CN114411127A - Chemical nickel plating pretreatment activating solution based on ruthenium-palladium system and preparation method thereof - Google Patents
Chemical nickel plating pretreatment activating solution based on ruthenium-palladium system and preparation method thereof Download PDFInfo
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- CN114411127A CN114411127A CN202210091541.4A CN202210091541A CN114411127A CN 114411127 A CN114411127 A CN 114411127A CN 202210091541 A CN202210091541 A CN 202210091541A CN 114411127 A CN114411127 A CN 114411127A
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- ruthenium
- palladium
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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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses an activating solution for chemical nickel plating pretreatment based on a ruthenium-palladium system and a preparation method thereof, wherein the activating solution comprises the following raw materials in mass concentration: ruthenium salt 10-15mg/L, palladium salt 10-15mg/L, concentrated sulfuric acid 10000-20000mg/L, complexing agent 20-40mg/L, stabilizer 12-30mg/L, surfactant 15-60mg/L, dispersant 25-50mg/L, and carrying assistant 16-50 mg/L. The semi-ruthenium semi-palladium is used as an active main body to replace full palladium, and comprises a surfactant, a complexing agent, a dispersing agent, a stabilizing agent, a carrying assistant and the like; the complexing agent system and the dispersing agent system realize the high-concentration copper ion tolerance of the semi-ruthenium semi-palladium activating solution and good wetting in the micro blind holes and the step grooves; the stabilizer obviously prolongs the service life of the bath solution; the carrier adjuvant can cooperate with the catalytic action of palladium and ruthenium.
Description
Technical Field
The invention relates to the technical field of chemical nickel plating, in particular to an activating solution for chemical nickel plating pretreatment based on a ruthenium-palladium system and a preparation method thereof.
Background
On one hand, the market share of electroless nickel and gold is large, 40 percent, and meanwhile, because palladium is expensive and the surface activation treatment of the line width and the line distance below 1.5-2.5mil is easy to cause the diffusion plating phenomenon, the research and the development of a new activating solution for realizing the surface treatment of high-end electronic product circuits on FPC and PCB have become necessary requirements for the development of market industry.
Patent No. CN110724943A discloses that the invention provides a palladium-free activating solution before chemical nickel plating on copper surface, a preparation method and a nickel plating method, the palladium-free activating solution includes: nickel salt, reducing agent, complexing agent, stabilizing agent and pH regulator; the palladium-free activating solution before chemical nickel plating on the copper surface, the preparation method and the nickel plating method utilize the non-palladium activating plating solution to pre-plate a nickel plating layer with catalytic activity on the copper surface of the printed circuit board, so that the subsequent chemical nickel plating link can be continued, and the chemical nickel plating layer obtained by non-palladium activation has better corrosion resistance than the chemical nickel plating layer obtained by palladium activation.
However, the patent and the existing activating solution still have certain defects, such as: firstly, the method is not suitable for processing the surface with the line width and the line distance of less than 2.5 mil; secondly, the phenomena of diffusion plating and plating leakage are easy to occur in palladium activation; and the copper ion tolerance is lower than 120 ppm.
An effective solution to the problems in the related art has not been proposed yet.
Disclosure of Invention
Aiming at the problems in the related art, the invention provides an activating solution for chemical nickel plating pretreatment based on a ruthenium-palladium system and a preparation method thereof, so as to overcome the technical problems in the prior related art.
Therefore, the invention adopts the following specific technical scheme:
according to one aspect of the invention, the activating solution for the electroless nickel plating pretreatment based on the ruthenium-palladium system comprises the following raw materials in mass concentration:
ruthenium salt 10-15mg/L, palladium salt 10-15mg/L, concentrated sulfuric acid 10000-20000mg/L, complexing agent 20-40mg/L, stabilizer 12-30mg/L, surfactant 15-60mg/L, dispersant 25-50mg/L and carrying assistant 16-50 mg/L. Further, the ruthenium salt includes at least one of ruthenium acetate or ruthenium oxide.
Further, the palladium salt comprises at least one of palladium sulfate or palladium chloride.
Further, the complexing agent comprises a ruthenium complexing agent, a copper ion complexing agent and a palladium ion complexing agent, and the ratio of the ruthenium complexing agent to the copper ion complexing agent to the palladium ion complexing agent is 2: 1: 2.
further, the ruthenium complexing agent is ethylenediamine tetraacetic acid; the copper ion complexing agent is an amine compound composition, and the amine compound composition comprises piperidine and cyclohexylamine; the palladium ions are methylene glycol compounds.
