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WO2011070933A1 - Solution de dorure dure électrolytique et procédé de placage qui utilise celle-ci - Google Patents

Solution de dorure dure électrolytique et procédé de placage qui utilise celle-ci Download PDF

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Publication number
WO2011070933A1
WO2011070933A1 PCT/JP2010/071304 JP2010071304W WO2011070933A1 WO 2011070933 A1 WO2011070933 A1 WO 2011070933A1 JP 2010071304 W JP2010071304 W JP 2010071304W WO 2011070933 A1 WO2011070933 A1 WO 2011070933A1
Authority
WO
WIPO (PCT)
Prior art keywords
gold
plating solution
salt
electrolytic hard
film
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/JP2010/071304
Other languages
English (en)
Japanese (ja)
Inventor
誠人 古川
仁俊 孫
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
NE Chemcat Corp
Original Assignee
NE Chemcat Corp
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by NE Chemcat Corp filed Critical NE Chemcat Corp
Priority to CN2010800528667A priority Critical patent/CN102695819A/zh
Priority to EP10835855.7A priority patent/EP2511400A4/fr
Priority to KR1020127012784A priority patent/KR20120120134A/ko
Priority to SG2012041463A priority patent/SG181529A1/en
Publication of WO2011070933A1 publication Critical patent/WO2011070933A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • 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
    • C25D3/56—Electroplating: Baths therefor from solutions of alloys
    • C25D3/62—Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of gold
    • 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
    • C25D3/56—Electroplating: Baths therefor from solutions of alloys

