WO2022070983A1 - バレルめっき用スズめっき液 - Google Patents

バレルめっき用スズめっき液 Download PDF

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Publication number
WO2022070983A1
WO2022070983A1 PCT/JP2021/034277 JP2021034277W WO2022070983A1 WO 2022070983 A1 WO2022070983 A1 WO 2022070983A1 JP 2021034277 W JP2021034277 W JP 2021034277W WO 2022070983 A1 WO2022070983 A1 WO 2022070983A1
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Prior art keywords
tin
plating solution
plating
barrel
tin plating
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Application number
PCT/JP2021/034277
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English (en)
French (fr)
Japanese (ja)
Inventor
英之 三瓶
和洋 宮本
昂平 神庭
Original Assignee
メルテックス株式会社
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Application filed by メルテックス株式会社 filed Critical メルテックス株式会社
Priority to CN202180006228.XA priority Critical patent/CN114651090A/zh
Priority to KR1020227035069A priority patent/KR20220151680A/ko
Publication of WO2022070983A1 publication Critical patent/WO2022070983A1/ja

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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/30—Electroplating: Baths therefor from solutions of tin
    • C25D3/32—Electroplating: Baths therefor from solutions of tin characterised by the organic bath constituents used
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
    • A01N47/40—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having a double or triple bond to nitrogen, e.g. cyanates, cyanamides
    • A01N47/42—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having a double or triple bond to nitrogen, e.g. cyanates, cyanamides containing —N=CX2 groups, e.g. isothiourea
    • A01N47/44—Guanidine; Derivatives thereof
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D17/00—Constructional parts, or assemblies thereof, of cells for electrolytic coating
    • C25D17/16—Apparatus for electrolytic coating of small objects in bulk

