WO2017064874A1 - 無電解白金めっき液 - Google Patents

無電解白金めっき液 Download PDF

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Publication number
WO2017064874A1
WO2017064874A1 PCT/JP2016/056047 JP2016056047W WO2017064874A1 WO 2017064874 A1 WO2017064874 A1 WO 2017064874A1 JP 2016056047 W JP2016056047 W JP 2016056047W WO 2017064874 A1 WO2017064874 A1 WO 2017064874A1
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platinum
electroless
plating solution
acid
platinum plating
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English (en)
French (fr)
Japanese (ja)
Inventor
友人 加藤
秀人 渡邊
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Kojima Chemicals Co Ltd
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Kojima Chemicals Co Ltd
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Priority to EP16855128.1A priority Critical patent/EP3363928A4/en
Priority to US15/767,817 priority patent/US20180305819A1/en
Publication of WO2017064874A1 publication Critical patent/WO2017064874A1/ja
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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
    • C23C18/44—Coating with noble metals using reducing agents

Definitions

  • the present invention relates to an electroless platinum plating solution.
  • an electroless platinum plating solution contains dinitrodiamine platinum or dinitrotetraammine platinum as a platinum salt, ethylenediamine or ammonia as a complexing agent, and hydrazine monohydrate or sodium borohydride as a reducing agent.
  • dinitrodiamine platinum or dinitrotetraammine platinum as a platinum salt
  • ethylenediamine or ammonia as a complexing agent
  • hydrazine monohydrate or sodium borohydride as a reducing agent.
  • Dinitrodiamine platinum and dinitrotetraammine platinum are sparingly soluble in water. Therefore, by adding ethylenediamine or ammonia as a complexing agent to the electroless platinum plating solution, a platinum complex in which ethylenediamine or ammonia is coordinated to platinum is formed and dissolved in water.
  • metal ions or metal complexes can be reduced on the surface of the plating substrate to deposit a metal.
  • a reducing agent for adding a reducing agent to the electroless platinum plating solution, metal ions or metal complexes can be reduced on the surface of the plating substrate to deposit a metal.
  • the platinum complex in which ethylenediamine or ammonia is coordinated to platinum is not easily reduced, hydrazine monohydrate or sodium borohydride having a strong reducing action is added to the electroless platinum plating solution as a reducing agent.
  • hydrazine monohydrate and sodium borohydride have too much reducing power, there is a problem that platinum is precipitated in the plating solution due to the reduction of the platinum complex and hydrogen is generated in accordance with the reduction reaction. .
  • the stability of the solution is improved by adding heavy metal ions such as lead and thallium and thiol compounds as stabilizers.
  • the concentration control of the heavy metal ions and thiol compounds is necessary, the operation of the plating solution becomes complicated.
  • the heavy metal ions are harmful to the human body and may be co-deposited on the deposited platinum film to lower the film purity.
  • ammonia gas is generated from the plating solution with use, the working environment is lowered by the odor accompanying the generation of ammonia gas.
  • an object of the present invention is to provide an electroless platinum plating solution that can obtain excellent solution stability without using heavy metal ions or thiol compounds and can prevent generation of ammonia gas. There is.
  • the inventors of the present invention have found that the conventional electroless platinum plating solution decreases the stability of the solution for the following reason. That is, in a conventional electroless platinum plating solution, a platinum complex is formed by coordination of ethylenediamine or ammonia used as a complexing agent to platinum ions. Since ethylenediamine or ammonia forms a strong complex with platinum ions, a reducing agent with a strong reducing action is required to reduce the platinum complex and deposit it on the surface of the plating substrate. As a result, the electroless platinum plating solution is reduced and decomposed by the reducing power of the reducing agent having a strong reducing action. Therefore, the present inventors have achieved the above problem by employing the following electroless platinum plating solution.
  • the electroless platinum plating solution of the present invention includes a water-soluble platinum compound and one or more reducing agents selected from the group consisting of formalin, glucose, formic acid, and formate.
  • the water-soluble platinum compound includes platinum (II) chloride, platinum (II) chloride, platinum (II) chloride, platinum (IV) chloride, and chloride.
  • platinum (IV) acid platinum chloride (IV) acid salt
  • hexahydroxoplatinum (IV) acid platinum chloride (IV) acid salt
  • dichlorotetraammineplatinum (II) A platinum compound is preferred.
  • the electroless platinum plating solution according to the present invention preferably contains an organic acid as a complexing agent.
  • the organic acid is preferably one or more compounds selected from aliphatic hydroxy acids having a molecular weight of 90 to 500.
  • the platinum compound since a water-soluble platinum compound is used, the platinum compound generates a platinum complex even if it does not contain a complexing agent that strongly forms a complex with platinum ions such as ethylenediamine and ammonia. Almost dissolved in water.
  • a platinum complex produced from a water-soluble platinum compound is easily reduced as compared with a platinum complex in which ethylenediamine or ammonia is coordinated to platinum produced by a conventional electroless platinum plating solution. For this reason, even if formalin, glucose, and formate having a weak reducing action are used as the reducing agent, the platinum complex can be easily reduced.
