CN108754467B - Ruthenium palladium alloy chemical plating solution and plating method and application thereof - Google Patents
Ruthenium palladium alloy chemical plating solution and plating method and application thereof Download PDFInfo
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- CN108754467B CN108754467B CN201810675967.8A CN201810675967A CN108754467B CN 108754467 B CN108754467 B CN 108754467B CN 201810675967 A CN201810675967 A CN 201810675967A CN 108754467 B CN108754467 B CN 108754467B
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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
- C23C18/48—Coating with alloys
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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
Abstract
The invention discloses a ruthenium palladium alloy chemical plating solution, application thereof and a method for chemically plating a ruthenium palladium alloy layer. The ruthenium-palladium alloy electroless plating solution comprises a solvent, water-soluble ruthenium salt with the concentration of 0.1-10 mmol/L, water-soluble palladium salt with the concentration of 0.1-10 mmol/L, a complexing agent with the concentration of 1-20 mmol/L, an auxiliary agent with the concentration of 1-50 mmol/L, hydrazine hydrate with the concentration of 1-20 mmol/L and a pH regulator. The ruthenium palladium alloy electroless plating solution can be applied to electronic devices and printed circuit boards. The method for chemically plating the ruthenium palladium alloy layer comprises the step of placing a substrate in the ruthenium palladium alloy chemical plating solution for plating treatment. The ruthenium-palladium alloy chemical plating solution has good stability, high palladium-ruthenium deposition rate, controllability, high ruthenium content in a plating layer, good quality of the plating layer and good combination with a substrate and a subsequent plating layer. In addition, the chemical plating condition of the ruthenium palladium alloy chemical plating solution is mild.
Description
Technical Field
The invention relates to the technical field of chemical plating, in particular to a ruthenium palladium alloy chemical plating solution and a plating method and application thereof.
Background
In the manufacturing process of electronic devices and printed circuit boards, the surfaces of the devices or the bonding pads of the printed circuit boards need to be treated so as to meet the requirements of corrosion resistance and weldability in the using process of the electronic devices and the printed circuit boards. There are many types of conventional surface treatment methods: the method comprises the processing modes of electroplating, chemical plating and the like, and the types of the plated metals can also be divided into: tin, nickel, silver, palladium, gold, and the like.
The metal palladium has the characteristics of high melting point and high hardness, and has high corrosion resistance, high wear resistance and the like when being applied to the electronic industry, but because the price of the palladium is also very high and is not increased rapidly, a new process needs to be developed, and the consumption of the palladium metal is reduced to further reduce the cost. The metal ruthenium is as noble as the metal palladium, but it is much less expensive. Ruthenium also has many excellent properties compared to palladium, for example: 1) the melting point of Ruthenium (Ruthenium, Ru) is 2334 ℃ which is much higher than the melting point of palladium (1555 ℃; 2) ruthenium has much higher corrosion resistance than metals such as palladium and gold, and is safe even in boiling aqua regia.
Based on the characteristics of high temperature resistance and low cost of ruthenium, chemical ruthenium plating solution is available at present, but in actual production, the pure ruthenium layer generated by the existing chemical ruthenium plating solution has poor weldability, and the reaction rate is not easy to control, thereby affecting the performance stability and weldability of related products. Although attempts have been made to prepare ruthenium-palladium mixed plating solutions, in actual production, it has been found that the ruthenium content of the palladium-ruthenium alloy film produced by the palladium-ruthenium mixed plating solution is significantly lower than that of ruthenium in the palladium-ruthenium mixed plating solution, for example, the ruthenium content of the ruthenium-palladium mixed plating solution accounts for more than 15% of the palladium-ruthenium metal content, but the ruthenium metal content of the plating layer is far lower than 15% and is only 0.3%, and it cannot be determined whether ruthenium is chemically plated or physically entrained in the palladium plating layer, and therefore, the ruthenium-palladium alloy plating layer can hardly be realized by the existing ruthenium-palladium mixed plating solution.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a ruthenium-palladium alloy chemical plating solution, a plating method and application thereof, so as to solve the technical problems that a pure ruthenium layer generated by the existing chemical ruthenium plating solution has poor weldability and reaction rate is not easy to control, and a ruthenium-palladium mixed plating solution can hardly realize a ruthenium-palladium alloy plating layer.
