polymer, it is characterized in that at the frosting pattern sedimentation:
(1) by the electroless plating of selective light chemically modified, prepares metal electrode at frosting in conjunction with selective area.
(2) adopt electrochemical oxidation process, on the metal electrode that frosting forms, realize the pattern sedimentation of conduction high polymer.
Concrete steps are:
(1) is photomask with quartz/chromium plate, as light source the patterned area of frosting carried out irradiation with UV-light;
(2) the irradiated plastic sheet of accepting figure transfer is immersed in the 0.3-0.8mol/L ethylenediamine solution, with 0.4-0.6mol/L 1-[3 '-(N, the N-dimethyl amido) propyl group]-the 3-ethyl-carbodiimide hydrochloride is a coupler, reacts 2.5-4 hour, clean up with distilled water;
(3) will in the plastic sheet immersion 1-3mmol/L of (2) reaction chlorauric acid solution, react 2-4 hour, after water cleans, again with reaction in its immersion 0.1-0.3mol/L sodium borohydride solution 5-10 minute.
(4) will after the plastic sheet water flushing of (3) reaction, immerse in the 0.2-0.5mol/L potassium bisulfide solution ultrasonic cleaning 30-60 minute.
(5) with after the flushing of the plastic sheet water after the ultrasonic cleaning, be immersed in the chemical plating fluid, reacted 30-60 minute down, just can form even, fine and closely woven thin au electrode, clean, dry up in specific selection zone in 45-50 ℃.Wherein, take corresponding chemical plating fluid according to different precious metals or transition metal electrodes such as preparation gold, copper, nickel, platinum, palladium, silver.
(6) metal electrode on the plastic sheet is immersed in the monomer solution of conduction high polymer, doping agent is a 0.5-0.8mol/L hydrochloric acid.Under 0.8 ± 0.1V current potential, adopt the potentiostatic method synthesized polyaniline; Perhaps in the potential range of-0.3-1.2V, adopt cyclic voltammetry compositing conducting superpolymer, thereby on the metal electrode on the plastic sheet, realize the pattern sedimentation of conduction high polymer.
Of the present inventionly be used to realize that the plastics of conduction high polymer pattern sedimentation can be the thermoplastic macromolecule materials to specific wavelength UV-light sensitivity such as polycarbonate (PC), polyethylene terephthalate (PET), polymethylmethacrylate (PMMA).
The metal electrode that forms at frosting of the present invention can be precious metal or transition metal materials such as gold, copper, nickel, platinum, palladium, silver.Be that chemical plating fluid is the salt that contains corresponding precious metal or cross metallizing, the solution of complexing agent and reductive agent.
Conduction high polymer of the present invention can be conduction high polymers such as polyaniline, polypyrrole, Polythiophene, poly-thionine, poly-pyrocatechol, poly-phenylene vinylene (ppv) (PPV), poly-Ortho Toluidine, poly-phenylaniline.
Because the present invention adopts electrochemical oxidation process to realize the pattern sedimentation of conduction high polymer at frosting; avoided the use of chemical oxidizing agent; thereby effectively eliminated the residual of reagent; improved the performance of sample; and the amount of electrochemical oxidation process consumption reagent seldom; this just can be avoided the discharging of a large amount of acid waste waters, has protected surrounding environment.Simultaneously, compare with the LP method, the present invention need not use the very big organic solvent toluene of toxicity in the process of frosting pattern sedimentation conduction high polymer, thereby has further guaranteed operator's safety.
Embodiment
With pattern sedimentation conduction high polymer-polyaniline on polycarbonate (PC) sheet is embodiment 1, of the present invention on the PC sheet method of pattern sedimentation polyaniline, the steps include:
A, usefulness low pressure mercury lamp are as light source, and quartz/chromium plate is made mask, and irradiation is carried out in the selection zone on PC sheet surface.When other frosting such as PET, PMMA is realized the pattern sedimentation of conduction high polymer, as long as change plastic material into corresponding PET, PMMA.
B, irradiated PC sheet is put into 0.4mol/L quadrol-0.4mol/L 1-[3 '-(N, N-dimethyl amido) propyl group]-3-ethyl-carbodiimide hydrochloride (coupler) solution in reaction 3 hours, clean up with distilled water.