Definitions

  • the present invention relates to a tin plating solution used for barrel plating, and more particularly to a tin plating solution that suppresses the generation of mold seen when a conventional tin plating solution is used.
  • tin plating solutions have been widely used as plating solutions for terminal plating and oxidative corrosion prevention plating in the field of electronic component materials.
  • tin plating has been used as an alternative to solder plating.
  • tin plating solutions are used, in the field of multilayer ceramic capacitors, which are chip components, it is common to form a tin plating layer on the surface of the external electrode of the multilayer ceramic capacitor.
  • the tin-plated layer of the external electrode of the monolithic ceramic capacitor has excellent solder wettability, and functions as a useful one when surface-mounting on a printed wiring board through a surface-mounting process such as solder reflow.
  • a general tin plating solution used for barrel plating contains additives such as various inorganic acids, organic acids, and pH adjusters, in addition to tin salts, which are sources of tin ions.
  • Patent Document 1 discloses a tin plating solution having a long solution life after bathing, excellent long-term storage stability, and can be used at a bath temperature exceeding 30 ° C.
  • Japanese Patent Publication Japanese Patent Laid-Open No. 2006-328528
  • the tin plating solution disclosed in Patent Document 1 may be adjusted to a pH value from weakly acidic to close to neutral, and the plating bath and subsequent washing may be performed in a bath temperature environment exceeding 30 ° C. At this time, since the pH of the plating solution is close to neutral, the bath temperature environment exceeds 30 ° C., and the plating solution contains an organic acid such as citric acid which is a nutrient for mold, it is used in the washing step after the plating step. In some cases, mold was generated in the washing water, and the generated mold adhered to the product to be plated, causing a problem of deteriorating the plating quality.
  • the present invention has been made in view of such circumstances, and in the water washing step after the tin plating step, it is possible to suppress the generation of mold in the washing water even in a bath temperature environment exceeding 30 ° C. It is an object of the present invention to provide a tin plating solution for barrel plating.
  • the tin plating solution for barrel plating is a tin plating solution used for barrel plating, and is a polyalkylene biguanide compound shown in Chemical formula 1 below and a salt thereof as an antifungal agent. It is characterized by containing one kind or two or more kinds selected from the group consisting of. [In the formula, R 1 is an alkylene group having 2 to 8 carbon atoms, and n is an integer of 2 to 18. ]
  • the tin plating solution for barrel plating according to the present invention contains one or more selected from the group consisting of polyalkylene biguanide compounds and salts thereof in the tin plating solution, so that the pH of the tin plating solution can be adjusted. Even in a bath temperature environment of weakly acidic to near neutral and exceeding 30 ° C., it is possible to suppress the generation of mold in the washing water in the water washing step after the tin plating step.
  • the antifungal agent used in addition to the tin plating solution for barrel plating according to the present invention is one selected from the group consisting of the polyalkylene biguanide compound shown in Chemical formula 1 below and salts thereof. Or two or more.
  • the addition of substances other than those required for tin plating to the tin plating solution usually adversely affects the quality of the tin plating film.
  • the quality of the formed tin plating film is not adversely affected.
  • R 1 is an alkylene group having 2 to 8 carbon atoms
  • n is an integer of 2 to 18.
  • Biguanide compounds such as polyalkylene biguanide compounds and their salts have the property of cations and exert a bactericidal effect by adsorbing to the surface of bacteria having a negative charge. Due to its effect, it is used for sterilization and sterilization of food manufacturing machines and instruments, medical devices and instruments, and since it has little effect on the human body and is highly safe, it can also be used as a cleaning solution for contact lenses and sterilization sprays. It is known to be used.
  • one or more of the antifungal agents according to the present invention selected from the group consisting of polyalkylene biguanide compounds and salts thereof are added to the tin plating solution used in barrel plating. ..
  • the pH of the tin plating solution is weakly acidic to close to neutral, and even in a bath temperature environment exceeding 30 ° C., it is possible to suppress the generation of mold in the water washing step after the tin plating step. be. Further, it does not adversely affect the quality of the formed tin plating film.
  • the one or more selected from the group consisting of polyalkylene biguanide compounds and salts thereof may be one or more selected from the group consisting of polyhexamethylene biguanide and salts thereof. preferable. This is because the generation of mold in the water-washing water can be further suppressed in the water-washing step after the tin-plating step without adversely affecting the quality of the formed tin-plated film.
  • the tin plating liquid for barrel plating according to the present invention contains tin salt as a tin ion supply source, a metal complexing agent, a conductive salt, an auxiliary conductive salt, a pH adjuster, and the like.
  • the tin plating solution containing the antioxidant contains one or more selected from the group consisting of the polyalkylene biguanide compound and salts thereof, which are the above-mentioned antifungal agents. And one or more selected from the group consisting of this polyalkylene biguanide compound and salts thereof shall be one or more selected from the group consisting of polyhexamethylene biguanide and salts thereof. Is preferable.
  • the pH of the tin plating solution is weakly acidic to close to neutral, and tin plating is performed even in a bath temperature environment exceeding 30 ° C. In the washing step after the step, the generation of mold in the washing water can be suppressed.
  • Tin salt that is the source of tin ions in the tin plating solution for barrel plating according to the present invention is a first tin salt that is soluble in water (hereinafter, simply referred to as "tin salt").
  • tin salt it is preferable to use one or more selected from tin methanesulfonate, tin sulfate, tin ethanesulfonate, and tin isethionic acid.
  • the content of the tin salt in the tin plating solution for barrel plating according to the present invention is preferably 4.5 g / L to 30 g / L in terms of tin.
  • the tin salt content is less than 4.5 g / L in terms of tin, the current efficiency is lowered and the plating speed does not satisfy the industrially required productivity, and at the same time, the smoothness and film thickness of the tin plating layer are uniform. Sex is impaired.