In order to achieve the above object, according to one aspect of the present invention, there is provided a ruthenium palladium alloy electroless plating solution. The ruthenium-palladium alloy electroless plating solution comprises water-soluble ruthenium salt with the concentration of 0.1-10 mmol/L, water-soluble palladium salt with the concentration of 0.1-10 mmol/L, complexing agent with the concentration of 1-20 mmol/L, auxiliary agent with the concentration of 1-50 mmol/L, hydrazine hydrate with the concentration of 1-20 mmol/L, pH regulator and the balance of water.
In another aspect, the invention provides the use of the ruthenium palladium alloy electroless plating solution of the invention. In particular to the application of the ruthenium palladium alloy chemical plating solution in electronic devices and printed circuit boards.
In another aspect, the present invention provides a method for electroless plating of ruthenium-palladium alloy layers. The method for chemically plating the ruthenium palladium alloy layer comprises the step of placing a substrate in the ruthenium palladium alloy chemical plating solution for plating treatment.
Compared with the prior art, the ruthenium-palladium alloy chemical plating solution has good stability, so that no palladium or ruthenium is deposited on the aqueduct wall or other non-activated areas in the plating process, and the plating solution can be kept stable for a long time at room temperature after the plating is finished and the plated piece is taken out. The ruthenium palladium alloy chemical plating solution has high and controllable palladium and ruthenium deposition rate in chemical plating, can be controlled within the range of 0.5-3 mu m/h, has high ruthenium content in a plating layer, has good quality of the plating layer, and is well combined with a substrate and a subsequent plating layer. In addition, the chemical plating condition of the ruthenium palladium alloy chemical plating solution is mild.
The ruthenium-palladium alloy chemical plating solution has the advantages of stable system, high palladium-ruthenium deposition rate, controllability, mild plating conditions, good plating quality, good combination with a substrate and the like, so that the applicability of the ruthenium-palladium alloy chemical plating solution is effectively expanded and enhanced, and the quality of products such as electronic devices, printed circuit boards and the like is improved.
The method for chemically plating the ruthenium-palladium alloy layer adopts the ruthenium-palladium alloy chemical plating solution to plate the substrate to be plated, so that the ruthenium-palladium alloy layer can be deposited on the surface of the substrate, and the ruthenium-palladium alloy layer has high ruthenium content, good quality and good combination with the substrate and a subsequent plating layer. In addition, the plating treatment condition is mild, and the deposition reaction in plating is fast and controllable.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present invention more clearly apparent, the present invention is further described in detail below with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
In one aspect, embodiments of the present invention provide a ruthenium palladium alloy electroless plating solution. The ruthenium palladium alloy electroless plating solution comprises a pH regulator besides a solvent component, and also comprises the following components in concentration:
wherein the water-soluble ruthenium salt and the water-soluble palladium salt contained in the ruthenium-palladium alloy electroless plating solution form a ruthenium source and a palladium source. In one embodiment, the water-soluble ruthenium salt can be RuCl3.3H2O、Ru(NH3)6Cl3、Ru(NH3)3(NO3)3And (RuNO)2(SO4)3At least one of (1). The water-soluble ruthenium salt can be PdCl2·2H2O、Pd(NH3)4Cl2And Pd (NH)3)4SO4At least one of (1). The selected water-soluble ruthenium salt and water-soluble palladium salt have good solubility and dispersibility, can form a stable ruthenium-palladium alloy plating layer in the chemical plating process, and improve the content of ruthenium. In specific embodiments, the concentrations of the water-soluble ruthenium salt and the water-soluble ruthenium salt can be the same or different 0.1, 0.5, 1, 2, 3, 4, 5, 6, 7, 8, 9, 10mmol/L, and the like.