  • formalin, glucose, formic acid, and formate as reducing agents all have a weaker reducing action than hydrazine monohydrate and sodium borohydride. For this reason, the electroless platinum plating solution is not decomposed by the reducing agent. Therefore, the electroless platinum plating solution can obtain excellent solution stability as compared with the conventional electroless platinum plating solution without using heavy metal ions or thiol compounds. Also, formalin, glucose, formic acid, and formate are all suitable in that the amount of hydrogen generation is small compared to hydrazine monohydrate and sodium borohydride as conventional reducing agents.
  • the electroless platinum plating solution does not contain a compound capable of generating ammonia gas such as ethylenediamine and ammonia, generation of ammonia gas can be prevented.
  • FIG. 2 is an SEM image of a platinum electroless coating obtained by electroless plating treatment with an electroless platinum plating solution of Example 1.
  • FIG. 3 is an SEM image of a platinum electroless coating obtained by electroless plating treatment with an electroless platinum plating solution of Example 2.
  • the electroless platinum plating solution of the present invention is an aqueous solution containing a water-soluble platinum compound and one or more reducing agents selected from the group consisting of formalin, glucose, formic acid, and formate.
  • water-soluble platinum compound examples include platinum (II) chloride, platinum (II) chloride, platinum (II) chloride, platinum (IV) chloride, platinum (IV) acid, and platinum chloride (IV).
  • Acid salt hexahydroxoplatinum (IV) acid, hexahydroxoplatinum (IV) acid salt, one or more water-soluble platinum compounds selected from the group consisting of dichlorotetraammineplatinum (II).
  • the electroless platinum plating solution preferably contains the water-soluble platinum compound in the range of 0.0005 mol / L to 0.05 mol / L, and in the range of 0.0025 mol / L to 0.01 mol / L. It is more preferable to contain. If the content of the water-soluble platinum compound in the electroless platinum plating solution is less than 0.0005 mol / L, it may be difficult to form a platinum electroless coating or the plating rate may be reduced. When L is exceeded, although the plating itself can be performed satisfactorily, the economic efficiency decreases.
  • Platinum chloride (IV) is easily dissolved in the electroless platinum plating solution to form a platinum complex represented by the following formula (1).
  • the platinum complexes represented by the above formulas (1) and (2) are more susceptible to reduction as compared with platinum complexes in which ethylenediamine is coordinated to platinum produced by a conventional electroless platinum plating solution. .
  • the electroless platinum plating solution does not need to use a reducing agent having a strong reducing action, and even if a reducing agent having a weak reducing action is used, the platinum complex can be easily reduced.
  • One or more reducing agents selected from the group consisting of formalin, glucose, formic acid, and formate all reduce the platinum complex represented by the above formulas (1) and (2), although the reducing action is small. It is possible to make it easy to do.
  • the decomposition products generated in the reduction reaction are mainly carbon dioxide and water, and there is an advantage that the amount of hydrogen generation is small compared to hydrazine monohydrate or sodium borohydride.
  • the electroless platinum plating solution is adjusted to a pH range of 6.5 to 12.0 as will be described later, but the reducing agent can be used over the entire pH range.
  • the electroless platinum plating solution preferably contains the reducing agent in a range of 0.1 mol / L to 1.0 mol / L, and in a range of 0.2 mol / L to 0.8 mol / L. More preferably.
  • the content of the reducing agent in the electroless platinum plating solution is less than 0.1 / mol L, an undeposited portion may occur.
  • the content exceeds 1.0 mol / L, the reducing agent has an excessive reducing action. Solution stability may be impaired.
  • sodium formate sodium formate, potassium formate, and ammonium formate can be used.
  • Sodium formate is preferred in terms of easy water solubility and ease of handling.
  • the electroless platinum plating solution uses a water-soluble platinum compound, a complexing agent is not necessarily required to dissolve the platinum compound in water. However, the electroless platinum plating solution can be further stabilized by adding a complexing agent.
  • the organic acid is preferably one or more compounds selected from aliphatic hydroxy acids having a molecular weight of 90 to 500, such as lactic acid, malic acid, citric acid, trisodium citrate, ammonium citrate, glycine, One or more compounds selected from the group consisting of gluconic acid, malonic acid, oxalic acid, succinic acid, acetic acid, maleic acid, and fumaric acid can be used.
  • the complexing agent also acts as a pH buffer material.
  • the electroless platinum plating solution preferably contains the organic acid in a range of 0.01 mol / L to 0.5 mol / L, and in a range of 0.02 mol / L to 0.3 mol / L. More preferably. If the content of the organic acid in the electroless platinum plating solution is less than 0.01 mol / L, it may not act as a complexing agent, and if it exceeds 0.5 mol / L, the plating itself can be performed satisfactorily. Decreases.
  • the electroless platinum plating solution may further include various components such as a surfactant, a stress relaxation agent, and a pH adjuster.
  • polyethylene glycol can be used, and various conventionally known surfactants can be used.
  • polyethylene glycol when polyethylene glycol is used as a surfactant, it improves the wettability of the surface of the plating substrate, and when bubbles are generated on the surface of the plating substrate, the bubbles can be easily separated from the surface of the plating substrate. it can.
  • stress relaxation agent saccharin, 1.4-butynediol, benzenesulfonic acid, naphthalenedisulfonic acid can be used, and various conventionally known stress relaxation agents can be used.
