CN111778496B - Activating agent for nickel plating of tin alloy activated copper layer and nickel plating method - Google Patents
Activating agent for nickel plating of tin alloy activated copper layer and nickel plating method Download PDFInfo
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- CN111778496B CN111778496B CN202010676182.XA CN202010676182A CN111778496B CN 111778496 B CN111778496 B CN 111778496B CN 202010676182 A CN202010676182 A CN 202010676182A CN 111778496 B CN111778496 B CN 111778496B
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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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/18—Pretreatment of the material to be coated
- C23C18/1803—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces
- C23C18/1824—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces by chemical pretreatment
- C23C18/1827—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces by chemical pretreatment only one step pretreatment
- C23C18/1831—Use of metal, e.g. activation, sensitisation with noble metals
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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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
- C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
- C23C18/36—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents using hypophosphites
Abstract
The invention belongs to the technical field of chemical nickel plating, and provides an activator for activating a copper layer by tin alloy to plate nickel and a nickel plating method, which are characterized in that: the activating agent comprises metal salt consisting of a component I and a component II, and also comprises an accelerant, a pH regulator and a brightener, wherein the component I is a tin salt, the component II is a catalytic metal salt, and the accelerant comprises thiourea, citric acid, tartaric acid, EDTA, sodium fluoride and polyethylene glycol. The nickel plating method comprises the following steps: degreasing, pre-copper, thick copper, activation and nickel plating. The invention has the following advantages and effects: the activator for activating the copper layer to plate the nickel does not contain noble metal palladium, so that the production cost of activating the copper surface can be greatly reduced; the operation process range of the activator for nickel plating of the tin alloy activated copper layer is wider, and the operation is easier; the production control is easy, the phenomena of plating leakage and plating overflow can not be generated in the operation process, and the qualification rate of products is greatly improved.
Description
Technical Field
The invention belongs to the technical field of chemical nickel plating, and particularly relates to an activating agent for nickel plating of a tin alloy activated copper layer and a nickel plating method.
Background
The LDS mobile phone antenna technology is a Laser-Direct-structuring technology, which uses a computer to control the movement of Laser according to the trace of a conductive pattern, so as to project the Laser onto a molded three-dimensional plastic device, and activate a circuit pattern within a few seconds. After copper is plated in the circuit pattern of the LDS mobile phone antenna, the corrosion resistance of the copper can be improved by plating nickel on the surface of the copper, and the copper substrate is usually protected by depositing a nickel plating layer on the surface of the copper substrate at present. Although the electrokinetic sequence of metallic nickel precedes hydrogen, it can undergo self-passivation to form a dense self-passivation film when exposed to air, thereby ensuring that the substrate is not further oxidized, and therefore possesses very excellent corrosion resistance.
Generally, in order to obtain a nickel plating layer on a copper surface by an electroless plating method, a layer of noble metal palladium having catalytic activity is replaced on the copper surface in advance. However, the catalytic activity of the metal palladium is too high, the problems of easy over plating and plating leakage exist when the metal palladium is adopted for activation, the price of the palladium is high, and the production cost is high.
The Chinese invention patent with application publication number CN 110724943A provides palladium-free activation solution before chemical nickel plating on the surface of copper, a preparation method and a nickel plating method, nickel salt is used as an activation base layer of the following chemical nickel plating, sodium hypophosphite and dimethylamino borane are used as reducing agents, a nickel plating layer with catalytic activity is pre-plated on the copper surface of a printed circuit board, and the subsequent chemical nickel plating link can be continued.
Tian dong in doctor's treatise on the study on the performance of replacement nickel plating and plating on copper surface obtains a replacement nickel plating layer capable of initiating autocatalysis type chemical nickel plating on the copper surface, and realizes the purpose of initiating chemical nickel plating on the surface of copper lines of a printed circuit board by replacing a palladium activation method with a replacement nickel plating method.
However, when the replacement nickel plating layer prepared under the strong acid condition is used as a catalytic layer of chemical nickel plating, the plating start time is slightly longer than the palladium activation, and the catalytic activity of the replacement nickel plating layer does not reach the palladium activation level completely; when the displacement nickel plating layer is used as a protective plating layer for a copper substrate, the plating layer thickness is thin, and a method for increasing the plating layer thickness needs to be developed.