Definitions

  • the present invention relates to an electrolytic hard gold plating solution that is capable of forming a dense plating film that hardly generates pinholes even if the plating film is thin, and a plating method using the same.
  • the present invention relates to an electrolytic hard gold plating solution suitably used for partial plating of electronic parts such as connectors and a plating method using the same.
  • a hard gold plating having excellent wear resistance is applied to a contact member that is an electrical contact of a connector that electrically connects electronic devices and electronic components.
  • a contact member of an electronic component is manufactured by the following method. First, nickel plating is performed on the surface of a copper material or the like serving as a base material to form a nickel film. Next, hard gold plating is performed on the nickel film to form a gold film. Thereby, the contact member in which the nickel film and the gold film are sequentially formed on the copper material is obtained.
  • a gold film in which a large number of pinholes are formed cannot sufficiently protect the nickel film. Therefore, it is desirable that the gold film has no pinhole.
  • Patent Document 1 describes that a contact member is partially plated using a hard gold plating solution containing a brightener. This plating solution has high throwing power. However, in this plating solution, the brightener component is taken into the gold film. When additive components such as a brightener component are incorporated into the gold film, the gold purity of the gold film decreases. As a result, the contact resistance of the contact member is increased or the corrosion resistance is deteriorated.
  • the problem to be solved by the present invention is an electrolytic hard gold plating solution that is suitably used for partial plating treatment and the like, and does not cause pinholes in the gold film even when a gold film having a film thickness of 0.1 ⁇ m or less is formed. Is to provide.
  • Another problem to be solved by the present invention is to provide a plating method using this electrolytic hard gold plating solution.
  • the present inventors examined thinning of the gold film. As a result, it has been found that when the organic crystal modifier according to the present invention is blended in the plating solution, no pinhole is generated in the gold film even if the film thickness of the gold film is about 0.05 ⁇ m. Furthermore, the present inventors have found that the above plating solution forms a gold film with high gold purity. The present inventors have completed the present invention based on the above findings.
  • At least one of gold cyanide and gold cyanide salt A water-soluble cobalt salt or a water-soluble nickel salt; An organic acid conductive salt, An aromatic sulfonic acid compound; One or a combination of two or more selected from the group consisting of carboxylic acids, oxycarboxylic acids, and salts thereof; A five-membered heterocyclic compound containing nitrogen; and Electrolytic hard gold plating solution characterized by containing.
  • a plating method for forming a gold film at a desired plating location by spraying the electrolytic hard gold plating solution according to [1] onto the desired plating location.
  • the gold film formed using the electrolytic hard gold plating solution of the present invention does not form pinholes even when the film thickness is about 0.05 ⁇ m. Since the nickel film surface is completely covered and protected by the gold film, the corrosion resistance of the material to be plated is high. In addition, the amount of gold used can be reduced, and the economy is excellent.
  • gold cyanide and gold cyanide salt are blended as a gold source. Both may be blended.
  • gold cyanide salt include potassium gold cyanide, sodium gold cyanide, and ammonium gold cyanide. These may be blended alone or in combination of two or more.
  • the total concentration of gold cyanide and gold cyanide salt in the electrolytic hard gold plating solution of the present invention is 0.1 to 20 g / L in total, preferably 2 to 15 g / L, and preferably 3 to 10 g / L. Particularly preferred. If the gold concentration is less than 0.1 g / L, the cathode current efficiency is poor, and a gold film having a predetermined film thickness cannot be obtained. Even if the gold concentration exceeds 20 g / L, the cathode current efficiency does not increase in proportion to the gold concentration, so there is no particular advantage of increasing the gold concentration. Further, the plating solution is frequently taken out during the plating process, and the loss of the plating solution is increased.
  • An aromatic sulfonic acid compound is blended in the electrolytic hard gold plating solution of the present invention.
  • the aromatic sulfonic acid compound acts as an organic oxidizing agent.
  • the aromatic sulfonic acid compounds include 2-nitrobenzenesulfonic acid, 3-nitrobenzenesulfonic acid, 4-nitrobenzenesulfonic acid, 2,4-dinitrobenzenesulfonic acid, 2-aminobenzenesulfonic acid, 3-aminobenzenesulfonic acid, 4 -Aminobenzenesulfonic acid, and salts thereof.