  • the electroless platinum plating solution is preferably adjusted to a pH range of 6.5 to 13.0 by adding a pH adjusting agent. If the pH in the electroless platinum plating solution is less than 6.5, the reducing action of the reducing agent may be reduced. Even if the pH of the electroless platinum plating solution exceeds 13.0, no particular problem occurs, but it is preferably 13.0 or less from the viewpoint of workability such as pH adjustment and bath management.
  • the electroless platinum plating solution can change the appearance of the obtained platinum electroless coating by adjusting the pH within the above range. For example, when the pH of the electroless platinum plating solution is 7, a gray platinum electroless coating can be obtained, and when the pH is 12, a white platinum electroless coating can be obtained.
  • a water-soluble platinum compound such as platinum (II) chloride, platinum (IV) chloride, hexahydroxoplatinum (IV), dichlorotetraammine platinum (II), etc. Therefore, even if it does not contain a complexing agent, this platinum compound forms a platinum complex and can be easily dissolved in water. Moreover, the platinum complex produced
  • formalin, glucose, formic acid, and formate as reducing agents all have a weaker reducing action than hydrazine monohydrate and sodium borohydride. For this reason, the electroless platinum plating solution is not decomposed by the reducing agent. Therefore, the electroless platinum plating solution can obtain excellent solution stability as compared with the conventional electroless platinum plating solution without using heavy metal ions or thiol compounds. Also, formalin, glucose, formic acid, and formate are all suitable in that the amount of hydrogen generation is small compared to hydrazine monohydrate and sodium borohydride as conventional reducing agents.
  • the electroless platinum plating solution does not include a compound capable of generating ammonia gas such as ethylenediamine, generation of ammonia gas can be prevented.
  • a platinum film (platinum electrolytic film) is formed on the surface of the nickel film by performing electrolytic plating on the plating substrate.
  • an electroless plating process is performed by immersing a plating base material having a platinum electrolytic film formed on the surface of the nickel film in the electroless platinum plating solution of the present embodiment.
  • the platinum complex in the electroless platinum plating solution is reduced and deposited on the surface of the platinum electrolytic film, whereby a platinum film (platinum electroless film) can be formed on the surface of the platinum electrolytic film.
  • the electroless plating treatment using the electroless platinum plating solution of the present embodiment has a deposition rate of 1 to 2 ⁇ m / hour, and a deposition rate comparable to that of the conventional electroless platinum plating solution containing dinitrodiamine platinum or dinitrotetraammine platinum. Can be obtained.
  • the operating temperature of the electroless platinum plating solution is preferably in the range of 40 to 90 ° C. If the temperature is lower than 40 ° C., the plating rate may be slow, and if it exceeds 90 ° C., the amount of water evaporation increases and the composition variation may increase.
  • the plating time with the electroless platinum plating solution depends on the thickness of the platinum electroless film to be formed.
  • an electroless platinum plating solution containing 1.05 mol / L of dichlorotetraammineplatinum (II) as a water-soluble platinum compound (1.0 g / L in terms of platinum) by setting the plating time to 30 minutes A platinum electroless film having a thickness of 0.5 ⁇ m can be formed.
  • the above reducing agent mainly generates carbon dioxide and water along with the reduction reaction. Since carbon dioxide and water do not accumulate in the electroless platinum plating solution, the electroless platinum plating solution is not altered and can be used for a long time.
  • the electroless platinum plating solution of this embodiment is suitable for plating of electronic parts made of metal, electrode materials, synthetic resins such as ABS resin, polyamide resin, polycarbonate resin, non-conductive ceramics such as alumina and zirconia. It is. In particular, it can be suitably used for applications of oxygen sensor electrodes made of ceramics such as zirconia, and various jewelry.
  • a nickel film having a thickness of 3 ⁇ m was formed on a copper plate by electrolytic plating.
  • a plating base material was prepared by forming a platinum film (platinum electrolytic film) having a thickness of 0.1 ⁇ m on the surface of the nickel film by electrolytic plating.
  • Electroless plating treatment The obtained electroless platinum plating solution is heated to a temperature of 70 ° C., and the plating base material on which the platinum electrolytic film is formed is immersed in the electroless platinum plating solution to perform the electroless plating treatment, thereby obtaining a platinum electrolytic film.
  • a platinum film platinum electroless film was formed on the surface.
  • the thickness of the platinum electroless coating was measured every 10 minutes until the immersion time reached 60 minutes. The results are shown in FIG. From FIG. 1, it was confirmed that the deposition rate in the electroless plating process was 1.0 ⁇ m / hour.
  • a platinum electroless coating having a thickness of 0.5 ⁇ m was formed by performing electroless plating treatment for 60 minutes. It was visually confirmed that the obtained platinum electroless coating was gray. Further, when the surface of the obtained platinum electroless coating was observed with a scanning electron microscope (SEM) at a magnification of 30,000 times, as shown in FIG. Met.
  • SEM scanning electron microscope
  • the temperature of the electroless platinum plating solution is changed to 50 ° C., 60 ° C., 70 ° C., and 80 ° C., and the plating base material on which the platinum electrolytic film is formed is immersed in the electroless platinum plating solution for 2 hours.
  • the electroless plating process was performed.
  • disassembly of the said electroless platinum plating solution was determined by observing whether the platinum deposit produced in the said electroless platinum plating solution.
  • Table 1 shows the results.
