CN103476200A - Printed circuit addition manufacturing method based on nickel catalysis and chemical copper plating - Google Patents
Printed circuit addition manufacturing method based on nickel catalysis and chemical copper plating Download PDFInfo
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- CN103476200A CN103476200A CN2013104472308A CN201310447230A CN103476200A CN 103476200 A CN103476200 A CN 103476200A CN 2013104472308 A CN2013104472308 A CN 2013104472308A CN 201310447230 A CN201310447230 A CN 201310447230A CN 103476200 A CN103476200 A CN 103476200A
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Abstract
The invention relates to a printed circuit addition manufacturing method based on nickel catalysis and chemical copper plating, and belongs to the field of printed electronic technologies. Firstly, nickel ion ink and reducing agent ink are prepared and subpackaged in two color ink cartridges of an inkjet printer, the color of a printed image is set to be binary colors or broken colors of the two colors, when printed to a substrate, the two kinds of ink performs a superposition reaction on the substrate to form a metallic nickel nano-particle image with catalytic activity, then, the substrate is immersed in an chemical copper plating solution with a sodium hypophosphite reduction system to be plated, and therefore a copper conducting circuit is formed. The printed circuit manufactured with the method is tidy in edge of the circuit image, good in continuity and uniformity of a clad layer and good in electrical conductivity, the appearance is brassy yellow, the nickel content is smaller than 10%, and the electrical resistivity is within the range of 10<5>-10<4>omega*cm. Meanwhile, the manufacturing method has the advantages of being simple in process, low in cost, safe and environmentally friendly.
Description
Technical field
The invention belongs to printed electronic (Printed Electronics) technical field, relate in particular to a kind of with low cost, environmentally friendly printed circuit addition preparation method based on nickel catalysis and electroless copper.The present invention can be used for preparing the patterned conductive circuit in the products such as printed circuit board (pcb), LED substrate, antenna for mobile phone, radio-frequency (RF) tag (RFID) antenna.
Background technology
Conducting wire is as the important component part of Circuits System, and being mainly electronic devices and components, assembly, integrated module etc. provides signal and power to connect.The preparation technology of tradition based on hard base (hardboard PCB, ceramic base), soft base (Flexible PCB) conducting wire is based on " subtractive process ", mainly adopts the copper-clad plate mask etch process, and technological process is long, and problem of environmental pollution is more serious.In recent years, all print conducting wire and device preparation method based on the addition process technological thought is short with its technological process, production equipment is simple, efficient energy-saving, be easy to a series of remarkable advantages such as flexible base R2R technique realization, can realize the functional characteristics such as electric transmission, signal emission, electromagnetic shielding and electricity, magnetic, light, heat, be subject to scientific research and industrial circle and pay much attention to.
The conducting wire all print preparation technology who had already developed mainly comprises: technique thinking one: printing conductive function printing ink (metal nano printing ink, conducting polymer printing ink etc.), dry (hot setting, irradiation, illumination etc.) formation conducting wire of processing; Technique thinking two: printing catalysis printing ink, regrowth (chemical plating, plating, electro-deposition etc.) forms conducting wire.
Wherein technique thinking one is used sodium rice metallic particles slurry as function printing ink usually, and it is high that material nano changes into, and for improving conductivity, often adopts noble silver, further increased cost.And dryings such as the hot setting of these class methods, irradiation, illumination or have high temperature problem (the base material temperature tolerance is had relatively high expectations), or there is in printing ink organic system removal process problems such as easily causing the line pattern distortion.These class methods also easily occur that printing ink is unstable, and particle is easily reunited, thereby is not suitable with spray printing device, and the adhesive force of circuit and the problem such as continuity is poor.Technique thinking two is due to the general solution-type catalytic ink that adopts, blocking sprayer not, and after printing, without hot setting, and the coating adhesion that chemical plating forms is large, and conductivity is high, becomes the focus of current research.