C, will immerse in the 1mmol/L chlorauric acid solution reaction through the PC sheet of (B) reaction 2 hours, after water cleans, again it be immersed in the 0.1mol/L sodium borohydride solution reaction 5 minutes.
D, will after the PC sheet water flushing of (C) reaction, immerse in the 0.2mol/L potassium bisulfide solution ultrasonic cleaning 30 minutes.
E, with after the PC sheet water after the ultrasonic cleaning flushing, be immersed in the chemical gold plating liquid (8mmol/L gold sodium sulfide, 0.125mol/L S-WAT and 0.6mol/L formaldehyde), reacted 30 minutes down in 45-50 ℃, just can form even, fine and closely woven thin au electrode in specific selection zone, clean, dry up.
F, the metal electrode on the PC sheet immersed contain in the solution of 0.2mol/L aniline monomer, doping agent is a 0.5-0.8mol/L hydrochloric acid, under the 0.75V current potential, adopt the potentiostatic method synthesized polyaniline, perhaps in the potential range of-0.1-0.8V, adopt the cyclic voltammetry synthesized polyaniline, just can realize the pattern sedimentation of polyaniline on the POLYCARBONATE SHEET surface.When doped sulfuric acid radical ion or phosphate anion, as long as doping agent is changed into sulfuric acid or the 0.4-0.7mol/L phosphoric acid of 0.3-0.5mol/L.
With pattern sedimentation conduction high polymer-polypyrrole on polycarbonate (PC) sheet is embodiment 2, of the present invention on the PC sheet method of pattern sedimentation polypyrrole, the steps include:
A, usefulness low pressure mercury lamp are as light source, and quartz/chromium plate is made mask, and irradiation is carried out in the selection zone on PC sheet surface.When other frosting such as PET, PMMA is realized the pattern sedimentation of conduction high polymer, as long as change plastic material into corresponding PET, PMMA.
B, irradiated PC sheet is put into 0.8mol/L quadrol-0.6mol/L 1-[3 '-(N, N-dimethyl amido) propyl group]-3-ethyl-carbodiimide hydrochloride (coupler) solution in reaction 3 hours, clean up with distilled water.
C, will immerse in the 3mmol/L chlorauric acid solution reaction through the PC sheet of (B) reaction 4 hours, after water cleans, again it be immersed in the 0.3mol/L sodium borohydride solution reaction 10 minutes.
D, will after the PC sheet water flushing of (C) reaction, immerse in the 0.5mol/L potassium bisulfide solution ultrasonic cleaning 60 minutes.
E, with after the PC sheet water after the ultrasonic cleaning flushing, be immersed in chemical bronze plating liquid (5 gm/litre copper sulphate, 25 grams per liter unresolvable tartaric acid potassium sodium, 7 grams per liter sodium hydroxide, 10ml formaldehyde) in, reacted 60 minutes down, just can form even, fine and closely woven thin au electrode in specific selection zone in 45-50 ℃, clean, dry up.
F, the metal electrode on the PC sheet immersed contain in the solution of 0.1mol/L pyrrole monomer, doping agent is a 0.5-0.8mol/L hydrochloric acid.In the potential range of 0-1.2V, adopt the synthetic polypyrrole of cyclic voltammetry, just can realize the pattern sedimentation of polypyrrole on the POLYCARBONATE SHEET surface.When doped sulfuric acid radical ion or phosphate anion, as long as doping agent is changed into sulfuric acid or the 0.4-0.7mol/L phosphoric acid of 0.3-0.5mol/L.
With pattern sedimentation conduction high polymer on polycarbonate (PC) sheet-poly-thionine is embodiment 3, and the method that pattern sedimentation gathers thionine on the PC sheet of the present invention the steps include:
A, usefulness low pressure mercury lamp are as light source, and quartz/chromium plate is made mask, and irradiation is carried out in the selection zone on PC sheet surface.When other frosting such as PET, PMMA is realized the pattern sedimentation of conduction high polymer, as long as change plastic material into corresponding PET, PMMA.
B, irradiated PC sheet is put into 0.6mol/L quadrol-0.5mol/L 1-[3 '-(N, N-dimethyl amido) propyl group]-3-ethyl-carbodiimide hydrochloride (coupler) solution in reaction 3 hours, clean up with distilled water.