  • “X” means that the electroless platinum plating solution was decomposed within 1 hour
  • “ ⁇ ” means that it was decomposed within 2 hours
  • “ ⁇ ” indicates that it was completely decomposed after 2 hours. It means no.
  • the electroless platinum plating solution maintained at a temperature of 50 to 80 ° C. for 2 hours is naturally cooled, it is heated again to the same temperature the next day, and the plating substrate is immersed for 2 hours to be electroless. Plating treatment was performed. Even when the electroless platinum plating solution was heated to any temperature, the electroless plating treatment could be normally performed. From this, it is clear that the electroless platinum plating solution can be used continuously.
  • an electroless platinum plating solution was prepared in exactly the same manner as in Example 1 except that the pH (temperature 25 ° C.) was adjusted to 11.0.
  • the obtained electroless platinum plating solution is heated to a temperature of 70 ° C., and the plating base material on which the platinum electrolytic film is formed is immersed in the electroless platinum plating solution for 60 minutes to perform the electroless plating treatment.
  • a platinum electroless film having a thickness of 0.5 ⁇ m was formed on the surface of the electrolytic film. It was confirmed visually that the obtained platinum electroless coating had a white glossy appearance. Further, when the surface of the obtained platinum electroless coating was observed with an SEM at a magnification of 30,000, the surface shape of the platinum particles was small and smooth as shown in FIG.
  • the electroless platinum plating solution kept at a temperature of 50 to 80 ° C. for 2 hours was subjected to electroless plating treatment the same day as in Example 1 in the same manner. Even when the electroless platinum plating solution was heated to any temperature, the electroless plating treatment could be normally performed. From this, it is clear that the electroless platinum plating solution can be used continuously.
  • Example 1 an electroless platinum plating solution was prepared in exactly the same manner as in Example 2 except that hydrazine monohydrate 0.5 mol / L was used instead of sodium formate as the reducing agent. The pH (temperature 25 ° C.) was adjusted to 11.0. Next, the presence or absence of decomposition of the electroless platinum plating solution was determined using the obtained electroless platinum plating solution exactly as in Example 1. Table 1 shows the results.
  • Example 2 an electroless platinum plating solution was prepared in exactly the same manner as in Example 2 except that sodium borohydride 0.5 mol / L was used instead of sodium formate as the reducing agent. The pH (temperature 25 ° C.) was adjusted to 11.0. Next, the presence or absence of decomposition of the electroless platinum plating solution was determined using the obtained electroless platinum plating solution exactly as in Example 1. Table 1 shows the results.
  • Comparative Example 3 In this comparative example, it was completely the same as Comparative Example 1 except that 0.005 mol / L (1.0 g / L in terms of platinum) of dinitrodiammine platinum (II) was used as the platinum compound instead of dichlorotetraammine platinum (II).
  • An electroless platinum plating solution was prepared in the same manner, and then the pH (temperature 25 ° C.) was adjusted to 11.0. Next, the presence or absence of decomposition of the electroless platinum plating solution was determined using the obtained electroless platinum plating solution exactly as in Example 1. Table 1 shows the results.
  • Comparative Example 4 This comparative example is exactly the same as Comparative Example 2 except that 0.005 mol / L of dinitrodiammine platinum (II) (1.0 g / L in terms of platinum) was used as the platinum compound instead of dichlorotetraammine platinum (II).
  • An electroless platinum plating solution was prepared in the same manner, and then the pH (temperature 25 ° C.) was adjusted to 11.0. Next, the presence or absence of decomposition of the electroless platinum plating solution was determined using the obtained electroless platinum plating solution exactly as in Example 1. Table 1 shows the results.
  • the electroless platinum plating solutions of Examples 1 and 2 in which the platinum compound is dichlorotetraammineplatinum (II) and the reducing agent is sodium formate are both at a temperature of 50 to 80 ° C. It is clear that it does not decompose even after 2 hours in the range and has excellent solution stability.
  • the electroless platinum plating solutions of Comparative Examples 1 to 4 in which the reducing agent is hydrazine monohydrate or sodium borohydride are all decomposed within one hour at a temperature range of 70 to 80 ° C. It is apparent that the solution decomposes within 2 hours even in the temperature range of 50 to 60 ° C. and the solution stability is poor.
  • the electroless platinum plating solution of the present invention since the electroless platinum plating solution of the present invention has excellent solution stability, it can withstand long-term use. Further, since the electroless platinum plating solution does not contain a compound capable of generating ammonia gas such as ethylenediamine and ammonia, generation of ammonia gas can be prevented. For this reason, it is possible to prevent the work environment from being deteriorated due to the odor accompanying the generation of ammonia gas. In addition, the electroless platinum plating solution does not use a complexing agent that forms a strong complex with platinum ions such as ethylenediamine and ammonia, so use a reducing agent with a weak reducing action such as formalin, glucose, formic acid, and formate. can do. Moreover, these reducing agents can reduce the generation amount of hydrogen gas compared with hydrazine monohydrate and sodium borohydride.
  • the electroless platinum plating solution of the present embodiment is suitable for plating of electronic parts made of metal or the like, electrode materials, various synthetic resins, ceramics, and the like.
  • it can be suitably used for applications of oxygen sensor electrodes made of ceramics such as zirconia, and various jewelry.

