CN115595567A - Anti-tarnishing chemical silver plating solution - Google Patents
Anti-tarnishing chemical silver plating solution Download PDFInfo
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- CN115595567A CN115595567A CN202211052998.0A CN202211052998A CN115595567A CN 115595567 A CN115595567 A CN 115595567A CN 202211052998 A CN202211052998 A CN 202211052998A CN 115595567 A CN115595567 A CN 115595567A
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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
- C23C18/42—Coating with noble metals
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/10—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern
- H05K3/18—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern using precipitation techniques to apply the conductive material
- H05K3/181—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern using precipitation techniques to apply the conductive material by electroless plating
Abstract
The invention belongs to the field of printed circuit board preparation, and particularly relates to an anti-tarnishing chemical silver plating solution. The silver plating solution comprises the following components: silver oxide, a copper ion complexing agent, a composite antitarnish agent, sulfamic acid, a stabilizer, an accelerator, a nucleating agent, a wetting agent and deionized water; the concentration of the silver oxide in the anti-tarnishing chemical silver plating solution is 1.2 to 1.5g/L; the composite antitarnish agent is sodium polystyrene sulfonate and 3,4-ethylenedioxythiophene, and the weight ratio is sodium polystyrene sulfonate: 5363 and 3,4-ethylenedioxythiophene =1 (3~5), and the concentration of the composite antitarnish agent in the silver plating solution is 1 to 3g/L. The silver plating solution provided by the invention can realize better stability of the plating solution, and the formed plating layer is flat and uniform, has good thickness and white and bright metallic luster, and has better weather resistance.
Description
Technical Field
The invention belongs to the field of printed circuit board preparation, and particularly relates to an anti-tarnishing chemical silver plating solution.
Background
As a surface treatment process for a packaging carrier plate and a printed circuit board, chemical silver plating has the advantages of good flatness, solderability, oxidation resistance, heat resistance, conductivity and the like, has small atomic diffusivity and is relatively economical, and is especially prominent in 5G substrate application. Chemical silver plating is used in the assembly of electronic devices, but is easy to oxidize and discolor after silver plating and is easy to generate electrochemical migration phenomenon, in order to meet production requirements in recent years, new silver plating processes are continuously developed, the operation is simple, the cost is low, and the process flow mainly comprises acid oil removal, pure water washing, micro-etching, pure water washing, presoaking, chemical silver immersion, pure water washing, hot water washing and drying.
At present, the main problem of chemical silver is still that the chemical silver is susceptible to atmospheric pollution gas, such as discoloration reaction of blackening and yellowing of a silver layer caused by corrosion of gases containing chlorine, sulfur and the like, so that the service life of the surface treatment of the chemical silver for the PCB is only half a year, the application range of the chemical silver is greatly limited, but in 5G construction, the transmission effect of the silver to 5G frequency is the best, and therefore, the application prospect of the chemical silver is very wide.
The chemical silver plating solution in the prior art can be exemplified by a silver plating solution ammonium citrate system described in patent ZL201310312530.5, the pH value of the chemical silver plating solution is 8.2-10.2, the chemical silver plating solution is alkalescent to neutral-alkaline, although a certain stability can be achieved, the chemical silver plating solution cannot be used for a long time, and the obtained silver layer is not bright enough in metallic luster. The patent ZL201310312530.1 uses lanthanum oxide and ceric sulfate as additives to solve the problem of plating leakage, but the ion pollution degree is high and the stability of the plating solution is not high. The silver plating solution described in patent zl201210270962.x is composed of silver nitrate, succinimide, tartaric acid, triethanolamine, methanesulfonic acid and water. However, since tartaric acid has reducing properties, the silver layer obtained is bright, but the plating bath stability is poor.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the anti-tarnishing chemical silver plating solution can realize better stability of plating solution, and the formed plating layer is flat and uniform, has good thickness and white and bright metallic luster, and has better weather resistance.
The technical scheme of the invention for solving the technical problems is as follows: the anti-tarnishing chemical silver plating solution comprises the following components: silver oxide, a copper ion complexing agent, a composite antitarnish agent, sulfamic acid, a stabilizer, an accelerator, a nucleating agent, a wetting agent and deionized water;
the concentration of the silver oxide in the anti-discoloration chemical silver plating solution is 1.2 to 1.5g/L;
the composite antitarnish agent is sodium polystyrene sulfonate and 3,4-ethylenedioxythiophene, and the weight ratio is sodium polystyrene sulfonate: 5363 and 3,4-ethylenedioxythiophene =1 (3~5), and the concentration of the composite antitarnish agent in the silver plating solution is 1 to 3g/L. The composite antitarnish agent can be adsorbed on the surface of the plating layer to form a bright organic film, so that the protective capability of the silver layer is improved.