Prior art CN101640979A discloses a kind of manufacture method of conducting wire, this method will comprise that the printing ink of silver salt solution forms line pattern by the inkjet printing mode at substrate surface, adopting the radiation irradiation line pattern to make the silver ion reduction in silver salt is metallic silver corpuscle, thereby obtain prefabricated circuit, again at the coating surface metal of described prefabricated circuit, to form conducting wire, this method adopts silver to make catalyst, cost is high, and the conducting wire growth course has been used the formaldehyde bath system, easily cause human injury and environmental pollution.Prior art CN101580657A discloses printing ink and has utilized the method for this printing ink to manufacture electric conduction line, the printing ink that this method will comprise reducing agent and soluble palladium salt forms the circuit pattern by the inkjet printing mode at substrate surface, adopt the light beam irradiates line pattern to make palladium salt be reduced agent and be reduced to the palladium particle to obtain prefabricated circuit, carry out again chemical plating and form conducting wire, this method is dissolved in palladium salt and reducing agent in same printing ink altogether, ink stability is hard to keep, and palladium is expensive, cost is high, during chemical plating, the same formaldehyde that uses is made reducing agent, also there are human injury and environmental pollution.
In sum, conducting wire addition process preparation method based on technique thinking two adopts the noble metals such as palladium, silver to make catalyst usually, cost is higher, and what the conducting wire regrowth process adopted is all the copper plating bath of formaldehyde systems, toxicity and carcinogenicity are stronger, easily cause human injury and environmental pollution.Therefore, need the conducting wire novel preparation method of seeking a kind of with low cost, safety and environmental protection badly.
Summary of the invention
The invention provides a kind of printed circuit addition preparation method based on nickel catalysis and electroless copper, the method is not used the noble metals such as palladium, silver, adopt the catalyst of nickel as electroless copper, by preparing two kinds of inks, be divided in two print cartridges, only at the nano nickel catalysis figure that prints to two kinds of ink ability stacking reaction generation greater activity on base material, chemical plating is not used formaldehyde, the chemical bronze plating liquid that adopts sodium hypophosphite to make reducing agent carries out plating, has reduced process costs, safety and environmental protection.
Technical solution of the present invention is as follows:
Printed circuit addition preparation method based on nickel catalysis and electroless copper as shown in Figure 1, comprises the following steps:
Step 1: preparation nickel ion ink and reducing agent ink; The water-soluble salt solution that described nickel ion ink is metallic nickel adds organic additive and is formed; Described reducing agent ink is dissolved in strong alkali aqueous solution by boron hydride and adds organic additive to be formed; Wherein organic additive is used for viscosity and the surface tension of regulating nickel ion ink or reducing agent ink.
Step 2: two kinds of ink printed that step 1 is prepared, to base material, form the nano nickel particles line pattern with catalytic activity after stacking reaction;
Step 3: there is electroless copper on the nano nickel particles line pattern of catalytic activity at step 2 gained and form the target printed circuit.
Further: the viscosity of the ink of nickel ion described in step 1 is that 1～5mPas, surface tension are 30～50mN/m, and wherein nickel ion concentration is 0.01～1mol/L; The viscosity of the ink of reducing agent described in step 1 is that 1～5mPas, surface tension are 30～50mN/m, and wherein boron hydride concentration is 0.01～2mol/L, and the concentration of highly basic is 0.01～2mol/L; The water soluble salt of described metallic nickel can be nickelous sulfate, nickel chloride or nickel nitrate, described boron hydride can be sodium borohydride, potassium borohydride, lithium borohydride, zinc borohydride or hydroboration TBuA (TBAB), and described highly basic can be NaOH, potassium hydroxide or barium hydroxide; Described organic additive is ethylene glycol, isopropyl alcohol or the mixture of the two.
Further: the implementation that two kinds of ink printed that step 2 is prepared step 1 form the nano nickel particles line pattern with catalytic activity to stacking reaction on base material is: described nickel ion ink and reducing agent ink are divided in two kinds of color print cartridges of ink-jet printer, secondary color or secondary color that the printing color that figure is set is two kinds of colors, make to print to two kinds of inks on base material and react and generate the nano nickel particles line pattern with catalytic activity after superposeing.