C, will immerse in the 2mmol/L chlorauric acid solution reaction through the PC sheet of (B) reaction 3 hours, after water cleans, again it be immersed in the 0.2mol/L sodium borohydride solution reaction 8 minutes.
D, will after the PC sheet water flushing of (C) reaction, immerse in the 0.4mol/L potassium bisulfide solution ultrasonic cleaning 45 minutes.
E, with after the PC sheet water after the ultrasonic cleaning flushing, be immersed in chemical palladium plating solution (10 grams per liter palladium chlorides, 19 grams per liter disodium ethylene diamine tetraacetate, 25.6 grams per liter quadrol, 4.1 the grams per liter sodium hypophosphite), reacted 45 minutes down, just can form even, fine and closely woven thin au electrode in specific selection zone in 45-50 ℃, clean, dry up.When precious metal such as preparation copper, nickel, platinum, palladium, silver or transition metal electrode, as long as change chemical plating fluid into the corresponding metal plating bath.
F, the metal electrode on the PC sheet immersed contain in the monomeric solution of 4mmol/L thionine, doping agent is a 0.5-0.8mol/L hydrochloric acid.In the potential range of-0.3-1.2V, adopt the synthetic poly-thionine of cyclic voltammetry, just can realize gathering the pattern sedimentation of thionine on the POLYCARBONATE SHEET surface.When doped sulfuric acid radical ion or phosphate anion, as long as doping agent is changed into sulfuric acid or the 0.4-0.7mol/L phosphoric acid of 0.3-0.5mol/L.
With pattern sedimentation conduction high polymer on polycarbonate (PC) sheet-poly-pyrocatechol is embodiment 4, and the method that pattern sedimentation gathers pyrocatechol on the PC sheet of the present invention the steps include:
A, usefulness low pressure mercury lamp are as light source, and quartz/chromium plate is made mask, and irradiation is carried out in the selection zone on PC sheet surface.When other frosting such as PET, PMMA is realized the pattern sedimentation of conduction high polymer, as long as change plastic material into corresponding PET, PMMA.
B, irradiated PC sheet is put into 0.6mol/L quadrol-0.5mol/L 1-[3 '-(N, N-dimethyl amido) propyl group]-3-ethyl-carbodiimide hydrochloride (coupler) solution in reaction 3 hours, clean up with distilled water.
C, will immerse in the 2mmol/L chlorauric acid solution reaction through the PC sheet of (B) reaction 3 hours, after water cleans, again it be immersed in the 0.2mol/L sodium borohydride solution reaction 8 minutes.
D, will after the PC sheet water flushing of (C) reaction, immerse in the 0.4mol/L potassium bisulfide solution ultrasonic cleaning 45 minutes.
E, with after the PC sheet water after the ultrasonic cleaning flushing, be immersed in chemical plating liquid (Silver Nitrate 1～2 grams per liter, N-methyl p-aminophenol sulfate 5～10 grams per liters, citric acid 20～100 grams per liters) in, reacted 45 minutes down in 45-50 ℃, just can form even, fine and closely woven thin au electrode, clean, dry up in specific selection zone.When precious metal such as preparation copper, nickel, platinum, palladium, silver or transition metal electrode, as long as change chemical plating fluid into the corresponding metal plating bath.
F, the metal electrode on the PC sheet immersed contain in the monomeric solution of 0.2mol/L pyrocatechol, doping agent is a 0.5-0.8mol/L hydrochloric acid.In the potential range of-0.2-1.1V, adopt the synthetic poly-pyrocatechol of cyclic voltammetry, just can realize gathering the pattern sedimentation of pyrocatechol on the POLYCARBONATE SHEET surface.When doped sulfuric acid radical ion or phosphate anion, as long as doping agent is changed into sulfuric acid or the 0.4-0.7mol/L phosphoric acid of 0.3-0.5mol/L.
Claims (5)
1. conduction high polymer is characterized in that preparing metal electrode by the electroless plating of selective light chemically modified in conjunction with selective area at the thermal plastic high polymer frosting to specific wavelength UV-light sensitivity in the method for frosting pattern sedimentation; Adopt electrochemical oxidation process then, on the metal electrode that frosting forms, realize pattern sedimentation conduction high polymer.