Further, the copper ion complexing agent is itaconic acid and piperidine, and the weight ratio is itaconic acid: piperidine =1 (3~7), and the concentration of the copper ion complexing agent in the silver plating solution is 6 to 12g/L.
Further, the stabilizer is 1,2,4-triazole and triethyl phosphate, and the weight ratio is 1,2,4-triazole: triethyl phosphate (= (2~5): 1), wherein the concentration of the stabilizer in the silver plating solution is 0.8 to 2.4g/L.
Furthermore, the accelerator is 1,4-butanediol, and the concentration of the accelerator in the silver plating solution is 0.6 to 1.5g/L. The deposition of silver ions can be accelerated, and the efficiency is improved.
Further, the concentration of the sulfamic acid in the silver plating solution is 40 to 60g/L. It can dissolve silver oxide and provide acid environment.
Furthermore, the wetting agent is alkyl glycoside, and the concentration of the wetting agent in the silver plating solution is 3 to 6ml/L calculated by pure alkyl glycoside. The cleanliness in the holes can be improved, and the uniformity of the silver layer is promoted.
Further, the nucleating agent is 4,6-dimethyl-2-mercaptopyrimidine, and the concentration of the nucleating agent in the silver plating solution is 0.2 to 0.5g/L. Can promote the growth of new crystal nucleus and the flatness of the plating layer.
Further, the weight ratio of the accelerator to the nucleating agent is (1~3): 1. Under the proportion, the accelerator and the nucleating agent can play a good synergistic effect, can greatly improve the evenness of a plating layer and improve the dispersion uniformity of silver ions.
The invention also relates to the application of the chemical silver plating solution for surface treatment of a packaging carrier plate and/or a printed circuit board.
The beneficial effects of the invention include: the composite antitarnish agent polystyrene sodium sulfonate and 3,4-ethylenedioxythiophene are selected, and the use ratio is limited to be 1 (3~5), so that the antitarnish ability of silver can be effectively improved, and the service life of a chemical silver circuit board is prolonged. The nucleating agent 4,6-dimethyl-2-mercaptopyrimidine is selected, so that the growth of new crystal nuclei can be promoted, and the flatness of a plating layer can be promoted. The use ratio of the accelerator to the nucleating agent is (1~3): 1, the special ratio has a good synergistic effect, and the accelerator and the nucleating agent can greatly improve the flatness of a plating layer and improve the dispersion uniformity of silver ions.
Drawings
FIG. 1 is surface SEM images of a salt spray test (right) after silver plating and after silver plating in example 1 of the present invention;
FIG. 2 is surface SEM images of the salt spray test (right) after silver plating and after silver plating of comparative example 1;
FIG. 3 is a surface SEM image of the salt spray test (right) after silver plating and after silver plating of comparative example 2;
FIG. 4 is a surface SEM image of the salt spray test (right) after silver plating and after silver plating of comparative example 3;
fig. 5 is a surface SEM image of the salt spray test (right) after silver plating of comparative example 4 (left).
Detailed Description
The present invention will be described in detail with reference to examples, which are only preferred embodiments of the present invention and are not intended to limit the present invention. Unless otherwise specified, the following methods for preparing the silver plating solution were all carried out by conventional mixing and stirring.
Example 1
The anti-tarnishing chemical silver plating solution comprises the following components in percentage by weight: silver oxide, a copper ion complexing agent, a composite antitarnish agent, sulfamic acid, a stabilizer, an accelerator, a nucleating agent, a wetting agent and deionized water;
the concentration of the silver oxide is 1.2g/L; the composite antitarnish agent is sodium polystyrene sulfonate and 3,4-ethylenedioxythiophene, and the weight ratio is sodium polystyrene sulfonate: 3,4-ethylenedioxythiophene =1:3, and the overall concentration of the composite antitarnish agent is 3g/L; the copper ion complexing agent is itaconic acid and piperidine, and the weight ratio is itaconic acid: piperidine =1:3, and the overall concentration of the copper ion complexing agent is 6g/L; the stabilizer is a 1,2,4-triazole and triethyl phosphate compound, the weight ratio is 3:1, and the overall concentration of the stabilizer is 0.8g/L; the accelerator is 1,4-butanediol with the concentration of 0.6g/L; the concentration of the sulfamic acid is 40g/L; the wetting agent is alkyl glycoside, and the concentration is 3ml/L calculated by pure alkyl glycoside; the nucleating agent is 4,6-dimethyl-2-mercaptopyrimidine, and the concentration is 0.2/L; the balance being deionized water.
