JPH09256186A - Silver plating method - Google Patents
Silver plating methodInfo
- Publication number
- JPH09256186A JPH09256186A JP6431496A JP6431496A JPH09256186A JP H09256186 A JPH09256186 A JP H09256186A JP 6431496 A JP6431496 A JP 6431496A JP 6431496 A JP6431496 A JP 6431496A JP H09256186 A JPH09256186 A JP H09256186A
- Authority
- JP
- Japan
- Prior art keywords
- silver
- plating
- derivative
- plating bath
- precipitation
- 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.)
- Granted
Links
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 57
- 239000004332 silver Substances 0.000 title claims abstract description 57
- 238000007747 plating Methods 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title claims description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000001301 oxygen Substances 0.000 claims abstract description 16
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 16
- KZNICNPSHKQLFF-UHFFFAOYSA-N succinimide Chemical compound O=C1CCC(=O)N1 KZNICNPSHKQLFF-UHFFFAOYSA-N 0.000 claims abstract description 10
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 6
- 239000008139 complexing agent Substances 0.000 claims abstract description 6
- WJRBRSLFGCUECM-UHFFFAOYSA-N hydantoin Chemical compound O=C1CNC(=O)N1 WJRBRSLFGCUECM-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229960002317 succinimide Drugs 0.000 claims abstract description 6
- 150000001447 alkali salts Chemical class 0.000 claims abstract description 5
- 229940091173 hydantoin Drugs 0.000 claims description 5
- 150000001875 compounds Chemical class 0.000 claims description 4
- 238000001556 precipitation Methods 0.000 abstract description 12
- 230000002950 deficient Effects 0.000 abstract description 3
- 238000002347 injection Methods 0.000 abstract description 3
- 239000007924 injection Substances 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 3
- 239000011521 glass Substances 0.000 abstract description 2
- -1 sulfine compound Chemical class 0.000 abstract description 2
- 239000000243 solution Substances 0.000 abstract 1
- 239000002244 precipitate Substances 0.000 description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 230000008021 deposition Effects 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- YIROYDNZEPTFOL-UHFFFAOYSA-N 5,5-Dimethylhydantoin Chemical compound CC1(C)NC(=O)NC1=O YIROYDNZEPTFOL-UHFFFAOYSA-N 0.000 description 2
- RHYBFKMFHLPQPH-UHFFFAOYSA-N N-methylhydantoin Chemical compound CN1CC(=O)NC1=O RHYBFKMFHLPQPH-UHFFFAOYSA-N 0.000 description 2
- JEHKKBHWRAXMCH-UHFFFAOYSA-N benzenesulfinic acid Chemical compound O[S@@](=O)C1=CC=CC=C1 JEHKKBHWRAXMCH-UHFFFAOYSA-N 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- RFTORHYUCZJHDO-UHFFFAOYSA-N 1,3-dimethylimidazolidine-2,4-dione Chemical compound CN1CC(=O)N(C)C1=O RFTORHYUCZJHDO-UHFFFAOYSA-N 0.000 description 1
- DILXLMRYFWFBGR-UHFFFAOYSA-N 2-formylbenzene-1,4-disulfonic acid Chemical compound OS(=O)(=O)C1=CC=C(S(O)(=O)=O)C(C=O)=C1 DILXLMRYFWFBGR-UHFFFAOYSA-N 0.000 description 1
- FXJVNINSOKCNJP-UHFFFAOYSA-M 4-methylbenzenesulfinate Chemical compound CC1=CC=C(S([O-])=O)C=C1 FXJVNINSOKCNJP-UHFFFAOYSA-M 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 description 1
- CXOFVDLJLONNDW-UHFFFAOYSA-N Phenytoin Chemical compound N1C(=O)NC(=O)C1(C=1C=CC=CC=1)C1=CC=CC=C1 CXOFVDLJLONNDW-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 150000001469 hydantoins Chemical class 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000005373 porous glass Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- BHZRJJOHZFYXTO-UHFFFAOYSA-L potassium sulfite Chemical compound [K+].[K+].[O-]S([O-])=O BHZRJJOHZFYXTO-UHFFFAOYSA-L 0.000 description 1
- 235000019252 potassium sulphite Nutrition 0.000 description 1
- LZSBNSVOXWMXLL-UHFFFAOYSA-M potassium;benzenesulfinate Chemical compound [K+].[O-]S(=O)C1=CC=CC=C1 LZSBNSVOXWMXLL-UHFFFAOYSA-M 0.000 description 1
- LFAGQMCIGQNPJG-UHFFFAOYSA-N silver cyanide Chemical compound [Ag+].N#[C-] LFAGQMCIGQNPJG-UHFFFAOYSA-N 0.000 description 1
- 229940098221 silver cyanide Drugs 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- KFZUDNZQQCWGKF-UHFFFAOYSA-M sodium;4-methylbenzenesulfinate Chemical compound [Na+].CC1=CC=C(S([O-])=O)C=C1 KFZUDNZQQCWGKF-UHFFFAOYSA-M 0.000 description 1
- CHLCPTJLUJHDBO-UHFFFAOYSA-M sodium;benzenesulfinate Chemical compound [Na+].[O-]S(=O)C1=CC=CC=C1 CHLCPTJLUJHDBO-UHFFFAOYSA-M 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Landscapes
- Electroplating And Plating Baths Therefor (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】この発明は非シアン系銀めっき浴
の銀の沈殿を防止して、析出効率を高めることができる
銀めっき方法に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a silver plating method capable of preventing the precipitation of silver in a non-cyan type silver plating bath and enhancing the efficiency of precipitation.