Disclosure of Invention
The invention aims to provide an activating agent and a method for activating copper layer nickel plating by tin alloy, which have the effects of greatly reducing the cost and preventing the occurrence of plating leakage and excessive plating of the nickel plating.
The technical purpose of the invention is realized by the following technical scheme: the tin salt-based composite material comprises a metal salt consisting of a component I and a component II, an accelerant, a pH regulator and a brightener, wherein the component I is a tin salt, the component II is a catalytic metal salt, and the accelerant comprises thiourea, citric acid, tartaric acid, EDTA, sodium fluoride and polyethylene glycol.
By adopting the technical scheme, under the standard condition, the electrode potential of copper is far higher than that of nickel, so that replacement nickel plating on the surface of copper is difficult to realize in a simple salt solution, and the potential of the surface of copper needs to be reduced when nickel plating is carried out on the copper.
The invention is further provided with: the tin salt is one of stannous chloride, stannous sulfate and tin methanesulfonate.
The invention is further provided with: the catalytic metal salt is sodium molybdate.
The invention is further provided with: the catalytic metal salts include cobalt sulfate and sodium tungstate.
The invention is further provided with: the catalytic metal salts include sodium tungstate and ferrous sulfate.
By adopting the technical scheme, the tin salt can perform a displacement reaction with copper under an acidic condition, molybdenum, cobalt, tungsten and iron metal ions with lower induced potentials can form a low-potential tin alloy layer with catalytic activity on the surface of a copper substrate in the tin-copper displacement reaction process, the tin alloy layer can reduce the potential of the copper substrate surface, and displacement nickel plating on the copper surface is realized in the chemical nickel plating process, so that the chemical nickel plating is initiated, and a nickel coating is deposited on the copper substrate surface.
The invention is further provided with: the concentration of the tin salt is 5-50 g/L.
The invention is further provided with: the concentration of the catalytic metal salt is 1-20 g/L.
The invention is further provided with: the accelerant comprises 10-100 g/L of thiourea, 20-100 g/L of citric acid, 20-80 g/L, EDTA 10g/L of tartaric acid, 0.1-1 g/L of sodium fluoride and 0.1-10 g/L of polyethylene glycol.
By adopting the technical scheme, the thiourea can be used as a strong ligand of copper, so that the stable potential of the copper is changed, the copper becomes very active in a high-concentration thiourea solution, the electron release and the electron exchange in the tin-copper displacement reaction can be promoted, the released electrons can induce the reduction of low-potential metal ions, a tin alloy layer is formed on the surface of the copper base, and the thiourea can also be used as a stabilizer of chemical nickel plating; the sodium fluoride and the thiourea have synergistic effect, can enhance the electron release in the displacement reaction of tin and copper, and can also enhance the permeability of the activating solution at the same time, so that a tin alloy layer formed on the surface of the copper base is tightly combined with the copper base; the polyethylene glycol can enhance the dispersibility of the activating solution, when the LDS mobile phone antenna is plated with nickel, the LDS mobile phone antenna is complex and irregular in shape, has a plurality of pits, corners, through holes and the like, is difficult to plate, can completely permeate the activating solution and the base material under the synergistic effect of the polyethylene glycol and the sodium fluoride, can form a uniform plating layer on the surface with the complex shape, and can improve the flatness of the plating layer.
The method for plating the nickel on the tin alloy activated copper layer is characterized by comprising the following steps of:
s1 oil removal: placing the workpiece in a solution containing Na2CO3 20～40g/L、NaOH 20～30g/L、Na3PO3Carrying out ultrasonic oil removal in 10-30 g/L cleaning solution;
s2 pre-copper: washing the deoiled workpiece with water, putting the workpiece into a pre-copper solution, taking out after 10-30 min, and uniformly plating a layer of red brown copper on the workpiece;
s3 thick copper: washing the workpiece pre-copper in the step S2 with water, putting the workpiece into thick copper liquid, taking out the workpiece after 1-3 h, and plating a uniform and fine pink copper layer on the workpiece;
s4 acid washing: soaking the workpiece with the thick copper in the step S3 in a 5% hydrochloric acid solution for 1-2 min;
s5 activation: washing the workpiece pickled in the step S4 with water, then putting the workpiece into the activating agent according to any one of claims 1 to 8, wherein the activating temperature is 40-50 ℃, the pH value is 1.0-2.0, the activating time is 3-5 min, and taking out the workpiece after the activation is finished;
s6 nickel plating: and (4) washing the workpiece activated in the step (S4) with three times of water, putting the workpiece into nickel liquid, carrying out nickel plating at the temperature of 76-80 ℃, the pH value of 4.6-5.0 for 15-30 min, and taking out the workpiece after the nickel plating is finished to obtain a silver-white uniform nickel layer.