Example 2
The anti-tarnishing chemical silver plating solution comprises the following components in percentage by weight: silver oxide, a copper ion complexing agent, a composite antitarnish agent, sulfamic acid, a stabilizer, an accelerator, a nucleating agent, a wetting agent and deionized water;
the concentration of the silver oxide is 1.5g/L; the composite antitarnish agent is sodium polystyrene sulfonate and 3,4-ethylenedioxythiophene, and the weight ratio is sodium polystyrene sulfonate: 3,4-ethylenedioxythiophene =1:5, the overall concentration of the composite antitarnish agent is 3g/L; the copper ion complexing agent is itaconic acid and piperidine, and the weight ratio is itaconic acid: piperidine =1:7, and the total concentration of the copper ion complexing agent is 12g/L; the stabilizer is a 1,2,4-triazole and triethyl phosphate compound, the weight ratio is 3:1, and the overall concentration of the stabilizer is 2.4g/L; the accelerator is 1,4-butanediol with the concentration of 1.5g/L; the concentration of the sulfamic acid is 60g/L; the wetting agent is alkyl glycoside, and the concentration is 6ml/L calculated by pure alkyl glycoside; the nucleating agent is 4,6-dimethyl-2-mercaptopyrimidine, and the concentration is 0.5g/L; the balance being deionized water.
Example 3
The anti-tarnishing chemical silver plating solution comprises the following components in percentage by weight: silver oxide, a copper ion complexing agent, a composite antitarnish agent, sulfamic acid, a stabilizer, an accelerator, a nucleating agent, a wetting agent and deionized water;
the concentration of the silver oxide is 1.3g/L; the composite antitarnish agent is sodium polystyrene sulfonate and 3,4-ethylenedioxythiophene, and the weight ratio is sodium polystyrene sulfonate: 3,4-ethylenedioxythiophene =1:4, the overall concentration of the composite antitarnish agent is 2g/L; the copper ion complexing agent is itaconic acid and piperidine, and the weight ratio is itaconic acid: piperidine =1:5, and the overall concentration of the copper ion complexing agent is 9g/L; the stabilizer is a 1,2,4-triazole and triethyl phosphate compound, the weight ratio is 3:1, and the overall concentration of the stabilizer is 1.6g/L; the accelerator is 1,4-butanediol, and the concentration is 0.9g/L; the concentration of the sulfamic acid is 50g/L; the wetting agent is alkyl glycoside, and the concentration is 5ml/L calculated by pure alkyl glycoside; the nucleating agent is 4,6-dimethyl-2-mercaptopyrimidine, and the concentration is 0.3g/L; the balance being deionized water.
Comparative example 1
The anti-tarnishing chemical silver plating solution comprises the following components in percentage by weight: silver oxide, a copper ion complexing agent, a composite antitarnish agent, sulfamic acid, a stabilizer, an accelerator, a nucleating agent, a wetting agent and deionized water;
the concentration of the silver oxide is 1.3g/L; the composite antitarnish agent is sodium polystyrene sulfonate and 3,4-ethylenedioxythiophene, and the weight ratio is sodium polystyrene sulfonate: 3,4-ethylenedioxythiophene =1:4, the overall concentration of the composite antitarnish agent is 2g/L; the copper ion complexing agent is itaconic acid and piperidine, and the weight ratio is itaconic acid: piperidine =1:5, and the total concentration of the copper ion complexing agent is 9g/L; the stabilizer is a 1,2,4-triazole and triethyl phosphate compound, the weight ratio is 3:1, and the overall concentration of the stabilizer is 1.6g/L; the accelerator is 1,4-butanediol with the concentration of 0.9g/L; the concentration of the sulfamic acid is 50g/L; the wetting agent is alkyl glycoside, and the concentration is 5ml/L calculated by pure alkyl glycoside; the nucleating agent is 4,6-dimethyl-2-mercaptopyrimidine, and the concentration is 0.3g/L; the balance being deionized water.