Further: step 3 when step 2 gained has on the nano nickel particles line pattern of catalytic activity that electroless copper forms the target printed circuit, the copper plating bath sulfur acid copper 0.01～0.1mol/L of employing, natrium citricum 0.02～0.2mol/L, sodium hypophosphite 0.1～0.5mol/L, boric acid 0.1～1mol/L, nickelous sulfate 0.001～0.01mol/L, 2-mercaptobenzothiazole 0.1～5mg/L; The pH value of described copper plating bath is controlled between 8～10; The mode of electroless copper adopts drags the plating mode, and while dragging plating, the copper plating bath temperature is controlled between 65～85 ℃.
Printed circuit addition preparation method based on nickel catalysis and electroless copper provided by the invention, wherein relative theory and course of reaction can be described below:
In the chemical bronze plating liquid that is reducing agent at Using Sodium Hypophosphite, different metal to the catalytic activity of sodium hypophosphite oxidation reaction is: Au > Ni > Pd > Co > Pt > Cu(Li Ning. chemical plating practical technique second edition [M]. the .2012:48-50 of Chemical Industry Press).For transition metal, s can be with and d has crossover between being with, thereby affects the filling extent of d electronics.Under normal circumstances, the 3d energy level should be filled 10 electronics, but for nickel, due to what 3d and 4s can be with, overlappingly only have part to enter 3d to be with, partly entering 4s can be with, therefore, d can be with and hole occur, i.e. " d is with hole " (Zhen Kaiji etc. catalytic action basis [M]. the .2006 of Science Press).From catalytic reaction, d is with the existence in hole, make it to have and accept electronics and adsorbing species the ability of Cheng Jian with it from the external world, visible is feasible with Ni as the electroless copper catalyst of sodium hypophosphite reduction system, the nano nickle granules size simultaneously formed by printing is little, and between 10～30 nanometers, specific area is large, surface atom is many, can improve the catalytic activity of nickel.
Two kinds of inks that step 1 is prepared (nickel ion ink and reducing agent ink) are divided in two kinds of color print cartridges of ink-jet printer, secondary color or secondary color that the color that printing curve is set is two kinds of colors, in the time of on printing to substrate, two kinds of inks are from spray orifice ejection separately, form the small ink droplet of 10～30 microns of diameters, on base material, superpose and react
just form the metallic nickel nano granule figure on base material, the nickel particle size is (as shown in Figure 2) between 10～30 nanometers.
The prepared printed circuit by the present invention, the circuitous pattern neat in edge, coating continuity and uniformity are better, and outward appearance is brassy, and nickel content is less than 10%, and resistivity is 10
-5～10
-4between Ω cm, conductivity is good.
Compared with prior art, the present invention has following beneficial effect:
1. cost of manufacture is low: this technique does not adopt the noble metals such as palladium, silver, but the nano nickel that adopts inkjet printing to form is as the catalyst of subsequent chemistry plating.
2. safety and environmental protection: this technique does not adopt formaldehyde reduction system plating solution, adopts the sodium hypophosphite electroless copper liquid system of environmental protection to carry out the figure metallization and form the conductive copper wire road.
3. work simplification: ink separately stores, and good stability just can form the nano nickel catalysis line pattern with catalytic activity without steps such as irradiation, heating after printing.
The accompanying drawing explanation
Fig. 1 is the conducting wire preparation method's that provides of the technical program schematic flow sheet.
Fig. 2 is that the technical program embodiment 1 is printed the nano nickel catalysis figure SEM figure obtained.
Embodiment
Below in conjunction with accompanying drawing and embodiment, the technical program is further illustrated.