【０００２】[0002]
【従来の技術】銀めっきは、古くから装飾用、洋食器具
等に用いられ、そしてまたその優れた電気的特性のため
にスイッチやコネクタなどの材料として電子工業分野に
おいても広く利用されている。2. Description of the Related Art Silver plating has been used for a long time in ornaments, western foods and the like, and because of its excellent electrical characteristics, it has been widely used in the electronics industry as a material for switches and connectors.
【０００３】そして、銀めっきに用いられる銀めっき浴
としては、ほとんどがシアン化銀を含んだシアン浴であ
ったが、最近では、作業安全上或いは排水処理上の要請
から非シアン系の銀めっき浴も各種提案されている（例
えば、特開平６−３３０３７２号公報参照）。Most of the silver plating baths used for silver plating were cyanide baths containing silver cyanide, but recently, non-cyan type silver plating is required due to work safety or wastewater treatment. Various baths have been proposed (for example, see JP-A-6-330372).
【０００４】[0004]
【発明が解決しようとする課題】しかしながら、非シア
ン系の銀めっき浴では、銀の析出電位が他の金属に比べ
て貴であるため、浴中で分解して銀が沈殿し易いという
問題がある。銀が沈殿すると、浴中銀濃度低下による析
出速度の低下や、被めっき物表面への銀沈殿物の付着に
よる析出物特性の劣化に起因した不良品の発生という不
具合を生ずる。However, in the non-cyan type silver plating bath, the deposition potential of silver is nobler than that of other metals, and therefore, there is a problem that silver is easily decomposed in the bath to precipitate silver. is there. Precipitation of silver causes problems such as a decrease in the deposition rate due to a decrease in silver concentration in the bath and the occurrence of defective products due to the deterioration of the characteristics of the deposit due to the adhesion of the silver precipitate to the surface of the object to be plated.
【０００５】この発明はこのような従来の技術に着目し
てなされたものであり、銀が沈殿せず、安定して良好な
銀析出物を得ることができる銀めっき方法を提供するも
のである。The present invention has been made by paying attention to such a conventional technique, and provides a silver plating method in which silver does not precipitate and a stable silver deposit can be obtained. .
【０００６】[0006]
【課題を解決するための手段】この発明に係る銀めっき
方法は、光沢度調整剤として、亜硫酸及びそのアルカリ
塩又はスルフィン化合物を含有しており、錯化剤とし
て、コハク酸イミド及びその誘導体又はヒダントイン及
びその誘導体を含有してなる銀めっき浴に、酸素又は空
気を銀めっき浴中に分散供給させながらめっきを行うも
のである。銀めっき浴中に酸化力をもつ気体（酸素又は
空気）を分散させることにより、浴中の銀の沈殿を抑え
たり、或いは発生した銀の沈殿物を溶解させることがで
きるため、無駄な銀の消耗が抑えられると共に、発生し
た銀粒の析出物への付着による不良品の発生を抑制でき
る。The silver plating method according to the present invention contains sulfurous acid and an alkali salt thereof or a sulfin compound as a gloss adjusting agent, and succinimide and a derivative thereof as a complexing agent. The plating is performed while oxygen or air is dispersedly supplied to the silver plating bath containing hydantoin and its derivative. Dispersing a gas having oxidizing power (oxygen or air) in the silver plating bath can suppress the precipitation of silver in the bath or dissolve the generated silver precipitate, so that unnecessary silver The consumption can be suppressed, and the generation of defective products due to the adhesion of generated silver particles to the precipitate can be suppressed.