Comparative example 2
The anti-tarnishing chemical silver plating solution comprises the following components in percentage by weight: silver oxide, a copper ion complexing agent, a composite antitarnish agent, sulfamic acid, a stabilizer, a nucleating agent, a wetting agent and deionized water;
the concentration of the silver oxide is 1.3g/L; the composite antitarnish agent is sodium polystyrene sulfonate and 3,4-ethylenedioxythiophene, and the weight ratio is sodium polystyrene sulfonate: 3,4-ethylenedioxythiophene =1:4, the overall concentration of the composite antitarnish agent is 2g/L; the copper ion complexing agent is itaconic acid and piperidine, and the weight ratio is itaconic acid: piperidine =1:5, and the overall concentration of the copper ion complexing agent is 9g/L; the stabilizer is a 1,2,4-triazole and triethyl phosphate compound, the weight ratio is 3:1, and the overall concentration of the stabilizer is 1.6g/L; the concentration of the sulfamic acid is 50g/L; the wetting agent is alkyl glycoside, and the concentration is 5ml/L calculated by pure alkyl glycoside; the nucleating agent is 4,6-dimethyl-2-mercaptopyrimidine, and the concentration is 0.3g/L; the balance being deionized water.
Comparative example 3
The anti-tarnishing chemical silver plating solution comprises the following components in percentage by weight: silver oxide, a copper ion complexing agent, a composite antitarnish agent, sulfamic acid, a stabilizer, an accelerator, a nucleating agent, a wetting agent and deionized water;
the concentration of the silver oxide is 1.3g/L; the composite antitarnish agent is sodium polystyrene sulfonate and 3,4-ethylenedioxythiophene, and the weight ratio is sodium polystyrene sulfonate: 3,4-ethylenedioxythiophene =1:4, the overall concentration of the composite antitarnish agent is 2g/L; the copper ion complexing agent is itaconic acid and piperidine, and the weight ratio is itaconic acid: piperidine =1:5, and the total concentration of the copper ion complexing agent is 9g/L; the stabilizer is a 1,2,4-triazole and triethyl phosphate compound, the weight ratio is 3:1, and the overall concentration of the stabilizer is 1.6g/L; the accelerator is 1,4-butanediol with the concentration of 0.9g/L; the concentration of the sulfamic acid is 50g/L; the wetting agent is alkyl glycoside, and the concentration is 5ml/L calculated by pure alkyl glycoside; (ii) a The balance being deionized water.
Comparative example 4
The anti-tarnishing chemical silver plating solution comprises the following components in percentage by weight: silver oxide, a copper ion complexing agent, a composite antitarnish agent, sulfamic acid, a stabilizer, an accelerator, a nucleating agent, a wetting agent and deionized water;
the concentration of the silver oxide is 1.3g/L; the composite antitarnish agent is sodium polystyrene sulfonate and 3,4-ethylenedioxythiophene, and the weight ratio is sodium polystyrene sulfonate: 3,4-ethylenedioxythiophene =1:4, and the overall concentration of the composite antitarnish agent is 2g/L; the copper ion complexing agent is itaconic acid and piperidine, and the weight ratio is itaconic acid: piperidine =1:5, and the overall concentration of the copper ion complexing agent is 9g/L; the stabilizer is a 1,2,4-triazole and triethyl phosphate compound, the weight ratio is 3:1, and the overall concentration of the stabilizer is 1.6g/L; the accelerator is 1,4-butanediol with the concentration of 0.5g/L; the concentration of the sulfamic acid is 50g/L; the wetting agent is alkyl glycoside, and the concentration is 5ml/L calculated by pure alkyl glycoside; the nucleating agent is 4,6-dimethyl-2-mercaptopyrimidine, and the concentration is 0.1g/L; the balance being deionized water.
Taking a common plate with the same model and subjected to resistance welding, and carrying out the following steps: acid degreasing for 2min, pure water washing, micro-etching for 2min, pure water washing, presoaking for 1min, chemical silver for 2min (soaking by using the anti-discoloration chemical silver plating solution described below), washing and drying. The discoloration prevention test, the silver plating effect test and the stability test were performed on 3 examples and 4 comparative examples of the discoloration prevention chemical silver plating solution.
And (3) anti-discoloration test: 5% sodium chloride solution is used, the indoor temperature is 35 ℃, the pressure temperature of a saturated tank is 47 ℃, the pressure of the saturated tank is 1Kgf, the spraying amount is 1-2mL/h, and the testing time is 10h. The judgment standard is as follows: the silver surface is excellent in white and bright; the silver surface appears white, and the color is good when yellow dots or black dots are accidentally seen; the yellow spots or black spots on the silver surface are obviously increased or decreased; the silver surface shows black spots or yellow spots and is very poor in flake form. The experimental results are as follows:
the SEM pictures of the silver planes of example 1 and comparative examples 1 to 4 before the salt spray test are shown in fig. 1 to 5 (left), respectively, and the corrosion SEM pictures of the silver planes of example 1 and comparative examples 1 to 4 after the salt spray test are shown in fig. 1 to 5 (right), respectively. It can be seen that the plating layer formed by using the invention has better salt spray corrosion resistance and good discoloration prevention effect. It can also be seen that the accelerator and the nucleating agent of the invention improve the evenness of the plating layer and the dispersion uniformity of silver ions, and a synergistic effect exists between the accelerator and the nucleating agent.