Embodiment 1:
By 0.015mol NiSO
46H
2o is dissolved in the 40mL deionized water, then adds 1mL ethylene glycol and 5mL isopropyl alcohol, adds deionized water and is settled to 50mL and is the nickel ion ink; 0.025mol NaOH is dissolved in the 30mL deionized water, then by 0.034mol NaBH
4be dissolved in above NaOH solution, then add 5mL ethylene glycol and 10mL isopropyl alcohol, finally add deionized water and be settled to 50mL and be the reducing agent ink.Two kinds of inks are respectively charged in two kinds of color print cartridges of ink-jet printer, printer is ready.
Polyimides (PI) base material water is cleaned and dries, preparation base material preprocessing solution, wherein comprise: NaOH 1.5mol/L, sodium carbonate 0.2mol/L, tertiary sodium phosphate 0.01mol/L, this pretreatment fluid has the effect of oil removing and alligatoring to the polyimide base material surface, in thermostat water bath, the heated constant temperature treatment fluid is at 60 ℃, base material is immersed to this and wherein keep 6 minutes, take out with drying after twice of rinsed with deionized water to be printed.
By the pretreated base material printer of packing into, by Auto CAD, print colors being set is secondary color or the secondary color that two kinds of print cartridge colors of two kinds of inks are housed, can regulate the output variable of each chromatic ink and the precision of printing by setting of printing simultaneously, after having printed at the line pattern of the visible pitchy of substrate surface, show to have the Ni particle to generate, the base material hang airing after printing is to be plated.
The preparation chemical copper plating solution, wherein each concentration of component is: copper sulphate 0.04mol/L, natrium citricum 0.07mol/L, sodium hypophosphite 0.28mol/L, boric acid 0.48mol/L, nickelous sulfate 0.007mol/L, 2-mercaptobenzothiazole 1.5mg/L, pH is 9.
Controlling the chemical copper plating solution temperature is 65 ℃, will treat that plated substrate immerses in this copper plating bath plating 10 minutes, takes out and rinses well with deionized water, obtains that copper is yellow, half bright copper plating layer printed circuit, and resistivity is 4.3 * 10
-5Ω cm.
Embodiment 2:
By 0.013mol NiSO
46H
2o is dissolved in the 40mL deionized water, then adds 2mL ethylene glycol and 5mL isopropyl alcohol, adds deionized water and is settled to 50mL and is the nickel ion ink; 0.02mol NaOH is dissolved in the 35mL deionized water, then by 0.026mol NaBH
4be dissolved in above NaOH solution, then add 3mL ethylene glycol and 7mL isopropyl alcohol, finally add deionized water and be settled to 50mL and be the reducing agent ink.Two kinds of inks are respectively charged in two kinds of color print cartridges of ink-jet printer, printer is ready.
Polyimides (PI) substrate is cut into to the A5 size, with alcohol-pickled, water cleans and dries, the preparation preprocessing solution, wherein comprise: NaOH 2mol/L, sodium carbonate 0.3mol/L, tertiary sodium phosphate 0.02mol/L, heating constant temperature to 60 ℃ in thermostat water bath, immerse substrate in this solution and keep 5 minutes, takes out with drying after twice of rinsed with deionized water to be printed.
By the pretreated base material printer of packing into, by Auto CAD, print colors being set is secondary color or the secondary color that two kinds of print cartridge colors of two kinds of inks are housed, can regulate the output variable of each chromatic ink and the precision of printing by setting of printing simultaneously, line pattern at the visible pitchy of base material after having printed shows to have metal Ni particle to generate, and the substrate hang airing after printing is to be plated.
The preparation chemical bronze plating liquid, wherein each concentration of component is: copper sulphate 0.036mol/L, natrium citricum 0.068mol/L, sodium hypophosphite 0.264mol/L, boric acid 0.32mol/L, nickelous sulfate 0.006mol/L, 2-mercaptobenzothiazole 1mg/L, pH is 9.5.
Controlling the chemical copper plating solution temperature is 70 ℃, will treat that plated substrate immerses in this copper plating bath plating 10 minutes, takes out and rinses well with deionized water, obtain copper Huang, half bright copper plating layer printed circuit, through energy spectrum analysis, wherein copper content surpasses 92%, and resistivity is 4.3 * 10
-5Ω cm.