【０００７】[0007]
【発明の実施の形態】利用するめっき装置としては、密
閉型のめっき槽を有する噴射めっき装置が好適で、例え
ば３０リットルの容量のめっき槽に対しては、銀めっき
浴中に分散させる酸素の量としては、１００ｃｃ／分以
上であれば、少なくとも浴中の銀の沈殿を抑制すること
ができる。BEST MODE FOR CARRYING OUT THE INVENTION As a plating apparatus to be used, an injection plating apparatus having a closed type plating tank is suitable. For a plating tank having a capacity of 30 liters, for example, the amount of oxygen dispersed in the silver plating bath is If the amount is 100 cc / min or more, at least the precipitation of silver in the bath can be suppressed.
【０００８】また、めっき槽の浴中に酸素又は空気を均
一分散させるための酸素分散供給手段としては、ガラス
製、セラミックス製、或いはプラスチック製の多孔質体
等を用いることができる。As the oxygen dispersion supply means for uniformly dispersing oxygen or air in the bath of the plating tank, glass, ceramics, or plastic porous bodies can be used.
【０００９】銀めっき浴の浴温としては、３０〜９０℃
が好適である。これ以外の範囲だと、良好な析出物が得
られない。The bath temperature of the silver plating bath is 30 to 90 ° C.
Is preferred. If it is outside this range, good precipitates cannot be obtained.
【００１０】また、ｐＨは７〜１３が好適である。これ
以外の範囲だと、浴の安定性が低下する。The pH is preferably 7 to 13. If it is outside this range, the stability of the bath will be reduced.
【００１１】このめっき方法に使用する銀めっき浴は、
光沢度調整剤として、亜硫酸及びそのアルカリ塩又はス
ルフィン化合物を含有しており、錯化剤として、コハク
酸イミド及びその誘導体又はヒダントイン及びその誘導
体を含有したものが良い。The silver plating bath used in this plating method is
It is preferable to contain sulfurous acid and an alkali salt thereof or a sulfin compound as a glossiness adjusting agent, and to contain succinimide and a derivative thereof or hydantoin and a derivative thereof as a complexing agent.
【００１２】スルフィン化合物の具体例としては、Ｐ−
トルエンスルフィン酸、Ｐ−トルエンスルフィン酸カリ
ウム、Ｐ−トルエンスルフィン酸ナトリウム、ベンゼン
スルフィン酸、ベンゼンスルフィン酸ナトリウム、ベン
ゼンスルフィン酸カリウムが好適である。Specific examples of the sulfine compound include P-
Toluenesulfinic acid, potassium P-toluenesulfinate, sodium P-toluenesulfinate, benzenesulfinic acid, sodium benzenesulfinate and potassium benzenesulfinate are preferred.
【００１３】ヒダントイン化合物としては、ヒダントイ
ン、１−メチルヒダントイン、１，３−ジメチルヒダン
トイン、５，５−ジメチルヒダントイン、１−メタノー
ル−５，５−ジメチルヒダントイン、５，５−ジフェニ
ルヒダントイン等が好適である。Suitable hydantoin compounds are hydantoin, 1-methylhydantoin, 1,3-dimethylhydantoin, 5,5-dimethylhydantoin, 1-methanol-5,5-dimethylhydantoin, 5,5-diphenylhydantoin and the like. is there.
【００１４】この酸素供給による分解沈殿抑制の効果
は、銀めっき浴が、光沢度調整剤として、亜硫酸及びそ
のアルカリ塩又はスルフィン化合物を含有しており、錯
化剤として、コハク酸イミド及びその誘導体又はヒダン
トイン及びその誘導体を含有しした非シアン浴の場合に
顕著である。その理由は、これらの浴は、シアン浴に比
べると銀錯イオンの安定性が低く、上記還元性の添加剤
を用いた場合には、銀沈を生じやすいためである。The effect of suppressing decomposition and precipitation by supplying oxygen is that the silver plating bath contains sulfurous acid and its alkali salt or a sulfin compound as a gloss adjusting agent, and succinimide and its derivative as a complexing agent. Or, it is remarkable in the case of a non-cyan bath containing hydantoin and its derivative. The reason is that these baths have lower stability of silver complex ions than the cyan baths, and silver precipitation is likely to occur when the reducing additive is used.
【００１５】[0015]
【実施例】密閉型のめっき槽を有する噴射めっき装置を
使用して、銅の試験片に銀めっきする場合の実施例を説
明する。この噴射めっきは、温度６０℃、ポンプ流量１
２リットル／分、めっき面積１ｃｍ2 、電流密度５０Ａ
／ｄｍ2 で、酸素分散供給手段としてはガラス製多孔質
体が使用され、めっき槽の浴中には酸素量として１００
ｃｃ／分以上の空気が供給されている。[Example] An example in which a copper test piece is silver-plated by using an injection plating apparatus having a closed plating tank will be described. This spray plating has a temperature of 60 ° C and a pump flow rate of 1
2 liters / minute, plating area 1 cm 2 , current density 50 A
/ Dm 2 , a porous glass body is used as the oxygen dispersion supply means, and the oxygen content in the bath of the plating tank is 100
Air of cc / min or more is supplied.