The invention is further provided with: the nickel liquid is composed of 10-50 g/L of nickel sulfate, 10-100 g/L, NaOH 10-50 g/L of lactic acid, 20-80 g/L of malic acid, 20-80 g/L of ammonium sulfate, 10-50 g/L of sodium acetate, 10-50 g/L of sodium succinate, 50-150 g/L of sodium hypophosphite, 10-20 g/L of sodium borohydride and 1-10 mL/L of coordination agent.
The invention has the beneficial effects that:
1. the activator for activating the copper layer by using the tin alloy to plate the nickel does not contain noble metal palladium, so that the production cost of activating the copper surface can be greatly reduced.
2. The activator for nickel plating of the tin alloy activated copper layer has wider operation process range and is easier to operate.
3. The production process has the advantages of excellent stability, long service life and simple operation.
4. The production control is easy, the phenomena of plating leakage and plating overflow can not be generated in the operation process, and the qualification rate of products is greatly improved.
5. The method for nickel plating of the tin alloy activated copper layer is adopted, the operation control temperature is low, the chemical nickel plating process temperature in the general market is controlled to be 90 ℃ for normal production, and the chemical nickel plating process temperature in the scheme is controlled to be 76-80 ℃ for normal production; the paint does not contain organic harmful substances such as cadmium, mercury, lead, hexavalent chromium and the like; the process is stable, energy-saving and environment-friendly, and the uniform surface of the plating layer can achieve mirror surface brightness; the nickel plating solution is particularly suitable for chemical nickel plating of circuit boards and plastic accessories in the electronic industry; the coating has an amorphous form and excellent flexibility and ductility; the defective products of the plating layer are easy to remove; the bath solution has excellent stability, and the continuous operation can reach 6-8 cycle periods.
Detailed Description
The technical solutions in the examples will be clearly and completely described below. It is to be understood that the described embodiments are merely a few embodiments of the invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without any inventive step, are within the scope of the present invention.
Example 1
The activating agent for activating the nickel plating of the copper layer by the tin alloy is characterized in that: the environment-friendly polishing solution comprises metal salt, an accelerant, a pH regulator and a brightening agent, wherein the metal salt comprises a component I and a component II, the component I is stannous chloride 50g/L, the component II is sodium molybdate 1g/L, and the accelerant comprises thiourea 100g/L, citric acid 20g/L, tartaric acid 80g/L, EDTA 10g/L, sodium fluoride 1g/L and polyethylene glycol 0.1 g/L.
Example 2
The activating agent for activating the nickel plating of the copper layer by the tin alloy is characterized in that: the environment-friendly corrosion inhibitor comprises a metal salt, an accelerant, a pH regulator and a brightening agent, wherein the metal salt is composed of a component I and a component II, the component I is 5g/L of stannous sulfate, the component II is 10g/L of cobalt sulfate and 1/L of sodium tungstate, and the accelerant comprises 100g/L of thiourea, 20g/L of citric acid, 80g/L, EDTA 10g/L of tartaric acid, 1g/L of sodium fluoride and 0.1g/L of polyethylene glycol.
Example 3
The activating agent for activating the nickel plating of the copper layer by the tin alloy is characterized in that: the polishing solution comprises a metal salt, an accelerator, a pH regulator and a brightener, wherein the metal salt comprises a component I and a component II, the component I is 50g/L of tin methanesulfonate, the component II is 1g/L of sodium tungstate and 10g/L of ferrous sulfate, and the accelerator comprises 10g/L of thiourea, 100g/L of citric acid, 20g/L, EDTA 80g/L of tartaric acid, 0.1g/L of sodium fluoride and 10g/L of polyethylene glycol.
