CN114411127B - 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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- CN114411127B CN114411127B CN202210091541.4A CN202210091541A CN114411127B CN 114411127 B CN114411127 B CN 114411127B CN 202210091541 A CN202210091541 A CN 202210091541A CN 114411127 B CN114411127 B CN 114411127B
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- palladium
- ruthenium
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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
-
- 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 a ruthenium-palladium system-based chemical nickel plating pretreatment activating solution and a preparation method thereof, wherein the activating solution comprises the following raw materials in mass concentration: 10-15mg/L of ruthenium salt, 10-15mg/L of palladium salt, 10000-20000mg/L of concentrated sulfuric acid, 20-40mg/L of complexing agent, 12-30mg/L of stabilizer, 15-60mg/L of surfactant, 25-50mg/L of dispersing agent and 16-50mg/L of carrying auxiliary agent. By using half ruthenium and half palladium as an active main body to replace full palladium, the full palladium comprises a surfactant, a complexing agent, a dispersing agent, a stabilizing agent, a carrying auxiliary agent and the like; the complexing agent system and the dispersing agent system realize high-concentration copper ion tolerance of the semi-ruthenium and 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 auxiliary agent can cooperate with the catalysis of palladium and ruthenium.
Description
Technical Field
The invention relates to the technical field of electroless nickel plating, in particular to an electroless nickel plating pretreatment activating solution based on a ruthenium-palladium system and a preparation method thereof.
Background
On one hand, the market share of the electroless nickel gold is large, the ratio of the electroless nickel gold is 40%, meanwhile, due to the high price of palladium, the surface activation treatment of the wire width of less than 1.5-2.5mil is easy to cause a plating phenomenon, and in order to realize the surface treatment of high-end electronic product circuits on FPC and PCB, the research and development of new activation liquid has become a necessary requirement for the development of market industry.
Patent number CN110724943A discloses that the invention provides a palladium-free activating solution before electroless nickel plating of copper surfaces, a preparation method and a nickel plating method, and the palladium-free activating solution comprises the following components: nickel salt, reducing agent, complexing agent, stabilizing agent and pH regulator; the method utilizes the non-palladium activation plating solution to preplate a nickel plating layer with catalytic activity on the copper surface of the printed circuit board, so that the subsequent chemical nickel plating ring can be continuously carried out, the chemical nickel plating layer obtained by non-palladium activation has better corrosion resistance than the chemical nickel plating layer obtained by palladium activation, the non-palladium activation solution related by the method contains two reducing agents of boron and phosphorus and a certain amount of stabilizing agent, the high reduction rate is ensured, meanwhile, the stability of the solution can still be ensured, and the method is utilized to treat the printed circuit board with double-sided windowing, so that the occurrence of plating leakage probability of the printed circuit board which is treated by the non-palladium activation is greatly reduced.
However, the patent and the prior activating solution still have certain disadvantages, such as: (1) it is not suitable for processing surfaces with linewidth to linewidth of less than 2.5 mil; (2) the palladium activation is easy to generate the phenomenon of seepage plating and missing plating; (3) copper ion tolerance is less than 120ppm.
For the problems in the related art, no effective solution has been proposed at present.
Disclosure of Invention
Aiming at the problems in the related art, the invention provides an electroless nickel plating pretreatment activating solution based on a ruthenium-palladium system and a preparation method thereof, so as to overcome the technical problems in the prior art.
For this purpose, the invention adopts the following specific technical scheme:
according to one aspect of the invention, there is provided an electroless nickel pretreatment activation solution based on a ruthenium-palladium system, comprising the following raw material composition in mass concentration:
10-15mg/L of ruthenium salt, 10-15mg/L of palladium salt, 10000-20000mg/L of concentrated sulfuric acid, 20-40mg/L of complexing agent, 12-30mg/L of stabilizer, 15-60mg/L of surfactant, 25-50mg/L of dispersing agent and 16-50mg/L of carrying auxiliary agent. 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 proportion 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 piperidine; the palladium ion complexing agent is a methylene glycol compound.