Further, the stabilizer comprises zirconia and phosphoric acid, and the mass concentration ratio of the zirconia to the phosphoric acid is 1: 2.
further, the surfactant is fatty alcohol-polyoxyethylene ether.
Further, the dispersing agent is polyethylene glycol.
Further, the carrier adjuvant is polyacrylic acid.
According to another aspect of the invention, the preparation method of the electroless nickel plating pretreatment activating solution based on the ruthenium-palladium system is also provided, and comprises the following steps:
s1, preparing a surfactant and sulfuric acid according to the corresponding proportion concentration ratio to form a first agent;
s2, mixing a complexing agent, a stabilizing agent, ruthenium salt and palladium salt according to the corresponding mass concentration ratio to form an agent B;
s3, mixing the concentration of the dispersant according to the corresponding mass concentration ratio to form a third component;
s4, forming a butyl agent by using the carrying auxiliary agent according to the corresponding mass concentration ratio;
s5, under the normal temperature environment, according to the ratio of 1: 1: 1: 1, and the first agent, the second agent, the third agent and the fourth agent are opened by 10 percent per liter.
The invention has the beneficial effects that: the semi-ruthenium semi-palladium is used as an active main body to replace full palladium, and comprises a surfactant, a complexing agent, a dispersing agent, a stabilizing agent, a carrying assistant and the like; developing a semi-ruthenium semi-palladium complexing agent system and a dispersing agent system to realize high-concentration copper ion tolerance of the semi-ruthenium semi-palladium activating solution and good wetting in micro blind holes and step grooves; the development of a semiruthenium semipalladium stabilizer can obviously prolong the service life of the bath solution, and the development of a carrying auxiliary agent can coordinate the catalytic action of palladium and ruthenium.
Through the reasonable configuration of the proportion of the ruthenium ions, the palladium ions and various additives, the activating solution can be suitable for surface treatment of line width and line distance of 1.5-2.5mil, the phenomena of diffusion plating and plating leakage after nickel plating are avoided, and the phenomena of diffusion plating and plating leakage easily caused by palladium activation in the prior art are effectively improved, so that the stability and the effect of nickel plating are greatly improved; and ensure that the copper ion tolerance is higher than 150ppm, thereby further enhancing the stability of the activating solution and enriching application scenes.
Specifically, the ruthenium salt provides ruthenium ions; the palladium salt provides palladium ions; the surfactant plays a role in cleaning and promoting the liquid medicine to permeate into the holes; the dispersing agent is adsorbed on the surface of the base material, and plays a role in promoting the reduction and dispersion of ruthenium ions and palladium ions; the carrying auxiliary agent can cooperate with the dispersing agent to carry palladium ions and ruthenium ions which are orderly distributed at an activation point to play a catalytic role.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
FIG. 1 is a flow chart of the preparation method of the activation solution for electroless nickel plating pretreatment based on ruthenium-palladium system according to the embodiment of the invention.
Detailed Description
According to one embodiment of the present invention, the following problems are solved: 1. surface treatment suitable for line width and line distance of 1.5-2.5mil is developed; 2. the phenomena of diffusion plating and plating leakage can not occur after nickel plating; 3. the copper ion tolerance is higher than 150ppm, and the electroless nickel plating pretreatment activating solution based on a ruthenium-palladium system is provided and comprises the following raw materials in mass concentration:
ruthenium salt 10-15mg/L, palladium salt 10-15mg/L, concentrated sulfuric acid 10000-20000mg/L, complexing agent 20-40mg/L, stabilizer 12-30mg/L, surfactant 15-60mg/L, dispersant 25-50mg/L and carrying assistant 16-50 mg/L.
In one embodiment, the ruthenium salt includes at least one of ruthenium acetate or ruthenium oxide, which is primarily used to provide ruthenium ions.
In one embodiment, the palladium salt comprises at least one of palladium sulfate or palladium chloride, which is used primarily to provide palladium ions.
In addition, the concentrated sulfuric acid is used to provide an acidic environment that prevents adsorption of the ink on ruthenium ions and palladium ions.
In one embodiment, the complexing agent comprises a ruthenium complexing agent, a copper ion complexing agent and a palladium ion complexing agent, and the ratio of the ruthenium complexing agent to the copper ion complexing agent to the palladium ion complexing agent is 2: 1: 2.
in one embodiment, the ruthenium complexing agent is ethylenediaminetetraacetic acid (EDTA);
the copper ion complexing agent is an amine compound composition, and the amine compound composition comprises piperidine and cyclohexylamine;
the palladium ions are methylene glycol compounds.
