CN115595567B - Anti-discoloration chemical silver plating solution - Google Patents
Anti-discoloration chemical silver plating solution Download PDFInfo
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- CN115595567B CN115595567B CN202211052998.0A CN202211052998A CN115595567B CN 115595567 B CN115595567 B CN 115595567B CN 202211052998 A CN202211052998 A CN 202211052998A CN 115595567 B CN115595567 B CN 115595567B
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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
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Abstract
The invention belongs to the field of printed circuit board preparation, and particularly relates to a color-changing-preventing chemical silver plating solution. The silver plating solution comprises the following components: silver oxide, a copper ion complexing agent, a composite anti-discoloration 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 1.2-1.5 g/L; the compound anti-discoloration agent is sodium polystyrene sulfonate and 3, 4-ethylenedioxythiophene, and the weight ratio of the compound anti-discoloration agent is sodium polystyrene sulfonate: 3, 4-ethylenedioxythiophene=1 (3-5), wherein the concentration of the composite anti-discoloration agent in silver plating liquid is 1-3 g/L. The silver plating solution provided by the invention can realize better plating solution stability, and the formed plating layer is flat and uniform, has good thickness, white and bright metallic luster and better weather resistance.
Description
Technical Field
The invention belongs to the field of printed circuit board preparation, and particularly relates to a color-changing-preventing chemical silver plating solution.
Background
As a surface treatment process for packaging carrier boards and printed circuit board boards, electroless 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 particularly has the greatest significance in 5G substrate application. Chemical silver plating is used in electronic device assembly, but is easy to oxidize and discolor after silver plating and is easy to cause electrochemical migration phenomenon, and in order to meet production requirements in recent years, a plurality of new silver plating processes are continuously issued, and the method is simple to operate and low in cost, and the process flow mainly comprises acid degreasing, pure water washing, microetching, pure water washing, presoaking, chemical silver leaching, pure water washing, hot water washing and drying.
At present, the main problem of chemical silver is still that the chemical silver is easy to be influenced by atmospheric pollution gas, such as blackening, yellowing and other color-changing reactions 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 PCB chemical silver is only half a year, the application range of the PCB chemical silver is greatly limited, but in 5G construction, the silver has the best effect of conveying 5G frequency, and therefore, the application prospect of the chemical silver is very wide.
The prior art chemical silver plating solution can be exemplified by a silver plating solution ammonium citrate system described in patent ZL201310312530.5, the pH value of the silver plating solution ammonium citrate system is from 8.2 to 10.2, the silver plating solution ammonium citrate system is slightly alkaline to moderately alkaline, although the silver plating solution ammonium citrate system can achieve certain stability, the silver plating solution ammonium citrate system cannot be held if used for a long time, and the obtained silver layer is not white and bright enough. 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 higher, and the plating solution stability is not high. The silver plating solution described in patent zl201210270962.X is composed of silver nitrate, succinimide, tartaric acid, triethanolamine, methylsulfonic acid and water. However, since tartaric acid has reducibility, the obtained silver layer is bright, but the plating solution stability is poor.
Disclosure of Invention
The technical problems to be solved by the invention are as follows: the anti-discoloration chemical silver plating solution can realize better plating solution stability, and the formed plating layer is even and uniform, has good thickness and white and bright metallic luster, and has better weather resistance.
The technical scheme for solving the technical problems is as follows: the anti-discoloration chemical silver plating solution comprises the following components: silver oxide, a copper ion complexing agent, a composite anti-discoloration 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 1.2-1.5 g/L;
the compound anti-discoloration agent is sodium polystyrene sulfonate and 3, 4-ethylenedioxythiophene, and the weight ratio of the compound anti-discoloration agent is sodium polystyrene sulfonate: 3, 4-ethylenedioxythiophene=1 (3-5), wherein the concentration of the composite anti-discoloration agent in silver plating liquid is 1-3 g/L. The composite anti-discoloration agent can be adsorbed on the surface of the plating layer to form a layer of 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 6-12 g/L.
Further, the stabilizer is 1,2, 4-triazole and triethyl phosphate, and the weight ratio of the stabilizer is 1,2, 4-triazole: triethyl phosphate= (2-5): 1, wherein the concentration of the stabilizing agent in the silver plating solution is 0.8-2.4 g/L.
Further, the accelerator is 1, 4-butanediol, and the concentration of the accelerator in silver plating liquid is 0.6-1.5 g/L. Can accelerate the deposition of silver ions and improve the efficiency.