  • the tin salt content exceeds 30 g / L in terms of tin, the tin content in the plating solution becomes large, the tin electrodeposition rate is too fast, and it becomes difficult to control the film thickness of the plating layer. , Tin oxide precipitate formation cannot be avoided.
  • the content of the tin salt in the tin plating solution for barrel plating according to the present invention is more preferably 10 g / L to 20 g / L in terms of tin. From an industrially productive point of view, there are usually fluctuations in the plating conditions when tin plating is performed at a certain level, and considering the inevitable fluctuations in the plating conditions that cannot be controlled, tin of more stable quality is used. This is because a plating layer can be formed.
  • the metal complexing agent of the tin plating solution for barrel plating according to the present invention stabilizes tin ions supplied from tin salts in the tin plating solution as a chelate complex.
  • the metal complexing agent is preferably one or more selected from sodium gluconate, gluconic acid or a salt thereof, citric acid or a salt thereof, pyrophosphate or a salt thereof. This is because the metal complexing agent described here efficiently forms a chelate complex with tin ions ionized in a solution from a tin salt which is a tin ion supply source.
  • the content of the metal complexing agent in the tin plating solution for barrel plating according to the present invention is preferably 50 g / L to 300 g / L.
  • the content of the metal complexing agent is less than 50 g / L, it becomes difficult to form a chelate complex with all the tin ions in the plating solution on the premise of the content of the tin salt in the above-mentioned plating solution, and the metal complexing agent is liberated. Due to the presence of tin ions, the formation of tin oxide precipitates cannot be prevented.
  • the conductive salt of the tin plating solution for barrel plating according to the present invention stabilizes the energized state when electrolyzing the tin plating solution, increases the current efficiency of tin precipitation, and enhances productivity.
  • the conductive salt is preferably one or more selected from ammonium sulfate, sodium sulfate, and potassium sulfate. This is because the quality change of the tin plating solution is the smallest and no impurities remain in the tin plating layer.
  • the content of the conductive salt in the tin plating solution for barrel plating according to the present invention is preferably 1 g / L to 200 g / L.
  • the content of the conductive salt is less than 1 g / L, the effect of improving the energization stability when electrolysis is performed cannot be obtained. Even if the content of the conductive salt exceeds 200 g / L, the energization stability at the time of electrolysis is not improved any more, which is a waste of resources.
  • the auxiliary conductive salt according to the present invention is used in combination with the above-mentioned conductive salt in order to stabilize the energized state when electrolyzing the tin plating solution.
  • the auxiliary conductive salt is preferably one or more selected from methanesulfonic acid, ethanesulfonic acid, sulfuric acid, and isethionic acid. This is because when used in combination with the conductive salt, it does not affect the properties of the plating solution during tin plating and stabilizes the energized state when the tin plating solution is electrolyzed.
  • the content of the auxiliary conductive salt according to the present invention is preferably 1.5 g / L to 300 g / L.
  • the content of the auxiliary conductive salt is less than 1.5 g / L, the effect of improving the energization stability when electrolysis is performed cannot be obtained. Even if the content of the auxiliary conductive salt exceeds 300 g / L, the energization stability at the time of electrolysis is not improved any more, which is a waste of resources.
  • pH adjuster for the tin plating solution for barrel plating according to the present invention is suitable for forming a tin chelate complex by reacting tin ions supplied from a tin salt with a metal complexing agent in the tin plating solution. It is used for stabilizing the tin chelate complex once formed, and finally for adjusting the pH of the tin plating solution according to the present invention to be suitable for tin plating.
  • the pH adjuster is preferably one or more selected from sodium hydroxide, potassium hydroxide, and aqueous ammonia. These are selected as pH adjusters because they do not affect the properties of the plating solution when tin plating is performed and a good tin plating layer can be formed.
  • the pH value of the tin plating solution for barrel plating according to the present invention adjusted using the above-mentioned pH adjuster is preferably 3.5 to 8.0.
  • the pH value of the tin plating solution is in the strongly acidic region of less than 3.5, there is a high possibility that the unplated portion on the surface of the tin-plated product will be eroded.
  • the pH value of the tin plating solution exceeds 8.0, the stability of the produced tin chelate complex is impaired, tin cannot be immobilized and tin ions are formed, and tin oxide precipitates are formed, so that the tin plating solution can be used as a tin plating solution. This is because the life of the solution is shortened.
  • antioxidant of the tin plating solution for barrel plating according to the present invention it is preferable to use one or more selected from ascorbic acid, catechol, hydroquinone and ascorbic acid salt. This is to prevent natural oxidation due to contact between the atmosphere and the plating solution and efficiently prevent the generation of precipitation of tin oxide.
  • the content of the antioxidant in the tin plating solution for barrel plating according to the present invention is preferably 0.1 g / L to 30 g / L. If the content of the antioxidant is less than 0.1 g / L, a sufficient antioxidant effect cannot be obtained. Even if the content of the antioxidant exceeds 30 g / L, the antioxidant effect cannot be obtained any more, and the life of the tin plating solution cannot be expected to be extended. Moreover, adding an excessive amount of the antioxidant causes a change in the quality of the tin plating solution, which is not preferable. Therefore, more preferably, the concentration of the antioxidant is used in the range of 1 g / L to 10 g / L. This is because it is possible to obtain a reliable antioxidant effect, and it is possible to reliably prevent quality changes as a tin plating solution due to excessive addition of an antioxidant.
  • Antifungal agent The antifungal agent according to the present invention is preferably used by adding it to the above-mentioned tin plating solution for barrel plating.
  • the content of the antifungal agent in the tin plating solution for barrel plating according to the present invention is preferably 0.1 to 30 g / L.
  • the content of the antifungal agent is less than 0.1 g / L, the effect of preventing the generation of mold is not sufficiently exhibited, which is not preferable.
  • the content of the antifungal agent exceeds 30 g / L, the effect of preventing the generation of mold remains unchanged, and the cost of the antifungal agent to be added increases, which is not preferable.