Further, the stabilizer comprises zirconium oxide and phosphoric acid, and the mass concentration ratio is 1:2.
further, the surfactant is fatty alcohol polyoxyethylene ether.
Further, the dispersing agent is polyethylene glycol.
Further, the carrier auxiliary agent is polyacrylic acid.
According to another aspect of the present invention, there is also provided a method for preparing an electroless nickel plating pretreatment activating solution based on a ruthenium-palladium system, comprising the steps of:
s1, preparing a surfactant and concentrated sulfuric acid according to a concentration ratio in a corresponding proportion to form an alpha-olefin;
s2, mixing the complexing agent, the stabilizer, ruthenium salt and palladium salt according to the proportion of the corresponding mass concentration to form an agent B;
s3, proportioning the concentration of the dispersing agent according to the corresponding mass concentration to form a third agent;
s4, proportioning the carrying auxiliary agent according to the corresponding mass concentration to form a bulk agent;
s5, under the normal temperature environment, according to the following formula 1:1:1:1, and the solution is prepared according to the proportion of opening cylinders, and the agent A, the agent B, the agent C and the agent Ding Ji are opened by 10 percent per liter of opening cylinders.
The beneficial effects of the invention are as follows: by using half ruthenium and half palladium as an active main body to replace full palladium, the full palladium comprises a surfactant, a complexing agent, a dispersing agent, a stabilizing agent, a carrying auxiliary agent and the like; developing a half ruthenium half palladium complexing agent system and a dispersing agent system, and realizing good wetting of a half ruthenium half palladium activating solution in a micro blind hole and a step groove, wherein the tolerance of copper ions is high; the development of the semi-ruthenium and semi-palladium stabilizer can obviously improve the service life of the tank liquor, and the development of the carrying auxiliary agent can cooperate with the catalytic action of palladium and ruthenium.
Through the reasonable configuration of the proportion of the ruthenium ions, the palladium ions and the various additives thereof, the activating solution can be suitable for the surface treatment with the line width of 1.5-2.5mil, so that the phenomenon of diffusion plating and plating leakage can not occur after nickel plating, the phenomenon of easy diffusion plating and plating leakage during palladium activation in the prior art is effectively improved, and the stability and effect of nickel plating are greatly improved; and ensures that the copper ion tolerance is higher than 150ppm, thereby further enhancing the stability of the activating solution and enriching the application scene.
Specifically, ruthenium salts provide ruthenium ions; the palladium salt provides palladium ions; the surfactant has the functions of cleaning and promoting the penetration of the liquid medicine into the holes; the dispersing agent is adsorbed on the surface of the substrate to promote the reduction and dispersion of ruthenium ions and palladium ions; the carrier auxiliary agent can be cooperated with the dispersing agent, and the carrier palladium ions and ruthenium ions are orderly distributed at the activation points 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 that are 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 other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a flow chart of a method for preparing an electroless nickel pretreatment activation liquid based on a ruthenium-palladium system in accordance with an embodiment of the invention.
Detailed Description
According to one embodiment of the present invention, the following problems are solved: 1. developing surface treatment suitable for line width and line spacing of 1.5-2.5 mil; 2. the phenomenon of seepage plating and missing plating can not occur after nickel plating; 3. 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:
10-15mg/L of ruthenium salt, 10-15mg/L of palladium salt, 10000-20000mg/L of concentrated sulfuric acid, 20-40mg/L of complexing agent, 12-30mg/L of stabilizer, 15-60mg/L of surfactant, 25-50mg/L of dispersing agent and 16-50mg/L of carrying auxiliary agent.
In one embodiment, the ruthenium salt comprises at least one of ruthenium acetate or ruthenium oxide, which is primarily used to provide ruthenium ions.
In one embodiment, the palladium salt includes at least one of palladium sulfate or palladium chloride, which is primarily used to provide palladium ions.
In addition, the concentrated sulfuric acid is used for providing an acidic environment and preventing ink adsorption 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 ethylenediamine tetraacetic acid (EDTA);
the copper ion complexing agent is piperidine;
the palladium ion complexing agent is a methylene glycol compound.