  • an aromatic sulfonic acid compound having a nitro group as a substituent is preferable. These may be blended alone or in combination of two or more.
  • the electrolytic hard gold plating solution containing these aromatic sulfonic acid compounds specifically raises the redox potential of gold in a low current density region (less than 20 A / dm 2 current density). As a result, gold deposition is suppressed in the low current density region.
  • an electrolytic hard gold plating solution in which these aromatic sulfonic acid compounds are blended does not suppress gold deposition in a medium to high current density region (current density 20 to 200 A / dm 2 ). As a result, a normal gold film is formed in the medium to high current density region.
  • the electrolytic hard gold plating solution of the present invention can suppress the formation of a plating film other than the desired plating position of the material to be plated by controlling the current density.
  • the concentration of the organic oxidizing agent blended in the electrolytic hard gold plating solution of the present invention is 0.1 to 20 g / L, preferably 0.5 to 5 g / L, and particularly preferably 1 to 3 g / L.
  • concentration of the organic oxidizer is less than 0.1 g / L, the effect of suppressing gold precipitation in the low current density region is small. Even if the concentration of the organic oxidant exceeds 20 g / L, the effect of suppressing gold precipitation in the low current density region remains unchanged and is high.
  • carboxylic acid or oxycarboxylic acid or a salt thereof is blended. These act as complexing agents.
  • Carboxylic acid or oxycarboxylic acid, and salts thereof include formic acid, glycolic acid, lactic acid, oxybenzoic acid, oxalic acid, malonic acid, succinic acid, malic acid, tartaric acid, phthalic acid, diglycolic acid, citric acid, and these
  • the salt of is illustrated.
  • alkali metal salts such as sodium salt and potassium salt, alkaline earth metal salts such as calcium salt, and salts such as ammonia and amine are preferable. These may be blended alone or in combination of two or more.
  • the concentration of the complexing agent in the electrolytic hard gold plating solution of the present invention is 1 to 100 g / L, preferably 5 to 600 g / L.
  • concentration of the complexing agent is less than 1 g / L, inorganic impurities that dissolve from the material to be plated are easily taken into the gold film.
  • inorganic impurities are taken into the gold film, the gold purity of the gold film decreases. As a result, the appearance of the gold film is deteriorated, the contact resistance of the contact member is increased, or the corrosion resistance is deteriorated. Even if the concentration of the complexing agent exceeds 100 g / L, an effect commensurate with it cannot be obtained, so that it is not economical.
  • the electrolytic hard gold plating solution of the present invention is mixed with a water-soluble cobalt salt or a water-soluble nickel salt.
  • cobalt salt include cobalt sulfate, cobalt nitrate, cobalt chloride, and basic cobalt carbonate.
  • nickel salt include nickel sulfate, nickel sulfamate, nickel sulfite, and nickel chloride. These may be blended alone or in combination of two or more.
  • the concentration of the cobalt salt or nickel salt in the electrolytic hard gold plating solution of the present invention is 0.01 to 10 g / L, preferably 0.1 to 1.0 g / L.
  • concentration of the cobalt salt or nickel salt is less than 0.01 g / L, the hardness of the gold film is lowered. Even if the concentration of the cobalt salt or nickel salt exceeds 10 g / L, an effect commensurate with it cannot be obtained, and therefore it is not economical.
  • the water solubility of the cobalt salt or the nickel salt blended in the electrolytic hard gold plating solution of the present invention means water solubility to the extent that it can be dissolved in water at the above concentration.
  • organic acid conductive salt is added to the electrolytic hard gold plating solution of the present invention.
  • organic acid conductive salt include potassium formate, potassium citrate, potassium phosphate, potassium nitrate, and potassium succinate. These may be blended alone or in combination of two or more.
  • the concentration of the organic acid conductive salt in the electrolytic hard gold plating solution of the present invention is 10 to 200 g / L, preferably 50 to 100 g / L.
  • concentration of the organic acid conductive salt is less than 10 g / L, the appearance of the gold film is deteriorated and a normal gold film cannot be obtained. Even if the concentration of the organic acid conductive salt exceeds 200 g / L, an effect commensurate with it cannot be obtained, and this is not economical.
  • a five-membered heterocyclic compound containing nitrogen is blended in the electrolytic hard gold plating solution of the present invention.
  • the five-membered heterocyclic compound containing nitrogen acts as an organic crystal modifier.
  • a five-membered heterocyclic compound containing nitrogen is adsorbed on gold cyanide ions in the plating bath, or adsorbed or complexed with gold ions after deligandation (cyanide ions) in an electric double layer.