Example 4
In this embodiment, the method for nickel plating using the activating solution for nickel plating of the tin alloy activated copper layer in embodiment 3 includes the following steps:
s1 oil removal: placing the workpiece in a solution containing Na2CO3 40g/L、NaOH 20g/L、Na3PO3Ultrasonic degreasing is carried out in 30g/L cleaning solution;
s2 pre-copper: washing the deoiled workpiece with water, putting the workpiece into a pre-copper solution, taking out after 10min, and uniformly plating a layer of red brown copper on the workpiece;
s3 thick copper: washing the workpiece pre-copper in the step S2 with water, putting the workpiece into thick copper liquid, and taking out the workpiece after 3 hours to plate a uniform and fine pink copper layer on the workpiece;
s4 acid washing: soaking the workpiece with the thick copper in the step S3 in a 5% hydrochloric acid solution for 1-2 min;
s5 activation: washing the pickled workpiece obtained in the step S4 with water, then placing the washed workpiece into the activating agent according to any one of claims 1, wherein the activating temperature is 50 ℃, the pH value is 1.0, the activating time is 5min, and taking out the workpiece after the activation is finished;
s6 nickel plating: and (4) washing the workpiece activated in the step (S5) by three times of water, putting the workpiece into nickel liquid, carrying out nickel plating at the temperature of 76 ℃, the pH value of 5.0 and the reaction time of 15min, and taking out the workpiece after the nickel plating is finished to obtain a silvery white and uniform nickel layer.
The nickel liquid is composed of 50g/L nickel sulfate, 10g/L, NaOH50g/L lactic acid, 20g/L malic acid, 80g/L ammonium sulfate, 10g/L sodium acetate, 50g/L sodium succinate, 150g/L sodium hypophosphite, 20g/L sodium borohydride and 1mL/L complexing agent.
Example 5
In this embodiment, the nickel plating method using the activating solution for activating the copper layer with tin alloy in the above embodiment 3 includes the following steps:
s1 oil removal: placing the workpiece in a solution containing Na2CO3 20g/L、NaOH 30g/L、Na3PO3Ultrasonic degreasing is carried out in 10g/L cleaning solution;
s2 pre-copper: washing the deoiled workpiece with water, putting the workpiece into a pre-copper solution, taking out after 30min, and uniformly plating a layer of red brown copper on the workpiece;
s3 thick copper: washing the workpiece pre-copper in the step S2 with water, putting the workpiece into thick copper liquid, taking out the workpiece after 1 hour, and plating a uniform and fine pink copper layer on the workpiece;
s4 acid washing: soaking the workpiece with the thick copper in the step S3 in a 5% hydrochloric acid solution for 1-2 min;
s5 activation: washing the pickled workpiece obtained in the step S4 with water, then placing the washed workpiece into the activating agent according to any one of the claims 1, wherein the activating temperature is 40 ℃, the pH value is 2.0, the activating time is 3min, and taking out the workpiece after the activation is finished;
s6 nickel plating: and (4) washing the workpiece activated in the step (S4) by three times of water, putting the workpiece into nickel liquid, carrying out nickel plating at the temperature of 80 ℃, the pH value of 4.6 and the reaction time of 30min, and taking out the workpiece after the nickel plating is finished to obtain a silvery white and uniform nickel layer.
The nickel liquid consists of 10g/L of nickel sulfate, 100g/L, NaOH10 g/L of lactic acid, 80g/L of malic acid, 20g/L of ammonium sulfate, 50g/L of sodium acetate, 10g/L of sodium succinate, 50g/L of sodium hypophosphite, 10g/L of sodium borohydride and 10mL/L of complexing agent.
The thickness of copper on the antenna after the LDS antenna material is subjected to thick copper is 8-12 mu m, and after washing, activation nickel plating is respectively carried out by adopting the activation solutions of the examples 1-3, so that both the example 1 and the example 2 can carry out lead plating, but the reaction time is long, the skip plating is serious, the reaction speed of the example 3 is high, and uniform nickel plating can be carried out on letters, numbers and small lines.
The embodiments 4 to 5 achieve better nickel plating effect, the operation deposition speed can reach 16-18mu/h, the salt spray test of the coating 5um can reach 48-72 h, and the Baige test grade can reach 5B.