Further, the concentration of sulfamic acid in the silver plating solution is 40-60 g/L. Acts to dissolve the silver oxide and provides an acidic environment.
Further, the wetting agent is alkyl glycoside, and the concentration of the wetting agent in silver plating solution is 3-6 ml/L based on pure alkyl glycoside. Can improve the cleanliness in the holes and promote the uniformity of the silver layer.
Further, the nucleating agent is 4, 6-dimethyl-2-mercaptopyrimidine, and the concentration of the nucleating agent in silver plating liquid is 0.2-0.5 g/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. In this proportion, the accelerator and the nucleating agent can have better synergistic effect, can greatly improve the flatness of the coating and improve the dispersion uniformity of silver ions.
The invention also relates to the application of the electroless silver plating solution for surface treatment of packaging carrier boards and/or printed circuit boards.
The beneficial effects of the invention include: the composite anti-discoloration agent sodium polystyrene sulfonate and 3, 4-ethylenedioxythiophene are selected, the use ratio is limited to 1 (3-5), the anti-discoloration capability of silver can be effectively improved, and the service life of the chemical silver circuit board is prolonged. The nucleating agent 4, 6-dimethyl-2-mercaptopyrimidine is selected to promote the growth of new crystal nucleus and the flatness of the coating. The use ratio of the accelerator to the nucleating agent is (1-3): 1, the special ratio plays a good synergistic effect, and the accelerator and the nucleating agent can greatly improve the flatness of the coating and improve the dispersion uniformity of silver ions.
Drawings
FIG. 1 is a surface SEM image of the silver plated (left) and salt spray test (right) of example 1 of the present invention;
FIG. 2 is a surface SEM image of the salt spray test (right) after silver plating of comparative example 1 (left);
FIG. 3 is a surface SEM image of the salt spray test (right) after silver plating of comparative example 2 (left);
FIG. 4 is a surface SEM image of the salt spray test (right) after silver plating of comparative example 3;
fig. 5 is a surface SEM image of comparative example 4 after silver plating (left) and salt spray test after silver plating (right).
Detailed Description
The present invention will be described in detail with reference to the following examples, which are only preferred embodiments of the present invention and are not limiting thereof. The following silver plating solution preparation methods are all conventional mixing and stirring methods unless otherwise specified.
Example 1
Each liter of the anti-tarnish chemical silvering liquid comprises the following components: silver oxide, a copper ion complexing agent, a composite anti-discoloration 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 compound anti-discoloration agent is sodium polystyrene sulfonate and 3, 4-ethylenedioxythiophene, and the weight ratio of the compound anti-discoloration agent is sodium polystyrene sulfonate: 3, 4-ethylenedioxythiophene=1:3, the overall concentration of the composite anti-tarnish agent is 3g/L; the copper ion complexing agent is itaconic acid and piperidine, and the weight ratio of the itaconic acid is: piperidine=1:3, the concentration of the copper ion complexing agent as a whole is 6g/L; the stabilizer is a compound of 1,2, 4-triazole and triethyl phosphate, the weight ratio is 3:1, and the integral concentration of the stabilizer is 0.8g/L; the accelerator is 1, 4-butanediol, and the concentration is 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 of deionized water.
Example 2
Each liter of the anti-tarnish chemical silvering liquid comprises the following components: silver oxide, a copper ion complexing agent, a composite anti-discoloration 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 compound anti-discoloration agent is sodium polystyrene sulfonate and 3, 4-ethylenedioxythiophene, and the weight ratio of the compound anti-discoloration agent is sodium polystyrene sulfonate: 3, 4-ethylenedioxythiophene=1:5, the overall concentration of the composite anti-tarnish agent is 3g/L; the copper ion complexing agent is itaconic acid and piperidine, and the weight ratio of the itaconic acid is: piperidine=1:7, the concentration of the copper ion complexing agent as a whole is 12g/L; the stabilizer is a compound of 1,2, 4-triazole and triethyl phosphate, the weight ratio is 3:1, and the integral concentration of the stabilizer is 2.4g/L; the accelerator is 1, 4-butanediol, and the concentration is 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 of deionized water.