【００１６】また、この実施例で使用した銀めっき浴の
組成は以下の通りである。 ＊硝酸銀（銀として）……………………………… ８０ｇ／リットル ＊５，５−ジメチルヒダントイン…………………３００ｇ／リットル ＊水酸化カリウム……………………………………１５０ｇ／リットル ＊亜硫酸カリウム…………………………………… ６０ｇ／リットル ＊ｐＨ………………………………………………… １１．０The composition of the silver plating bath used in this example is as follows. * Silver nitrate (as silver) ……………………………… 80g / liter * 5,5-Dimethylhydantoin ……………… 300g / liter * Potassium hydroxide ……………… ……………… 150g / liter * Potassium sulfite …………………………………… 60g / liter * pH …………………………………………………… 11.0
【００１７】そして、めっき中に銀めっき浴の銀が沈殿
するかどうか調べてみた。また、酸素を供給しない比較
実験も行った。両者の銀めっき浴における銀の沈殿状態
を、８０℃に昇温したまま保持し、めっき槽の窓（透明
耐熱ビニール製）への銀の付着を見るという方法により
調べたところ、酸素を供給した方は銀の沈殿が生ぜず、
酸素を供給しない方は、従来技術通りに銀が沈殿した。
また、めっき実験（６５℃、５０Ａ／ｄｍ2 、噴流式）
を行ったところ、酸素を供給しない場合は、めっき物表
面への銀粒子の付着が見られた。Then, it was examined whether silver in the silver plating bath was precipitated during plating. In addition, a comparative experiment in which oxygen was not supplied was also performed. When the precipitation state of silver in both silver plating baths was kept at 80 ° C. while being heated and the adhesion of silver to the window (made of transparent heat-resistant vinyl) of the plating tank was examined, oxygen was supplied. One does not have silver precipitation,
Those who did not supply oxygen precipitated silver as in the prior art.
In addition, plating experiment (65 ° C, 50 A / dm 2 , jet type)
When no oxygen was supplied, the adhesion of silver particles to the surface of the plated product was observed.
【００１８】[0018]
【発明の効果】銀めっき浴中に酸化力をもつ気体（酸素
又は空気）を分散させることにより、浴中の銀の沈殿を
抑えたり、或いは発生した銀の沈殿物を溶解させること
ができ、銀の析出効率の向上を図ることができる。EFFECT OF THE INVENTION By dispersing a gas having an oxidizing power (oxygen or air) in the silver plating bath, it is possible to suppress the precipitation of silver in the bath or dissolve the generated silver precipitate, It is possible to improve the silver deposition efficiency.
Claims (1)
ルカリ塩又はスルフィン化合物を含有しており、錯化剤
として、コハク酸イミド及びその誘導体又はヒダントイ
ン及びその誘導体を含有してなる銀めっき浴に、酸素又
は空気を銀めっき浴中に分散供給させながらめっきを行
うことを特徴とする銀めっき方法。1. A silver plating bath containing sulfurous acid and an alkali salt thereof or a sulfinic compound as a glossiness adjusting agent, and succinimide and a derivative thereof or hydantoin and a derivative thereof as a complexing agent. A silver plating method, wherein plating is performed while oxygen or air is dispersedly supplied in a silver plating bath.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP06431496A JP3512943B2 (en) | 1996-03-21 | 1996-03-21 | Silver plating method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP06431496A JP3512943B2 (en) | 1996-03-21 | 1996-03-21 | Silver plating method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH09256186A true JPH09256186A (en) | 1997-09-30 |
| JP3512943B2 JP3512943B2 (en) | 2004-03-31 |
Family
ID=13254661
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP06431496A Expired - Fee Related JP3512943B2 (en) | 1996-03-21 | 1996-03-21 | Silver plating method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3512943B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000355792A (en) * | 2000-01-27 | 2000-12-26 | Electroplating Eng Of Japan Co | Gold plating liquid and gold plating method using the same |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109504989A (en) * | 2018-12-11 | 2019-03-22 | 湖北工程学院 | A kind of bright brush plating silver plating liquid and its preparation process, application method |
-
1996
- 1996-03-21 JP JP06431496A patent/JP3512943B2/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000355792A (en) * | 2000-01-27 | 2000-12-26 | Electroplating Eng Of Japan Co | Gold plating liquid and gold plating method using the same |
Also Published As
| Publication number | Publication date |
|---|---|
| JP3512943B2 (en) | 2004-03-31 |
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