Those skilled in the art it should be known that in conjunction with the present invention and general knowledge known in this field above-mentioned embodiment is not limitation of the invention further.According to the disclosed technical scheme of summary of the invention, those skilled in the art should know: in the nickel ion ink, the water soluble salt of metallic nickel used, except nickelous sulfate, can also adopt nickel chloride or nickel nitrate; In the reducing agent ink, boron hydride used, except sodium borohydride, can also adopt lithium borohydride, zinc borohydride or hydroboration TBuA (TBAB); In the reducing agent ink, highly basic used, except NaOH, can also adopt potassium hydroxide or barium hydroxide; In nickel ion ink and reducing agent ink, organic additive has been adjusting viscosity and capillary effect, itself does not participate in reaction, therefore it is all feasible adopting ethylene glycol, isopropyl alcohol or the arbitrary proportion mixture of the two, about viscosity and the capillary adjustable range of nickel ion ink and reducing agent ink, can be regulated according to the relevant parameter of ink-jet printer in addition.
In addition, those skilled in the art should know in conjunction with the present invention and general knowledge known in this field, only provide relevant preferred practical range about nickel ion ink, reducing agent ink and chemical plating fluid about the restriction of solute concentration in technical solution of the present invention, being to obtain in order better to realize technical solution of the present invention the printed circuit that performance is more excellent, is not necessary in order to implement technical solution of the present invention.Those skilled in the art fully can be according to description of the invention, determine relevant solute concentration and then realize the present invention in concentration range provided by the invention, even being not precluded within definite relevant solute concentration outside concentration range provided by the invention and also can realizing the present invention.
Finally, during about electroless copper, the description of the temperature range of plating solution neither be necessary, do not get rid of the possibility that adopts chemical bronze plating liquid provided by the invention copper facing success at normal temperatures, and just in temperature range provided by the invention, copper facing can improve copper facing speed.
In a word, the invention provides a kind of printed circuit addition preparation method based on nickel catalysis and electroless copper, the method is not used the noble metals such as palladium, silver, adopts the catalyst of nickel as electroless copper, by preparing two kinds of inks, be divided in two print cartridges, only, at the nano nickel catalysis figure that prints to two kinds of ink ability stacking reaction generation greater activity on base material, chemical plating is not used formaldehyde, and the chemical bronze plating liquid that adopts sodium hypophosphite to make reducing agent carries out plating, reduced process costs, safety and environmental protection.
Claims (10)
1. the printed circuit addition preparation method based on nickel catalysis and electroless copper comprises the following steps:
Step 1: preparation nickel ion ink and reducing agent ink; The water-soluble salt solution that described nickel ion ink is metallic nickel adds organic additive and is formed; Described reducing agent ink is dissolved in strong alkali aqueous solution by boron hydride and adds organic additive to be formed; Wherein organic additive is used for viscosity and the surface tension of regulating nickel ion ink or reducing agent ink;
Step 2: two kinds of ink printed that step 1 is prepared, to base material, form the nano nickel particles line pattern with catalytic activity after stacking reaction;
Step 3: there is electroless copper on the nano nickel particles line pattern of catalytic activity at step 2 gained and form the target printed circuit.
2. the printed circuit addition preparation method based on nickel catalysis and electroless copper as claimed in claim 1, it is characterized in that, the viscosity of the ink of nickel ion described in step 1 is that 1～5mPas, surface tension are 30～50mN/m, and wherein nickel ion concentration is 0.01～1mol/L; The viscosity of described reducing agent ink is that 1～5mPas, surface tension are 30～50mN/m, and wherein boron hydride concentration is 0.01～2mol/L, and the concentration of highly basic is 0.01～2mol/L.
3. the printed circuit addition preparation method based on nickel catalysis and electroless copper as claimed in claim 1 or 2, is characterized in that, the water soluble salt of metallic nickel described in step 1 is nickelous sulfate, nickel chloride or nickel nitrate.