  • the upper limit of the content of the antifungal agent is more preferably 20 g / L. This is because the cost of the antifungal agent to be added can be suppressed.
  • the upper limit of the content of the antifungal agent is more preferably 10 g / L. This is because the cost of the antifungal agent to be added can be further suppressed.
  • the barrel containing the product to be plated is immersed in the tin plating solution and electrolyzed under the condition of a bath temperature of 10 ° C to 50 ° C. It is preferable to do so.
  • the characteristic of this plating method is that the plating operation can be performed in a bath temperature range of 10 ° C to 50 ° C. When the bath temperature is less than 10 ° C., coarse tin-plated crystals are precipitated, and it becomes difficult to obtain a smooth tin-plated layer having excellent film thickness uniformity.
  • the current density during tin plating using the tin plating solution for barrel plating according to the present invention is preferably in the range of 0.05 A / dm 2 to 0.5 A / dm 2 .
  • the current density is less than 0.05 A / dm 2 , the precipitation rate of tin is naturally slow and the industrial productivity is not satisfied.
  • a current density exceeding 0.5 A / dm 2 is adopted, the smoothness of the tin plating film is impaired.
  • the tin plating solution for barrel plating according to the present invention described above is used for barrel plating capable of plating a large amount at one time, and is used for chip-type laminated ceramic capacitors and chip-type ceramics. It is suitable for forming a tin-plated layer of small parts that are substituted for coils, chip-type ceramic thermistors, inductors, varistors, resistors, and the like.
  • the tin salt, the metal complexing agent, the conductive salt, the auxiliary conductive salt, and the antioxidant were adjusted so that the component concentrations were in the range shown in the embodiment for carrying out the invention.
  • Meltex Inc.'s tin plating solution Melplate SN-2680 was used. Then, 2 g / L of polyhexamethylene biguanide was added to the tin plating solution as an antifungal agent to prepare a tin plating solution for barrel plating.
  • the pH of the tin plating solution was adjusted to 5.0 using sodium hydroxide as a pH adjuster.
  • Comparative Example 1 In Comparative Example 1, a tin plating solution for barrel plating was prepared in the same manner as in Examples except that 2 g / L of benzalkonium chloride was used as an antifungal agent.
  • Comparative Example 2 a tin plating solution for barrel plating was prepared in the same manner as in Example except that 2 g / L of sodium hypochlorite was used as an antifungal agent.
  • Comparative Example 3 In Comparative Example 3, a tin plating solution for barrel plating was prepared in the same manner as in Examples except that 2 g / L of didecyldimethylammonium chloride was used as an antifungal agent.
  • Comparative Example 4 a tin plating solution for barrel plating was prepared in the same manner as in Examples except that 2 g / L of thymol was used as an antifungal agent.
  • FIG. 1 shows the results of putting the tin plating solutions of Examples and Comparative Examples 1 to 4 in a beaker and confirming the presence or absence of turbidity and precipitation in the bath appearance of the tin plating solution. From the results of the bath appearance shown in FIG. 1, it was found that when didecyldimethylammonium chloride of Comparative Example 3 was used as the antifungal agent, the plating solution became turbid. Then, it was found that when thymol of Comparative Example 4 was used as the antifungal agent, precipitation occurred in the plating solution.
  • Figure 4 shows the measurement results of zero cross time.
  • the acceptance criteria here was that the zero cross time was 3 seconds or less.
  • the tip value of the bar graph is the average value of the zero cross times of 5 measurements. Then, the lowest point of the error bar displayed together with the bar graph shows the minimum value in the five measured values of the zero cross time, and the uppermost point of the error bar shows the maximum value in the five measured values of the zero cross time.
  • the average value of the zero cross time of both the MLCC and the resistor was 1.6 seconds. It was less than 3 seconds, which is the passing standard. Then, from the width displayed by the error bar, it became clear that the variation width of the zero cross time was about 0.5 seconds.
  • the aggregation rate was calculated according to the formula shown in Equation 1 below.
  • the evaluation result of the aggregation rate is shown in FIG.
  • the acceptance criteria here was that the agglomeration rate was 0.5% or less.
  • the agglomeration rate of barrel plating using the tin plating solution of the example to which polyhexamethylene biguanide was added as an antifungal agent was 0.1%, which satisfied the acceptance criteria.
  • Table 1 summarizes the evaluation items implemented so far and their results. As is clear from Table 1, it was the tin plating solution of the example using polyhexamethylene biguanide as the added mold inhibitor that prevented the generation of mold and all the evaluation results were good. On the other hand, it was clarified that the tin plating solution of the comparative example had a problem in any one or more of the evaluation items and could not be used as the tin plating solution.
  • the tin plating solution for barrel plating according to the present invention contains one or more selected from the group consisting of polyalkylene biguanide compounds and salts thereof as an antifungal agent in the tin plating solution.
  • the pH of the tin plating solution is weakly acidic to close to neutral, and even in a bath temperature environment exceeding 30 ° C., the quality of the tin plating film formed by using the tin plating solution is adversely affected. It became clear that there was no such thing. In addition, it was confirmed that in the water washing process after the tin plating process using the tin plating solution, the generation of mold in the water washing water was suppressed.
  • the tin plating solution for barrel plating according to the present invention contains the antifungal agent according to the present invention in the tin plating solution, so that the pH of the tin plating solution is weakly acidic to near neutral and the bath temperature exceeds 30 ° C. Even so, in the water washing step after the tin plating step, the generation of mold in the water washing water is suppressed, and the quality of the tin plating film formed by using the tin plating solution is not adversely affected. Therefore, in the water washing process after the barrel plating process, it is not necessary to deliver an antifungal agent to the water washing water in order to prevent the generation of mold.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Agronomy & Crop Science (AREA)
  • Pest Control & Pesticides (AREA)
  • Plant Pathology (AREA)
  • Health & Medical Sciences (AREA)
  • Dentistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Wood Science & Technology (AREA)
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  • Electroplating And Plating Baths Therefor (AREA)
PCT/JP2021/034277 2020-10-02 2021-09-17 バレルめっき用スズめっき液 WO2022070983A1 (ja)