In one embodiment, the stabilizer comprises zirconium oxide and phosphoric acid, and the mass concentration ratio is 1:2.
in one embodiment, the surfactant is a fatty alcohol polyoxyethylene ether, which is primarily intended to clean and promote penetration of the liquid medicine into the pores.
In one embodiment, the dispersing agent is polyethylene glycol, and the dispersing agent plays a role in promoting the reduction and dispersion of ruthenium ions and palladium ions through adsorption on the surface of the substrate.
In one embodiment, the carrier aid is polyacrylic acid, and the carrier aid can be cooperated with a dispersing agent to carry palladium ions and ruthenium ions to be orderly distributed at an activation point for catalysis.
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 concentrated sulfuric acid according to a concentration ratio in a corresponding proportion to form an alpha-olefin;
s2, mixing the complexing agent, the stabilizer, ruthenium salt and palladium salt according to the proportion of the corresponding mass concentration to form an agent B;
s3, proportioning the concentration of the dispersing agent according to the corresponding mass concentration to form a third agent;
s4, proportioning the carrying auxiliary agent according to the corresponding mass concentration to form a bulk agent;
s5, under the normal temperature environment, according to the following formula 1:1:1:1, and the solution is prepared according to the proportion of opening cylinders, and the agent A, the agent B, the agent C and the agent Ding Ji are opened by 10 percent per liter of opening cylinders.
Example 1
10-15mg/L of ruthenium salt, 10-15mg/L of palladium salt, 10-20g/L, EDTA-16 mg/L of concentrated sulfuric acid, 4-8mg/L of piperidine, 8-16mg/L of 1, 3-propanediol, 4-10mg/L of zirconia, 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 one
10-15mg/L of ruthenium salt, 10-15mg/L of palladium salt, 10-20g/L, EDTA-16 mg/L of concentrated sulfuric acid, 4-8mg/L of piperidine, 8-16mg/L of 1, 3-propanediol, 4-10mg/L of zirconia, 8-20mg/L of phosphoric acid and 15-60mg/L of fatty alcohol polyoxyethylene ether.
Comparative example two
10-15mg/L of ruthenium salt, 10-15mg/L of palladium salt, 10-20g/L, EDTA-16 mg/L of concentrated sulfuric acid, 4-8mg/L of piperidine, 8-16mg/L of 1, 3-propanediol, 15-60mg/L of fatty alcohol polyoxyethylene ether, 25-50mg/L of polyethylene glycol and 16-50mg/L of polyacrylic acid.
Comparative example three
10-15mg/L of ruthenium salt, 10-15mg/L of palladium salt, 10-20g/L, EDTA-16 mg/L of concentrated sulfuric acid, 4-10mg/L of zirconia, 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.
The following results and data were obtained by preparing and observing examples one and comparative examples one, comparative examples two and comparative examples three:
the first embodiment obtains the result that the phenomenon of seepage plating and missing plating can not occur after the surface treatment nickel plating with the wire width of 1.5-2.5mil, and the tolerance of copper ions is higher than 150ppm after 5 MTO;
comparative example one in which a part of the plating film was left to bleed after the surface treatment nickel plating at a line width of 3mil/3mil or less;
the stability of the second tank liquor of the comparative example is poor, and the use of the second tank liquor is less than 3MTO;
the three tank liquor of the comparative example is stable and the copper ion tolerance is lower than 120ppm.
Therefore, the raw materials and the proportions thereof used in the first embodiment have the best effect, no matter the composition has wider prospect, no phenomenon of seepage plating and missing plating occurs, and the highest stability is achieved.
In summary, by means of the above technical solution of the present invention, by using half ruthenium and half palladium as active bodies instead of full palladium, it includes surfactants, complexing agents, dispersants, stabilizers, carrying aids, etc.; developing a half ruthenium half palladium complexing system and a dispersing agent system, and realizing good wetting of a half ruthenium half palladium activating solution in a micro blind hole and a step groove, wherein the tolerance of copper ions is high; the development of the semi-ruthenium and semi-palladium stabilizer can obviously improve the service life of the tank liquor, and the development of the carrying auxiliary agent can cooperate with the catalytic action of palladium and ruthenium.