And (3) testing the silver plating effect: the electroless silver plating thickness and copper corrosion conditions were tested as follows. Wherein, copper face corrosion conditions test all withdraws silver through withdrawing silver water after silvering, sees the copper face and corrodes the condition: the copper surface has no corrosion phenomenon or has slight pits; slightly more pits, but acceptable as good (pit area less than 10%); pits are clearly very poor (pit area greater than 10%, less than 50%); the copper layer had poor dishing.
It can be seen that the silver plating solution provided by the invention has the advantages of large thickness of the silver layer prepared under the same conditions, high deposition rate in unit time and high efficiency. It can also be seen that the silver deposition effect of the present invention has a better corrosion to the copper surface and the service life of the circuit board has a better expectation.
And (3) stability testing: testing the service cycle of the silver plating solution, wherein 5MTO is excellent; 4MTO is good; 3MTO is poor; 2MTO is the difference; 1MTO is very poor.
It can be seen that the silver plating solution provided by the invention has better stability.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are all within the protection scope of the present invention.
It should be noted that the various features described in the above embodiments may be combined in any suitable manner without departing from the scope of the invention. The invention is not described in detail in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.
Claims (9)
1. The anti-tarnishing chemical silver plating solution is characterized by comprising the following components: silver oxide, a copper ion complexing agent, a composite antitarnish agent, sulfamic acid, a stabilizer, an accelerator, a nucleating agent, a wetting agent and deionized water;
the concentration of the silver oxide in the silver plating solution is 1.2 to 1.5g/L;
the composite antitarnish agent is sodium polystyrene sulfonate and 3,4-ethylenedioxythiophene, and the weight ratio is sodium polystyrene sulfonate: 5363 and 3,4-ethylenedioxythiophene =1 (3~5), and the concentration of the composite antitarnish agent in the silver plating solution is 1 to 3g/L.
2. The silver plating solution according to claim 1, wherein the copper ion complexing agent is itaconic acid and piperidine in a weight ratio of itaconic acid: piperidine =1 (3~7), and the concentration of the copper ion complexing agent in the silver plating solution is 6 to 12g/L.
3. The silver plating solution of claim 1, wherein the stabilizer is 1,2,4-triazole and triethyl phosphate, and the weight ratio is 1,2,4-triazole: triethyl phosphate (= (2~5): 1), wherein the concentration of the stabilizer in the silver plating solution is 0.8 to 2.4g/L.
4. The silver plating solution according to claim 1, wherein the accelerator is 1,4-butanediol, and the concentration in the silver plating solution is 0.6 to 1.5g/L.
5. The silver plating solution according to claim 1, wherein the concentration of the sulfamic acid in the silver plating solution is 40 to 60g/L.
6. The silver plating solution according to claim 1, wherein the wetting agent is an alkylglycoside, and the concentration of the alkylglycoside in the silver plating solution is 3 to 6ml/L.
7. The silver plating solution according to claim 1, wherein the nucleating agent is 4,6-dimethyl-2-mercaptopyrimidine, and the concentration in the silver plating solution is 0.2 to 0.5g/L.
8. The silver plating solution according to claim 1, wherein the weight ratio of the accelerator to the nucleating agent is (1~3): 1.
9. Use of a silver plating solution according to 1~8 in a packaging carrier and/or a printed circuit board for surface treatment.
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| CN111519219A (en) * | 2019-12-21 | 2020-08-11 | 东莞奕创表面处理科技有限公司 | Silver electroplating liquid composite additive and preparation method and application thereof |
| CN112126954A (en) * | 2020-09-30 | 2020-12-25 | 嘉兴学院 | Surface enhanced Raman spectroscopy SERS silver-plated active substrate based on brush plating and preparation method thereof |
| CN114672857A (en) * | 2022-05-30 | 2022-06-28 | 深圳市创智成功科技有限公司 | Preparation method of high-purity copper sulfate and copper electroplating process applied to copper interconnection |
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