The complexing agent, the adjuvant, the hydrazine hydrate and the pH regulator contained in the ruthenium-palladium alloy chemical plating solution form the auxiliary components of the water-soluble ruthenium salt and the water-soluble palladium salt, so that the uniform dispersion of the water-soluble ruthenium salt and the water-soluble palladium salt can be ensured, and the ruthenium-palladium alloy chemical plating solution has good stability; on the other hand, the ruthenium palladium alloy chemical plating solution has a rapid deposition rate in the plating process, is controllable, can maintain the pH of the plating solution to be stable, such as between 8 and 11, and can generate a ruthenium palladium alloy plating layer with good quality which is well combined with the bottom metal and the subsequent plating layer. In one embodiment, the complexing agent is a 1:1 condensation polymer of triethylene tetramine and salicylaldehyde. In particular embodiments, the concentration of the complexing agent may be 1, 5, 10, 20mmol/L, and the like. In another embodiment, the adjuvant is selected from one or two of sodium nitrite and citraconic acid, and in a specific embodiment, the concentration of the adjuvant can be 1, 5, 10, 15, 20, 25, 30, 35, 40, 45, 50mmol/L and the like. In another embodiment, the concentration of hydrazine hydrate can be 1, 5, 10, 15, 20mmol/L, and the like
The pH adjusting agent contained in the ruthenium palladium alloy electroless plating solution plays a role in stabilizing the pH of the ruthenium palladium alloy electroless plating solution, and in one embodiment, the pH adjusting agent may include an acidic pH adjusting agent and/or a basic pH adjusting agent. The pH value of the ruthenium palladium alloy chemical plating solution is stabilized in an alkaline range of 8-11 through the adjusting action of an acidic pH regulator and an alkaline pH regulator. In a particular embodiment, the acidic pH adjusting agent may be citric acid. The alkaline pH adjuster may be ethylenediamine.
In the above embodiments, the solvent of the ruthenium palladium alloy electroless plating solution is the solvent carrier of the above components, which can be water directly, such as deionized water.
Therefore, the ruthenium palladium alloy chemical plating solution can be stable in system, high in deposition rate, controllable, high in ruthenium content in the plating layer, good in quality of the plating layer and good in combination with a substrate and a subsequent plating layer through the synergistic effect of the components.
Based on the ruthenium-palladium alloy electroless plating solution, in another aspect, the embodiment of the invention also provides an application method of the ruthenium-palladium alloy electroless plating solution. Specifically, the ruthenium palladium alloy electroless plating solution is applied to electronic devices and printed circuit boards. Thus, the ruthenium palladium alloy layer is plated on the corresponding substrate to be plated, thereby ensuring the quality and the working stability of the corresponding products such as electronic devices, printed circuit boards and the like.
Based on the ruthenium palladium alloy electroless plating solution, the embodiment of the invention also provides a method for electroless plating of a ruthenium palladium alloy layer. The method comprises the step of placing the substrate in the ruthenium palladium alloy electroless plating solution for plating treatment. Therefore, the method for chemically plating the ruthenium-palladium alloy layer adopts the ruthenium-palladium alloy chemical plating solution to plate the substrate to be plated, so that the ruthenium-palladium alloy layer can be deposited on the surface of the substrate, and the ruthenium-palladium alloy layer has high ruthenium content, good plating quality and good combination with the substrate and a subsequent plating layer. In addition, the plating treatment has mild condition, and the deposition reaction in plating is fast and controllable. As an example, the temperature of the plating process is 55-70 deg.C. In addition, the detection proves that the rate of the ruthenium palladium alloy layer generated by deposition of the plating treatment can be controlled within the range of 0.5-3 mu m/h, and the ruthenium palladium alloy layer generated by deposition of the plating treatment contains 12-60% of ruthenium in percentage by mole. Therefore, the method for chemically plating the ruthenium-palladium alloy layer has the advantages that the rate of depositing the ruthenium-palladium alloy layer is high and controllable, the content of ruthenium in the generated ruthenium-palladium alloy layer is high, the content of palladium is effectively reduced on the premise of ensuring the quality of the ruthenium-palladium alloy layer, and the cost is reduced.
The embodiments of the present invention will now be described in further detail with reference to specific examples.
Example 1
The embodiment provides a palladium-ruthenium alloy chemical plating solution and a method for chemically plating a ruthenium-palladium alloy layer. The palladium ruthenium alloy electroless plating solution contains the components as shown in the following table 1. The plating method of the palladium-ruthenium alloy chemical plating solution or the method for chemically plating the ruthenium-palladium alloy layer comprises the following steps:
after the circuit board with the nickel as the substrate is activated on the surface properly, the palladium-ruthenium alloy chemical plating step is carried out, and the composition and conditions of the palladium-ruthenium alloy chemical plating solution are shown in table 1. After the pH value of the solution is adjusted to a set value by citric acid or ethylenediamine solution, the solution is heated to the plating temperature of 65 ℃, after 5 minutes of chemical plating, a plated part is taken out, cleaned and dried, and after analysis and test, the bonding force between metal layers is strong, the weldability is good, the thickness of the palladium-ruthenium alloy layer is about 0.16 μm, the ruthenium content is about 59 percent, the palladium content is about 41 percent, and the plating solution is kept stable in the plating process.