Example 3
Each liter of the anti-tarnish chemical silvering liquid comprises the following components: silver oxide, a copper ion complexing agent, a composite anti-discoloration 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 compound anti-discoloration agent is sodium polystyrene sulfonate and 3, 4-ethylenedioxythiophene, and the weight ratio of the compound anti-discoloration agent is sodium polystyrene sulfonate: 3, 4-ethylenedioxythiophene=1:4, the overall concentration of the composite anti-tarnish agent is 2g/L; the copper ion complexing agent is itaconic acid and piperidine, and the weight ratio of the itaconic acid is: piperidine=1:5, the concentration of the copper ion complexing agent as a whole is 9g/L; the stabilizer is a compound of 1,2, 4-triazole and triethyl phosphate, the weight ratio is 3:1, and the integral 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 of deionized water.
Comparative example 1
Each liter of the anti-tarnish chemical silvering liquid comprises the following components: silver oxide, a copper ion complexing agent, a composite anti-discoloration 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 compound anti-discoloration agent is sodium polystyrene sulfonate and 3, 4-ethylenedioxythiophene, and the weight ratio of the compound anti-discoloration agent is sodium polystyrene sulfonate: 3, 4-ethylenedioxythiophene=1:4, the overall concentration of the composite anti-tarnish agent is 2g/L; the copper ion complexing agent is itaconic acid and piperidine, and the weight ratio of the itaconic acid is: piperidine=1:5, the concentration of the copper ion complexing agent as a whole is 9g/L; the stabilizer is a compound of 1,2, 4-triazole and triethyl phosphate, the weight ratio is 3:1, and the integral 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 of deionized water.
Comparative example 2
Each liter of the anti-tarnish chemical silvering liquid comprises the following components: silver oxide, a copper ion complexing agent, a composite anti-discoloration 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 compound anti-discoloration agent is sodium polystyrene sulfonate and 3, 4-ethylenedioxythiophene, and the weight ratio of the compound anti-discoloration agent is sodium polystyrene sulfonate: 3, 4-ethylenedioxythiophene=1:4, the overall concentration of the composite anti-tarnish agent is 2g/L; the copper ion complexing agent is itaconic acid and piperidine, and the weight ratio of the itaconic acid is: piperidine=1:5, the concentration of the copper ion complexing agent as a whole is 9g/L; the stabilizer is a compound of 1,2, 4-triazole and triethyl phosphate, the weight ratio is 3:1, and the integral 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 of deionized water.
Comparative example 3
Each liter of the anti-tarnish chemical silvering liquid comprises the following components: silver oxide, a copper ion complexing agent, a composite anti-discoloration 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 compound anti-discoloration agent is sodium polystyrene sulfonate and 3, 4-ethylenedioxythiophene, and the weight ratio of the compound anti-discoloration agent is sodium polystyrene sulfonate: 3, 4-ethylenedioxythiophene=1:4, the overall concentration of the composite anti-tarnish agent is 2g/L; the copper ion complexing agent is itaconic acid and piperidine, and the weight ratio of the itaconic acid is: piperidine=1:5, the concentration of the copper ion complexing agent as a whole is 9g/L; the stabilizer is a compound of 1,2, 4-triazole and triethyl phosphate, the weight ratio is 3:1, and the integral 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 method comprises the steps of carrying out a first treatment on the surface of the The balance of deionized water.
Comparative example 4
Each liter of the anti-tarnish chemical silvering liquid comprises the following components: silver oxide, a copper ion complexing agent, a composite anti-discoloration 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 compound anti-discoloration agent is sodium polystyrene sulfonate and 3, 4-ethylenedioxythiophene, and the weight ratio of the compound anti-discoloration agent is sodium polystyrene sulfonate: 3, 4-ethylenedioxythiophene=1:4, the overall concentration of the composite anti-tarnish agent is 2g/L; the copper ion complexing agent is itaconic acid and piperidine, and the weight ratio of the itaconic acid is: piperidine=1:5, the concentration of the copper ion complexing agent as a whole is 9g/L; the stabilizer is a compound of 1,2, 4-triazole and triethyl phosphate, the weight ratio is 3:1, and the integral concentration of the stabilizer is 1.6g/L; the accelerator is 1, 4-butanediol, and the concentration is 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 of deionized water.
Taking a common plate with the same model after resistance welding, and carrying out the following steps: acid degreasing for 2min, pure water washing, microetching for 2min, pure water washing, presoaking for 1min, chemical silver for 2min (soaking with the anti-discoloration chemical silver plating solution described below), water washing and drying. The anti-tarnish electroless silver plating solution was subjected to an anti-tarnish test, a silver plating effect test, and a stability test for 3 examples and 4 comparative examples.