In one embodiment, the stabilizer comprises zirconia and phosphoric acid, and the mass concentration ratio is 1: 2.
in one embodiment, the surfactant is fatty alcohol-polyoxyethylene ether, which is primarily intended to clean and facilitate penetration of the liquid into the pores.
In one embodiment, the dispersing agent is polyethylene glycol, and the polyethylene glycol is adsorbed on the surface of the substrate to promote the reduction and dispersion of ruthenium ions and palladium ions.
In one embodiment, the carrier adjuvant is polyacrylic acid, and the carrier adjuvant can cooperate with the dispersant to carry palladium ions and ruthenium ions in ordered distribution for catalysis at the activation point.
According to another embodiment of the invention, the preparation method of the electroless nickel plating pretreatment activating solution based on the ruthenium-palladium system comprises the following steps:
s1, preparing a surfactant and sulfuric acid according to the corresponding proportion concentration ratio to form a first agent;
s2, mixing a complexing agent, a stabilizing agent, ruthenium salt and palladium salt according to the corresponding mass concentration ratio to form an agent B;
s3, mixing the concentration of the dispersant according to the corresponding mass concentration ratio to form a third component;
s4, forming a butyl agent by using the carrying auxiliary agent according to the corresponding mass concentration ratio;
s5, under the normal temperature environment, according to the ratio of 1: 1: 1: 1, and the first agent, the second agent, the third agent and the fourth agent are opened by 10 percent per liter.
Example one
10-15mg/L of ruthenium salt, 10-15mg/L of palladium salt, 10-20g/L, EDTA8-16mg/L of concentrated sulfuric acid, 4-8mg/L of piperidine, 8-16mg/L of 1, 3-propylene glycol, 4-10mg/L of zirconium oxide, 8-20mg/L of phosphoric acid, 15-60mg/L of fatty alcohol-polyoxyethylene ether, 25-50mg/L of polyethylene glycol and 16-50mg/L of polyacrylic acid.
Comparative example 1
10-15mg/L of ruthenium salt, 10-15mg/L of palladium salt, 10-20g/L, EDTA8-16mg/L of concentrated sulfuric acid, 4-8mg/L of piperidine, 8-16mg/L of 1, 3-propylene glycol, 4-10mg/L of zirconium oxide, 8-20mg/L of phosphoric acid and 15-60mg/L of fatty alcohol-polyoxyethylene ether.
Comparative example No. two
10-15mg/L of ruthenium salt, 10-15mg/L of palladium salt, 10-20g/L, EDTA8-16mg/L of concentrated sulfuric acid, 4-8mg/L of piperidine, 8-16mg/L of 1, 3-propylene glycol, 15-60mg/L of fatty alcohol-polyoxyethylene ether, 25-50mg/L of polyethylene glycol and 16-50mg/L of polyacrylic acid.
Comparative example No. three
10-15mg/L of ruthenium salt, 10-15mg/L of palladium salt, 10-20g/L, EDTA8-16mg/L of concentrated sulfuric acid, 4-10mg/L of zirconium oxide, 8-20mg/L of phosphoric acid, 15-60mg/L of fatty alcohol-polyoxyethylene ether, 25-50mg/L of polyethylene glycol and 16-50mg/L of polyacrylic acid.
Through the preparation and observation of example one and comparative example one, and comparative example two and comparative example three, the following results and data were obtained:
the results obtained in the first embodiment can prevent the phenomena of diffusion plating and plating leakage after the surface treatment nickel plating with the line width and the line distance of 1.5-2.5mil, and the copper ion tolerance is higher than 150ppm after 5 MTO;
comparative example one the phenomena of partial diffusion plating and plating leakage appear after the nickel plating of the surface treatment with the line width and the line distance of less than 3mil/3 mil;
the solution of the second comparative example has poor stability and uses less than 3 MTO;
the third bath solution of the comparative example is stable and has copper ion tolerance lower than 120 ppm.
Therefore, the comparison shows that the raw materials and the mixture ratio thereof used in the first embodiment have the best effect, have wider scene, do not generate the phenomena of diffusion plating and plating leakage, and have the highest stability.
In summary, by means of the above technical solution of the present invention, half ruthenium and half palladium are used as active main bodies instead of all palladium, including surfactants, complexing agents, dispersants, stabilizers, carrying aids, etc.; developing a semi-ruthenium semi-palladium complex system and a dispersant system to realize high-concentration copper ion tolerance of the semi-ruthenium semi-palladium activation solution and good wetting in micro blind holes and step grooves; the development of a semiruthenium semipalladium stabilizer can obviously prolong the service life of the bath solution, and the development of a carrying auxiliary agent can coordinate the catalytic action of palladium and ruthenium.