  • the inventor believes that a dense gold film is formed by controlling the crystal growth. Further, the five-membered heterocyclic compound containing nitrogen used in the present invention is not taken into the gold film. Therefore, the gold purity of the gold film is high.
  • Nitrogen-containing 5-membered heterocyclic compounds include imidazole, 2-methylimidazole, pyrazole, 3,5-dimethylpyrazole, 2-imidazoline, 2-pyrrolidone, hydantoin, 5,5-dimethylhydantoin, allantoline, succinimide DL-pyroglutamic acid, and salts thereof.
  • the concentration of the 5-membered heterocyclic compound containing nitrogen is 1 to 50 g / L, preferably 5 to 20 g / L, and particularly preferably 8 to 12 g / L.
  • the concentration of the 5-membered heterocyclic compound containing nitrogen is less than 1 g / L, the crystal adjustment effect is reduced, and a dense gold film cannot be obtained. Even if the concentration of the five-membered heterocyclic compound containing nitrogen exceeds 50 g / L, an effect commensurate with it cannot be obtained, so that it is not economical.
  • the electrolytic hard gold plating solution of the present invention can be used at pH 3.0 to 7.0, but is preferably used at pH 4.0 to 5.0.
  • pH When the pH is lower than 4.0, the cathode current efficiency is lowered and it becomes difficult to obtain a gold film having a predetermined film thickness.
  • the pH adjuster include sodium hydroxide, potassium hydroxide, ammonium hydroxide and dilute sulfuric acid.
  • the electrolytic hard gold plating solution of the present invention can be blended with other substances as long as the effects of the present invention are not hindered.
  • the plating method using the electrolytic hard gold plating solution of the present invention can be performed by a conventionally known plating method.
  • plating can be performed by a partial plating method in which the electrolytic hard gold plating solution of the present invention is sprayed from a platinum nozzle to a material to be plated using the platinum nozzle as an anode and the material to be plated as a cathode.
  • the equipment configuration and evaluation method used for the test are as follows.
  • a copper plate of 32 mm ⁇ 150 mm ⁇ 0.2 mm was prepared.
  • a nickel film having a thickness of 2 ⁇ m was formed on the copper plate using a nickel sulfamate plating solution, and this was used as a sample.
  • a mask plate made of silicone rubber having a 10 mm ⁇ 10 mm square opening was stacked on the sample and fixed.
  • the plating solution was sent to the plating solution injection port using a pump, and the plating solution was injected from the plating solution injection port to the opening of the mask plate. Thereby, partial plating was performed on the sample.
  • a platinum nozzle having a diameter of 5 mm was attached to the plating solution injection port, and this nozzle was used as an anode electrode.
  • the film thickness of the gold film was measured using a fluorescent X-ray film thickness measuring instrument SEA5120 manufactured by SII.
  • the presence or absence of pinholes generated in the gold film was evaluated by the nitrate aeration test method (JIS H8620 10.5), which is one of the porosity tests listed in the JIS standard.
  • the porosity test is a test for evaluating the size and number of pinholes in the plating layer.
  • nitric acid aeration test a sample is placed on a porcelain plate in a desiccator in which nitric acid is placed at the bottom of the container and left at about 23 ° C. for 1 hour.
  • Nitric acid vapor generated in the desiccator corrodes the nickel film through the pinhole.
  • spots appear on the gold film.
  • the occurrence state of the spots was evaluated by collating with a rating number standard chart defined in a JIS standard plating corrosion resistance test method (JIS H8502 11.5).
  • the plating solution was adjusted by the above composition.
  • the plating solution was adjusted to pH 4.2, and the sample was subjected to partial plating so that the solution temperature was 55 ° C., the current density was 40 A / dm 2 , and the gold film thickness was 0.05 ⁇ m.
  • the gold film formed on the sample had a lemon-yellow color tone and had a uniform appearance with no uneven appearance.
  • the rating number was 9.5-5, and the total corrosion area ratio exceeded 0.02 and was 0.05% or less.
  • Example 2 (Examples 2 to 5), (Comparative Examples 1 and 2) A plating solution was prepared according to the formulation shown in Table 1, and the sample was partially plated in the same manner as in Example 1. The gold film formed on the sample had a lemon-yellow color tone and had a uniform appearance with no uneven appearance. The results of the corrosion resistance evaluation are shown in Table 2.
  • the electrolytic hard gold plating solution of the present invention can form a dense gold film with very few pinholes even when the film thickness of the gold film is 0.1 ⁇ m or less. As a result, the corrosion resistance of the material to be plated is excellent.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electroplating And Plating Baths Therefor (AREA)