Priority Applications (2)

Application Number Priority Date Filing Date Title
CN202180006228.XA CN114651090A (zh) 2020-10-02 2021-09-17 滚镀用镀锡液
KR1020227035069A KR20220151680A (ko) 2020-10-02 2021-09-17 배럴 도금용 주석 도금액

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JP2020167498A JP2022059731A (ja) 2020-10-02 2020-10-02 バレルめっき用スズめっき液
JP2020-167498 2020-10-02

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KR (1) KR20220151680A (zh)
CN (1) CN114651090A (zh)
TW (1) TWI781771B (zh)
WO (1) WO2022070983A1 (zh)

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CN108754553A (zh) * 2018-06-26 2018-11-06 厦门大学 基于杂环类生物碱配位的三价金无氰镀金电镀液及其应用

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JP2000319796A (ja) * 1999-05-06 2000-11-21 Nippon Paint Co Ltd 流動電解装置を備えたカチオン電着塗装装置およびカチオン電着塗装方法
JP2003293186A (ja) * 2002-04-09 2003-10-15 Ishihara Chem Co Ltd 中性スズメッキ浴、当該浴を用いたバレルメッキ方法
JP2009533548A (ja) * 2006-04-06 2009-09-17 テクノロジーズ モレキュレール （テクモ） 表面上の銅電着用界面活性条件抑制剤
JP2014505167A (ja) * 2010-12-21 2014-02-27 ビーエーエスエフ ソシエタス・ヨーロピア レベリング剤を含有する金属電解めっき組成物
CN108754553A (zh) * 2018-06-26 2018-11-06 厦门大学 基于杂环类生物碱配位的三价金无氰镀金电镀液及其应用

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KR20220151680A (ko) 2022-11-15

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