Through the reasonable configuration of the proportion of the ruthenium ions, the palladium ions and the various additives thereof, the activating solution can be suitable for the surface treatment with the line width of 1.5-2.5mil, so that the phenomenon of diffusion plating and plating leakage can not occur after nickel plating, the phenomenon of easy diffusion plating and plating leakage during palladium activation in the prior art is effectively improved, and the stability and effect of nickel plating are greatly improved; and ensures that the copper ion tolerance is higher than 150ppm, thereby further enhancing the stability of the activating solution and enriching the application scene.
Specifically, ruthenium salts provide ruthenium ions; the palladium salt provides palladium ions; the surfactant has the functions of cleaning and promoting the penetration of the liquid medicine into the holes; the dispersing agent is adsorbed on the surface of the substrate to promote the reduction and dispersion of ruthenium ions and palladium ions; the carrier auxiliary agent can be cooperated with the dispersing agent, and the carrier palladium ions and ruthenium ions are orderly distributed at the activation points to play a catalytic role.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.
Claims (5)
1. The electroless nickel plating pretreatment activating solution based on the ruthenium-palladium system is characterized by comprising the following raw materials in mass concentration:
10-15mg/L of ruthenium salt, 10-15mg/L of palladium salt, 10000-20000mg/L of concentrated sulfuric acid, 20-40mg/L of complexing agent, 12-30mg/L of stabilizer, 15-60mg/L of surfactant, 25-50mg/L of dispersing agent and 16-50mg/L of carrying auxiliary agent;
the complexing agent comprises a ruthenium complexing agent, a copper ion complexing agent and a palladium ion complexing agent, and the proportion of the ruthenium complexing agent to the copper ion complexing agent to the palladium ion complexing agent is 2:1:2;
the stabilizer comprises zirconium oxide and phosphoric acid, wherein the mass concentration ratio of the zirconium oxide to the phosphoric acid is 1:2;
the surfactant is fatty alcohol polyoxyethylene ether;
the dispersing agent is polyethylene glycol;
the carrier auxiliary agent is polyacrylic acid.
2. The electroless nickel pretreatment activation liquid based on a ruthenium-palladium system according to claim 1, wherein the ruthenium salt comprises at least one of ruthenium acetate or ruthenium oxide.
3. The electroless nickel plating pretreatment activation liquid based on ruthenium-palladium system according to claim 1, wherein the palladium salt comprises at least one of palladium sulfate or palladium chloride.
4. The electroless nickel pretreatment activating solution based on ruthenium-palladium system according to claim 1, wherein the ruthenium complexing agent is ethylenediamine tetraacetic acid;
the copper ion complexing agent is piperidine;
the palladium ion complexing agent is a methylene glycol compound.
5. A method for preparing an electroless nickel pretreatment activating solution based on a ruthenium-palladium system, which is used for preparing the electroless nickel pretreatment activating solution based on the ruthenium-palladium system in claim 1, and is characterized by comprising the following steps:
s1, preparing a surfactant and concentrated sulfuric acid according to a concentration ratio in a corresponding proportion to form an alpha-olefin;
s2, mixing the complexing agent, the stabilizer, ruthenium salt and palladium salt according to the proportion of the corresponding mass concentration to form an agent B;
s3, proportioning the concentration of the dispersing agent according to the corresponding mass concentration to form a third agent;
s4, proportioning the carrying auxiliary agent according to the corresponding mass concentration to form a bulk agent;
s5, under the normal temperature environment, according to the following formula 1:1:1:1, and the solution is prepared according to the proportion of opening cylinders, and the agent A, the agent B, the agent C and the agent Ding Ji are opened by 10 percent per liter of opening cylinders.
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| CN202210091541.4A CN114411127B (en) | 2022-01-26 | 2022-01-26 | Chemical nickel plating pretreatment activating solution based on ruthenium-palladium system and preparation method thereof |
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