And (3) color change prevention test: and 5% sodium chloride solution is used, the indoor temperature is 35 ℃, the saturated barrel pressure is 47 ℃, the saturated barrel pressure is 1Kgf, the spraying amount is 1-2 mL/h, and the testing time is 10h. The evaluation criteria are: the silver surface is white and bright; the silver surface is white, and even yellow points or black points are good; the silver surface presents yellow points or black points which are obviously increased to be poor; the silver surface appears as black or yellow dots and is poorly flaky. The experimental results are as follows:
the SEM images of the silver surfaces of example 1 and comparative examples 1 to 4 are shown in fig. 1 to 5 (left), respectively, before salt spray testing, and the SEM images of the silver surfaces of example 1 and comparative examples 1 to 4 are shown in fig. 1 to 5 (right), respectively, after salt spray testing. It can be seen that the coating formed by using the method has better salt spray corrosion resistance and good anti-discoloration effect. It can also be seen that the accelerator and the nucleating agent of the invention both improve the flatness of the coating and the dispersion uniformity of silver ions, and have a synergistic effect between the accelerator and the nucleating agent.
Silver plating effect test: electroless silver plating thickness and copper corrosion conditions were tested as follows. The copper surface corrosion condition test is that silver is removed through silver removing water after silver plating, and the copper surface corrosion condition is seen: the copper surface is free from corrosion phenomenon or has slight pits; the pits were slightly more but acceptable (pit area less than 10%); pits are obviously much worse (pit area is more than 10%, less than 50%); copper layer dishing is poor.
It can be seen that the silver plating solution provided by the invention has the advantages of larger silver layer thickness, high deposition rate in unit time and higher efficiency. It can also be seen that the silver deposition effect of the invention has better corrosion condition on the copper surface, and the service life of the circuit board has better expectancy.
Stability test: testing the service cycle of the silver plating solution, wherein 5MTO is optimal; 4MTO was good; 3MTO was poor; 2MTO is poor; 1MTO was 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 above, but the present invention is not limited to the specific details of the above embodiments, and various simple modifications can be made to the technical solution of the present invention within the scope of the technical concept of the present invention, and all the simple modifications belong to the protection scope of the present invention.
In addition, the specific features described in the above embodiments may be combined in any suitable manner without contradiction. The various possible combinations of the invention are not described in detail in order to avoid unnecessary repetition.
Moreover, any combination of the various embodiments of the invention can be made without departing from the spirit of the invention, which should also be considered as disclosed herein.
Claims (3)
1. The anti-discoloration chemical silver plating solution is characterized by comprising the following components: silver oxide, a copper ion complexing agent, a composite anti-discoloration 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 1.2-1.5 g/L;
the copper ion complexing agent is itaconic acid and piperidine, and the weight ratio of the itaconic acid is: piperidine=1 (3-7), the concentration of the copper ion complexing agent in silver plating solution is 6-12 g/L;
the compound anti-discoloration agent is sodium polystyrene sulfonate and 3, 4-ethylenedioxythiophene, and the weight ratio of the compound anti-discoloration agent is sodium polystyrene sulfonate: 3, 4-ethylenedioxythiophene=1, (3-5), the concentration of the compound anti-discoloration agent in silver plating solution is 1-3 g/L;
the concentration of the sulfamic acid in the silver plating solution is 40-60 g/L;
the stabilizer is 1,2, 4-triazole and triethyl phosphate, and the weight ratio of the stabilizer is 1,2, 4-triazole: triethyl phosphate= (2-5): 1, wherein the concentration of the stabilizing agent in the silver plating solution is 0.8-2.4 g/L;
the weight ratio of the accelerator to the nucleating agent is (1-3) 1, the accelerator is 1, 4-butanediol, the concentration of the accelerator in silver plating liquid is 0.6-1.5 g/L, the nucleating agent is 4, 6-dimethyl-2-mercaptopyrimidine, and the concentration of the nucleating agent in silver plating liquid is 0.2-0.5 g/L.
2. Silver plating solution according to claim 1, characterized in that the wetting agent is an alkyl glycoside, the concentration in the silver plating solution being 3-6 ml/L, calculated as pure alkyl glycoside.
3. Use of a silver plating solution according to any of claims 1-2 for surface treatment of packaging carrier boards and/or printed circuit boards.
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