TABLE 1 palladium ruthenium alloy electroless plating solution
| Chemical reagent | Concentration of |
| Ruthenium chloride (RuCl)3·3H2O) | 9.2mmol/L |
| Palladium chloride (PdCl)2·2H2O) | 5.6mmol/L |
| Sodium nitrite (NaNO)2) | 30.4mmol/L |
| Complexing agent A | 15.0mmol/L |
| Hydrazine hydrate (N)2H4.H2O) | 15.0mmol/L |
| pH | 10.8 |
Example 2
The embodiment provides a palladium-ruthenium alloy chemical plating solution and a method for chemically plating a ruthenium-palladium alloy layer. The palladium ruthenium alloy electroless plating solution contains the components shown in table 2. The plating method of the palladium-ruthenium alloy chemical plating solution or the method for chemically plating the ruthenium-palladium alloy layer comprises the following steps:
plating was performed with reference to the plating method of example 1, in which all the other processing steps were the same as those of example 1 except that the plating time was changed to 15 minutes. After the chemical plating is finished, analysis tests show that the solderability is good, the thickness of the palladium ruthenium alloy layer is increased to be about 0.35 mu m, the ruthenium content is about 60 percent, the palladium content is about 40 percent, and the plating solution is kept stable in the plating process.
TABLE 2 palladium ruthenium alloy electroless plating solution
| Chemical reagent | Concentration of |
| Ruthenium ammonium nitrate (Ru (NH)3)3(NO3)3) | 9.6mmol/L |
| Palladium ammonia sulfate (Pd (NH)3)4SO4) | 8.6mmol/L |
| Sodium nitrite (NaNO)2) | 28.0mmol/L |
| Complexing agent A | 18.0mmol/L |
| Hydrazine hydrate (N)2H4.H2O) | 15.0mmol/L |
| pH | 10.8 |
Example 3
The embodiment provides a palladium-ruthenium alloy chemical plating solution and a method for chemically plating a ruthenium-palladium alloy layer. The palladium ruthenium alloy electroless plating solution contains the components as shown in the following table 3. The plating method of the palladium-ruthenium alloy chemical plating solution or the method for chemically plating the ruthenium-palladium alloy layer comprises the following steps:
after the copper is used as a substrate device and is activated on the surface properly, the palladium-ruthenium alloy chemical plating step is carried out, and the chemical plating solution composition and conditions are shown in table 3. After the pH value of the solution is adjusted to a set value by citric acid or ethylenediamine solution, the solution is heated to the plating temperature of 60 ℃, after 20 minutes of chemical plating, a plated part is taken out, cleaned and dried, and analyzed and tested, the bonding force between metal layers is strong, the neutral salt spray test in 72 hours has good corrosion resistance, the thickness of the palladium-ruthenium alloy layer is about 0.26 mu m, the ruthenium content is about 14 percent, the palladium content is about 86 percent, and the plating solution is kept stable in the plating process.
TABLE 3 palladium ruthenium alloy electroless plating solution
Example 4
The embodiment provides a palladium-ruthenium alloy chemical plating solution and a method for chemically plating a ruthenium-palladium alloy layer. The palladium ruthenium alloy electroless plating solution contains the components as shown in the following table 4. The plating method of the palladium-ruthenium alloy chemical plating solution or the method for chemically plating the ruthenium-palladium alloy layer comprises the following steps:
the plating was performed by referring to the plating method of example 3, in which all other processing steps and the chemical plating process were the same as those of example 1, the bonding force between the metal layers was strong after the chemical plating was completed, the corrosion resistance was good in a 72-hour neutral salt spray test, the thickness of the palladium ruthenium alloy layer was about 0.21 μm, the ruthenium content was about 58%, the palladium content was about 42%, and the plating solution was maintained stable during the plating process.