Claims (3)
1. The activating agent for activating the nickel plating of the copper layer by the tin alloy is characterized in that: the catalyst comprises a metal salt consisting of a component I and a component II, and also comprises an accelerator, a pH regulator and a brightener, wherein the component I is a tin salt, the component II is a catalytic metal salt, the accelerator comprises thiourea, citric acid, tartaric acid, EDTA, sodium fluoride and polyethylene glycol, the component I is 50g/L tin methanesulfonate, the component II is 1g/L sodium tungstate and 10g/L ferrous sulfate, and the accelerator comprises 10g/L thiourea, 100g/L citric acid, 20g/L, EDTA 80g/L tartaric acid, 0.1g/L sodium fluoride and 10g/L polyethylene glycol.
2. The method for plating the nickel on the tin alloy activated copper layer is characterized by comprising the following steps of:
s1 oil removal: placing the workpiece in a solution containing Na2CO3 20~40g/L、NaOH 20~30g/L、Na3PO3Carrying out ultrasonic oil removal in 10-30 g/L cleaning solution;
s2 pre-copper: washing the deoiled workpiece with water, putting the workpiece into a pre-copper solution, taking out after 10-30 min, and uniformly plating a layer of red brown copper on the workpiece;
s3 thick copper: washing the workpiece pre-copper in the step S2 with water, putting the workpiece into thick copper liquid, taking out the workpiece after 1-3 h, and plating a uniform and fine pink copper layer on the workpiece;
s4 acid washing: soaking the workpiece with the thick copper in the step S3 in a 5% hydrochloric acid solution for 1-2 min;
s5 activation: washing the workpiece pickled in the step S4 with water, then putting the workpiece into the activating agent of claim 1, wherein the activating temperature is 40-50 ℃, the pH value is 1.0-2.0, the activating time is 3-5 min, and taking out the workpiece after the activation is finished;
s6 nickel plating: and (4) washing the workpiece activated in the step (S4) with three times of water, putting the workpiece into nickel liquid, carrying out nickel plating at the temperature of 76-80 ℃, the pH value of 4.6-5.0 for 15-30 min, and taking out the workpiece after the nickel plating is finished to obtain a silver-white uniform nickel layer.
3. A method of nickel plating a tin alloy activated copper layer according to claim 2, characterized in that: the nickel liquid is composed of 10-50 g/L of nickel sulfate, 10-100 g/L, NaOH 10-50 g/L of lactic acid, 20-80 g/L of malic acid, 20-80 g/L of ammonium sulfate, 10-50 g/L of sodium acetate, 10-50 g/L of sodium succinate, 50-150 g/L of sodium hypophosphite, 10-20 g/L of sodium borohydride and 1-10 mL/L of coordination agent.
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| CN113151812B (en) * | 2021-04-20 | 2022-10-11 | 广东工业大学 | Tin activating solution, preparation method thereof and chemical nickel plating method |
| CN115341202B (en) * | 2022-08-03 | 2024-04-02 | 惠州市安泰普表面处理科技有限公司 | Activating solution for aluminum alloy before chemical nickel plating and pretreatment method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| EP1988192B1 (en) * | 2007-05-03 | 2012-12-05 | Atotech Deutschland GmbH | Process for applying a metal coating to a non-conductive substrate |
| CN111235557A (en) * | 2020-03-10 | 2020-06-05 | 广州传福化学技术有限公司 | Chemical nickel plating solution and chemical nickel plating method |
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| CN101446037B (en) * | 2008-12-29 | 2011-07-20 | 中国科学院长春应用化学研究所 | Preparation method of electric-conducting polyimide fiber |
| CN105296976A (en) * | 2015-10-21 | 2016-02-03 | 深圳市发斯特精密技术有限公司 | Chemical-copper solution and chemical copper plating method |
| EP3467152A4 (en) * | 2016-06-03 | 2019-12-04 | Furukawa Electric Co., Ltd. | Surface treatment material, production method thereof, and component formed using surface treatment material |
| CN107119266A (en) * | 2017-04-18 | 2017-09-01 | 广州传福化学技术有限公司 | Soldering copper piece surface chemical plating nickel solution and its nickel plating technology |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| EP1988192B1 (en) * | 2007-05-03 | 2012-12-05 | Atotech Deutschland GmbH | Process for applying a metal coating to a non-conductive substrate |
| CN111235557A (en) * | 2020-03-10 | 2020-06-05 | 广州传福化学技术有限公司 | Chemical nickel plating solution and chemical nickel plating method |
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