2, conduction high polymer according to claim 1 is characterized in that in the method for frosting pattern sedimentation
(1) is photomask with quartz/chromium plate, as light source the patterned area of frosting carried out irradiation with UV-light;
(2) the irradiated plastic sheet of accepting figure transfer is immersed in the 0.3-0.8mol/L ethylenediamine solution, with 0.4-0.6mol/L 1-[3 '-(N, the N-dimethyl amido) propyl group]-the 3-ethyl-carbodiimide hydrochloride is a coupler, reacts 2.5-4 hour, clean up with distilled water;
(3) will in the plastic sheet immersion 1-3mmol/L of (2) reaction chlorauric acid solution, react 2-4 hour, after water cleans, again with reaction in its immersion 0.1-0.3mol/L sodium borohydride solution 5-10 minute;
(4) will after the plastic sheet water flushing of (3) reaction, immerse in the 0.2-0.5mol/L potassium bisulfide solution ultrasonic cleaning 30-60 minute;
(5) with after the flushing of the plastic sheet water after the ultrasonic cleaning, be immersed in the chemical metal plating liquid, reacted 30-60 minute down, just can form even, fine and closely woven thin au electrode, clean, dry up in specific selection zone in 45-50 ℃;
(6) metal electrode on the plastic sheet is immersed in the monomer solution of the conduction high polymer of being with doping agent, under 0.8 ± 0.1V current potential, adopt the potentiostatic method synthesized polyaniline; Perhaps in the potential range of-0.3-1.2V, adopt cyclic voltammetry compositing conducting superpolymer, thereby on the metal electrode on the plastic sheet, realize the pattern sedimentation of conduction high polymer.Wherein doping agent is sulfuric acid or the 0.4-0.7mol/L phosphoric acid of 0.5-0.8mol/L hydrochloric acid, 0.3-0.5mol/L.
3, conduction high polymer according to claim 2 is in the method for frosting pattern sedimentation, it is characterized in that describedly being used to realize that the plastics of conduction high polymer pattern sedimentation are polycarbonate (PC), polyethylene terephthalate (PET), polymethylmethacrylate (PMMA).
4, conduction high polymer according to claim 2 is characterized in that in the method for frosting pattern sedimentation the metal electrode that forms at frosting is precious metal or transition metal materials such as gold, copper, nickel, platinum, palladium, silver; Be that chemical plating fluid is the salt that contains corresponding precious metal or cross metallizing, the solution of complexing agent and reductive agent.
5, conduction high polymer according to claim 2 is characterized in that in the method for frosting pattern sedimentation conduction high polymer is polyaniline, polypyrrole, Polythiophene, poly-thionine, poly-pyrocatechol, poly-phenylene vinylene (ppv) (PPV), poly-Ortho Toluidine, poly-phenylaniline.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104103757A (en) * | 2013-04-03 | 2014-10-15 | 中国科学院微电子研究所 | Preparation method of organic electrode |
| CN104831289A (en) * | 2014-02-10 | 2015-08-12 | 颜圣伦 | Surface treatment method of metal device |
| CN104862986A (en) * | 2015-05-13 | 2015-08-26 | 常州大学 | Preparation method for colored electromagnetic shielding fabric |
| CN104313666B (en) * | 2014-10-14 | 2017-07-28 | 江苏科技大学 | A kind of poly- aC and polyaniline duplicature and preparation method and application |
| CN108221009A (en) * | 2018-01-22 | 2018-06-29 | 邓家润 | A kind of process of surface treatment for being packed for iron flask |
-
2006
- 2006-09-04 CN CN 200610086146 patent/CN1912190A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104103757A (en) * | 2013-04-03 | 2014-10-15 | 中国科学院微电子研究所 | Preparation method of organic electrode |
| CN104831289A (en) * | 2014-02-10 | 2015-08-12 | 颜圣伦 | Surface treatment method of metal device |
| CN104313666B (en) * | 2014-10-14 | 2017-07-28 | 江苏科技大学 | A kind of poly- aC and polyaniline duplicature and preparation method and application |
| CN104862986A (en) * | 2015-05-13 | 2015-08-26 | 常州大学 | Preparation method for colored electromagnetic shielding fabric |
| CN108221009A (en) * | 2018-01-22 | 2018-06-29 | 邓家润 | A kind of process of surface treatment for being packed for iron flask |
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