TABLE 4 palladium ruthenium alloy electroless plating solution
| Chemical reagent | Concentration of |
| Ruthenium ammonium nitrate (Ru (NH)3)3(NO3)3) | 9.0mmol/L |
| Palladium ammonia sulfate (Pd (NH)3)4SO4) | 0.6mmol/L |
| Citraconic acid (CH3) C (COOH) CH (COOH) | 45.0mmol/L |
| Complexing agent A | 18.0mmol/L |
| Hydrazine hydrate (N)2H4.H2O) | 20.0mmol/L |
| pH | 8.5 |
Example 5
The embodiment provides a palladium-ruthenium alloy chemical plating solution and a method for chemically plating a ruthenium-palladium alloy layer. The palladium ruthenium alloy electroless plating solution contained the components as shown in table 5 below. The plating method of the palladium-ruthenium alloy chemical plating solution or the method for chemically plating the ruthenium-palladium alloy layer comprises the following steps:
the plating was performed by referring to the plating method of example 3, in which all other processing steps and the chemical plating process were the same as those of example 1, the bonding force between the metal layers was strong after the chemical plating was completed, the corrosion resistance was good in a 72-hour neutral salt spray test, the thickness of the palladium ruthenium alloy layer was about 0.18 μm, the ruthenium content was about 35%, the palladium content was about 65%, and the plating solution was maintained stable during the plating process.
TABLE 5 palladium ruthenium alloy electroless plating solution
| Chemical reagent | Concentration of |
| Ruthenium (Ru (NH) ammonium chloride3)6Cl3) | 0.5mmol/L |
| Palladium chloride (PdCl)2·2H2O) | 1.5mmol/L |
| Sodium nitrite (NaNO)2) | 5.0mmol/L |
| Complexing agent A | 10.0mmol/L |
| Hydrazine hydrate (N)2H4.H2O) | 5.0mmol/L |
| pH | 10.2 |
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 and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (5)
1. The ruthenium-palladium alloy electroless plating solution comprises a solvent and is characterized by further comprising water-soluble ruthenium salt with the concentration of 0.1-10 mmol/L, water-soluble palladium salt with the concentration of 0.1-10 mmol/L, a complexing agent with the concentration of 1-20 mmol/L, an auxiliary agent with the concentration of 1-50 mmol/L, hydrazine hydrate with the concentration of 1-20.0 mmol/L and a pH regulator; the pH regulator comprises an acidic pH regulator and an alkaline pH regulator; the acidic pH regulator is citric acid; the alkaline pH regulator is ethylenediamine, the pH of the ruthenium-palladium alloy chemical plating solution is 10.2, the complexing agent is a 1:1 condensation polymer of triethylene tetramine and salicylaldehyde, and the auxiliary agent is one or a combination of two of sodium nitrite and citraconic acid.
2. The ruthenium palladium alloy electroless plating solution according to claim 1 wherein: the water-soluble ruthenium salt is RuCl3.3H2O、Ru(NH3)6Cl3、Ru(NH3)3(NO3)3And (RuNO)2(SO4)3At least one of; and/or
The water-soluble ruthenium salt is PdCl2·2H2O、Pd(NH3)4Cl2And Pd (NH)3)4SO4At least one of (1).
3. Use of the ruthenium palladium alloy electroless plating solution for ruthenium palladium alloy according to any one of claims 1 to 2 in electronic devices, printed circuit boards, etc.
4. A method for electroless plating of a ruthenium palladium alloy layer, comprising the step of subjecting a substrate to plating treatment by placing the substrate in the ruthenium palladium alloy electroless plating solution according to any one of claims 1 to 3.
5. The method of claim 4, wherein: the temperature of the plating treatment is 55-70 ℃; and/or
The rate of depositing and generating the ruthenium palladium alloy layer in the plating treatment is 0.5-3 mu m/h; and/or
The ruthenium palladium alloy layer deposited after the plating treatment contains 12-60% of ruthenium by mol percent.
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| CN101135052B (en) * | 2006-08-30 | 2010-08-18 | 中国科学院大连化学物理研究所 | Method for preparing metallic complex film |
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| EP2192405B1 (en) * | 2008-11-26 | 2012-02-22 | ATOTECH Deutschland GmbH | Method for control of stabilizer additives in electroless metal and metal alloy plating electrolytes |
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| CN1740390A (en) * | 2005-09-09 | 2006-03-01 | 清华大学 | Chemical plating activating process and metal depositing process therewith |
| CN105723015A (en) * | 2013-10-28 | 2016-06-29 | 东洋钢钣株式会社 | Alloy-plate-coated material, and method for producing alloy-plate-coated material |
| EP3184667A1 (en) * | 2015-12-23 | 2017-06-28 | Uniwersytet Warszawski | Means for carrying out electroless metal deposition with atomic sub-monolayer precision |
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