Through the reasonable configuration of the proportion of the ruthenium ions, the palladium ions and various additives, the activating solution can be suitable for surface treatment of line width and line distance of 1.5-2.5mil, the phenomena of diffusion plating and plating leakage after nickel plating are avoided, and the phenomena of diffusion plating and plating leakage easily caused by palladium activation in the prior art are effectively improved, so that the stability and the effect of nickel plating are greatly improved; and ensure that the copper ion tolerance is higher than 150ppm, thereby further enhancing the stability of the activating solution and enriching application scenes.
Specifically, the ruthenium salt provides ruthenium ions; the palladium salt provides palladium ions; the surfactant plays a role in cleaning and promoting the liquid medicine to permeate into the holes; the dispersing agent is adsorbed on the surface of the base material, and plays a role in promoting the reduction and dispersion of ruthenium ions and palladium ions; the carrying auxiliary agent can cooperate with the dispersing agent to carry palladium ions and ruthenium ions which are orderly distributed at an activation point to play a catalytic role.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. The chemical nickel plating pretreatment activating solution based on a ruthenium-palladium system is characterized by comprising the following raw materials in mass concentration:
ruthenium salt 10-15mg/L, palladium salt 10-15mg/L, concentrated sulfuric acid 10000-20000mg/L, complexing agent 20-40mg/L, stabilizer 12-30mg/L, surfactant 15-60mg/L, dispersant 25-50mg/L and carrying assistant 16-50 mg/L.
2. The electroless nickel plating pretreatment activating solution according to claim 1, wherein the ruthenium salt comprises at least one of ruthenium acetate or ruthenium oxide.
3. An electroless nickel plating pretreatment activating solution according to claim 1, characterized in that the palladium salt comprises at least one of palladium sulfate or palladium chloride.
4. The electroless nickel plating pretreatment activating solution based on the ruthenium-palladium system according to claim 1, wherein the complexing agent comprises a ruthenium complexing agent, a copper ion complexing agent and a palladium ion complexing agent, and the ratio of the ruthenium complexing agent to the copper ion complexing agent to the palladium ion complexing agent is 2: 1: 2.
5. the electroless nickel plating pretreatment activating solution based on the ruthenium-palladium system according to claim 4, wherein the ruthenium complexing agent is ethylenediaminetetraacetic acid;
the copper ion complexing agent is an amine compound composition, and the amine compound composition comprises piperidine and cyclohexylamine;
the palladium ions are methylene glycol compounds.
6. The electroless nickel plating pretreatment activating solution based on the ruthenium-palladium system as claimed in claim 1, wherein the stabilizing agent comprises zirconia and phosphoric acid, and the mass concentration ratio of the zirconia to the phosphoric acid is 1: 2.
7. the electroless nickel plating pretreatment activating solution based on the ruthenium-palladium system as claimed in claim 1, wherein the surfactant is fatty alcohol-polyoxyethylene ether.
8. The electroless nickel plating pretreatment activating solution based on the ruthenium-palladium system according to claim 1, characterized in that the dispersing agent is polyethylene glycol.
9. The electroless nickel plating pretreatment activating solution according to the ruthenium-palladium system as claimed in claim 1, wherein the carrying assistant is polyacrylic acid.
10. The preparation method of the electroless nickel plating pretreatment activating solution based on the ruthenium-palladium system is used for preparing the electroless nickel plating pretreatment activating solution based on the ruthenium-palladium system in claim 1, and is characterized by comprising the following steps of:
s1, preparing a surfactant and sulfuric acid according to the corresponding proportion concentration ratio to form a first agent;
s2, mixing a complexing agent, a stabilizing agent, ruthenium salt and palladium salt according to the corresponding mass concentration ratio to form an agent B;
s3, mixing the concentration of the dispersant according to the corresponding mass concentration ratio to form a third component;
s4, forming a butyl agent by using the carrying auxiliary agent according to the corresponding mass concentration ratio;
s5, under the normal temperature environment, according to the ratio of 1: 1: 1: 1, and the first agent, the second agent, the third agent and the fourth agent are opened by 10 percent per liter.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115491664A (en) * | 2022-09-13 | 2022-12-20 | 广东利尔化学有限公司 | Ionic palladium activator for vertical copper deposition wire and preparation method thereof |
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