4. the printed circuit addition preparation method based on nickel catalysis and electroless copper as claimed in claim 1 or 2, is characterized in that, boron hydride described in step 1 is sodium borohydride, potassium borohydride, lithium borohydride, zinc borohydride or hydroboration TBuA.
5. the printed circuit addition preparation method based on nickel catalysis and electroless copper as claimed in claim 1 or 2, is characterized in that, highly basic described in step 1 is NaOH, potassium hydroxide or barium hydroxide.
6. the printed circuit addition preparation method based on nickel catalysis and electroless copper as claimed in claim 1 or 2, is characterized in that, organic additive described in step 1 is ethylene glycol, isopropyl alcohol or the mixture of the two.
7. the printed circuit addition preparation method based on nickel catalysis and electroless copper as claimed in claim 1 or 2, it is characterized in that, base material described in step 2 is polyimides, acrylonitrile-BS, PEN, PETG, Merlon, polystyrene or polymethyl methacrylate.
8. the printed circuit addition preparation method based on nickel catalysis and electroless copper as claimed in claim 1 or 2, it is characterized in that, the implementation that two kinds of ink printed that step 2 is prepared step 1 form the nano nickel particles line pattern with catalytic activity to stacking reaction on base material is: described nickel ion ink and reducing agent ink are divided in two kinds of color print cartridges of ink-jet printer, secondary color or secondary color that the printing color that figure is set is two kinds of colors, making to print to two kinds of inks on base material reacts and generates the nano nickel particles line pattern with catalytic activity after superposeing.
9. the printed circuit addition preparation method based on nickel catalysis and electroless copper as claimed in claim 1 or 2, it is characterized in that, step 3 when step 2 gained has on the nano nickel particles line pattern of catalytic activity that electroless copper forms the target printed circuit, the copper plating bath sulfur acid copper 0.01～0.1mol/L of employing, natrium citricum 0.02～0.2mol/L, sodium hypophosphite 0.1～0.5mol/L, boric acid 0.1～1mol/L, nickelous sulfate 0.001～0.01mol/L, 2-mercaptobenzothiazole 0.1～5mg/L; The pH value of described copper plating bath is controlled between 8～10; The mode of electroless copper adopts drags the plating mode, and while dragging plating, the copper plating bath temperature is controlled between 65～85 ℃.
10. the printed circuit addition preparation method based on nickel catalysis and electroless copper as claimed in claim 1 or 2, is characterized in that, before carrying out the described operation of step 2, described base material carried out to surface degreasing and roughening treatment.
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| CN106337172A (en) * | 2016-08-30 | 2017-01-18 | 辽宁科技学院 | Method for palladium-free activation chemical copper plating of surface of carbon steel |
| CN107974675A (en) * | 2017-11-29 | 2018-05-01 | 西华大学 | A kind of high strength alumin ium alloy and preparation method thereof |
| CN109423614A (en) * | 2017-08-22 | 2019-03-05 | 宁波江丰电子材料股份有限公司 | Target material assembly manufacturing method |
| CN110843370A (en) * | 2018-07-30 | 2020-02-28 | 卡西欧计算机株式会社 | Computer-readable recording medium, conductive circuit, and method for producing conversion chart |
| CN110983763A (en) * | 2019-12-18 | 2020-04-10 | 浙江蓝天制衣有限公司 | Chemical copper plating process suitable for clothing cotton fabric |
| CN113981421A (en) * | 2021-07-09 | 2022-01-28 | 西安电子科技大学 | Method for preparing erasable metal electrode on plastic surface |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106337172A (en) * | 2016-08-30 | 2017-01-18 | 辽宁科技学院 | Method for palladium-free activation chemical copper plating of surface of carbon steel |
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| CN110983763A (en) * | 2019-12-18 | 2020-04-10 | 浙江蓝天制衣有限公司 | Chemical copper plating process suitable for clothing cotton fabric |
| CN113981421A (en) * | 2021-07-09 | 2022-01-28 | 西安电子科技大学 | Method for preparing erasable metal electrode on plastic surface |
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Application publication date: 20131225 |