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PCT/JP2016/056047 2015-10-15 2016-02-29 無電解白金めっき液 Ceased WO2017064874A1 (ja)

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EP16855128.1A EP3363928A4 (en) 2015-10-15 2016-02-29 AUTOCATALYTIC PLATE PLATING SOLUTION
US15/767,817 US20180305819A1 (en) 2015-10-15 2016-02-29 Electroless platinum plating solution

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JP2015203809A JP6352879B2 (ja) 2015-10-15 2015-10-15 無電解白金めっき液
JP2015-203809 2015-10-15

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JP6572376B1 (ja) 2018-11-30 2019-09-11 上村工業株式会社 無電解めっき浴
JP7506404B2 (ja) * 2019-10-29 2024-06-26 学校法人 工学院大学 金属膜の製造方法、金属膜形成用組成物及び金属膜積層体
KR102293808B1 (ko) * 2019-12-02 2021-08-24 (재)한국건설생활환경시험연구원 무전해 백금 도금액 조성물 및 이를 이용한 도금방법

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Publication number Priority date Publication date Assignee Title
WO2018211727A1 (ja) * 2017-05-18 2018-11-22 日本高純度化学株式会社 無電解白金めっき液及びそれを用いて得られた白金皮膜
JPWO2018211727A1 (ja) * 2017-05-18 2020-03-26 日本高純度化学株式会社 無電解白金めっき液及びそれを用いて得られた白金皮膜
US10941494B2 (en) 2017-05-18 2021-03-09 Japan Pure Chemical Co., Ltd. Electroless platinum plating solution and platinum film obtained using same
JP7118446B2 (ja) 2017-05-18 2022-08-16 日本高純度化学株式会社 無電解白金めっき液及びそれを用いて得られた白金皮膜

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EP3363928A1 (en) 2018-08-22
EP3363928A4 (en) 2019-06-19
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