Abstract

L'invention divulgue une solution de placage qui ne forme pas de piqûres dans un film de métal même si l'épaisseur du film de métal est inférieure à 0,1 μm. Un placage partiel est réalisé en utilisant une solution de dorure dure électrolytique qui contient du cyanure d'or et/ou un sel de cyanure d'or, un sel de cobalt soluble dans l'eau ou un sel de nickel soluble dans l'eau, des sels conducteurs d'acides organiques, un composé d'acide sulfonique aromatique, une combinaison d'un ou de plusieurs élément(s) sélectionné(s) dans un groupe comprenant des acides carboxyliques, des acides oxycarboxyliques, ainsi que les sels de ceux-ci, et un composé hétérocyclique pentagonal contenant de l'azote. Par conséquent, aucune piqûre n'est formée dans un film de métal même si l'épaisseur du film de métal est inférieure à 0,1 μm.
PCT/JP2010/071304 2009-12-09 2010-11-30 Solution de dorure dure électrolytique et procédé de placage qui utilise celle-ci Ceased WO2011070933A1 (fr)

Priority Applications (4)

Application Number Priority Date Filing Date Title
CN2010800528667A CN102695819A (zh) 2009-12-09 2010-11-30 电解硬质金镀敷液及使用该镀敷液的镀敷方法
EP10835855.7A EP2511400A4 (fr) 2009-12-09 2010-11-30 Solution de dorure dure électrolytique et procédé de placage qui utilise celle-ci
KR1020127012784A KR20120120134A (ko) 2009-12-09 2010-11-30 전해 경질 금 도금액 및 이것을 사용하는 도금 방법
SG2012041463A SG181529A1 (en) 2009-12-09 2010-11-30 Electrolytic hard gold plating solution and plating method using same

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2009-279409 2009-12-09
JP2009279409A JP2011122192A (ja) 2009-12-09 2009-12-09 電解硬質金めっき液及びこれを用いるめっき方法

Publications (1)

Publication Number Publication Date
WO2011070933A1 true WO2011070933A1 (fr) 2011-06-16

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PCT/JP2010/071304 Ceased WO2011070933A1 (fr) 2009-12-09 2010-11-30 Solution de dorure dure électrolytique et procédé de placage qui utilise celle-ci

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EP (1) EP2511400A4 (fr)
JP (1) JP2011122192A (fr)
KR (1) KR20120120134A (fr)
CN (1) CN102695819A (fr)
SG (1) SG181529A1 (fr)
TW (1) TW201137184A (fr)
WO (1) WO2011070933A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111647918A (zh) * 2019-03-04 2020-09-11 日本电镀工程股份有限公司 电解镀金液及其制造方法、以及镀金方法及金配合物

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JP5025815B1 (ja) * 2011-08-10 2012-09-12 小島化学薬品株式会社 硬質金めっき液
JP5758361B2 (ja) * 2012-08-31 2015-08-05 日本エレクトロプレイテイング・エンジニヤース株式会社 ノンシアン系金‐パラジウム合金めっき液及びめっき方法
JP5152943B1 (ja) * 2012-09-19 2013-02-27 小島化学薬品株式会社 低遊離シアン金塩の製造方法
CN118352327B (zh) * 2024-01-10 2025-07-18 深圳市联合蓝海应用材料科技股份有限公司 替代纯金凸块封装倒装芯片的金银合金凸块及其制备方法

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JP2009007656A (ja) * 2007-06-29 2009-01-15 Japan Pure Chemical Co Ltd 電解金めっき液及びそれを用いて得られた金皮膜
JP2009165730A (ja) 2008-01-18 2009-07-30 Kozo Motoki 洗浄用ブラシ

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JP2003502513A (ja) * 1999-06-17 2003-01-21 デグサ ガルヴァノテヒニク ゲゼルシャフト ミット ベシュレンクテル ハフツング 光沢のある金層および金合金層を電着するための酸性浴および電着用光沢剤
JP3933930B2 (ja) 1999-06-17 2007-06-20 デグサ ガルヴァノテヒニク ゲゼルシャフト ミット ベシュレンクテル ハフツング 光沢のある金層および金合金層を電着するための酸性浴および電着用光沢剤
JP2009007656A (ja) * 2007-06-29 2009-01-15 Japan Pure Chemical Co Ltd 電解金めっき液及びそれを用いて得られた金皮膜
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Publication number Priority date Publication date Assignee Title
CN111647918A (zh) * 2019-03-04 2020-09-11 日本电镀工程股份有限公司 电解镀金液及其制造方法、以及镀金方法及金配合物

Also Published As

Publication number Publication date
TW201137184A (en) 2011-11-01
CN102695819A (zh) 2012-09-26
EP2511400A4 (fr) 2013-07-24
JP2011122192A (ja) 2011-06-23
EP2511400A1 (fr) 2012-10-17
KR20120120134A (ko) 2012-11-01
SG181529A1 (en) 2012-07-30

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