JPH02138484A - High phosphorus-content nickel plating method - Google Patents
High phosphorus-content nickel plating methodInfo
- Publication number
- JPH02138484A JPH02138484A JP28848088A JP28848088A JPH02138484A JP H02138484 A JPH02138484 A JP H02138484A JP 28848088 A JP28848088 A JP 28848088A JP 28848088 A JP28848088 A JP 28848088A JP H02138484 A JPH02138484 A JP H02138484A
- Authority
- JP
- Japan
- Prior art keywords
- plating
- film
- bath
- electroless
- phosphorus
- 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.)
- Pending
Links
- 238000007747 plating Methods 0.000 title claims abstract description 42
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 title claims description 8
- 239000011574 phosphorus Substances 0.000 claims abstract description 22
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 22
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000007772 electroless plating Methods 0.000 claims abstract description 12
- 238000009713 electroplating Methods 0.000 claims abstract description 11
- 229910000679 solder Inorganic materials 0.000 abstract description 10
- 239000000126 substance Substances 0.000 abstract description 7
- 239000000758 substrate Substances 0.000 abstract description 6
- 238000000576 coating method Methods 0.000 description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 6
- 239000011889 copper foil Substances 0.000 description 5
- 238000005299 abrasion Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000007654 immersion Methods 0.000 description 3
- 238000005476 soldering Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- SOBHUZYZLFQYFK-UHFFFAOYSA-K trisodium;hydroxy-[[phosphonatomethyl(phosphonomethyl)amino]methyl]phosphinate Chemical compound [Na+].[Na+].[Na+].OP(O)(=O)CN(CP(O)([O-])=O)CP([O-])([O-])=O SOBHUZYZLFQYFK-UHFFFAOYSA-K 0.000 description 2
- FTLYMKDSHNWQKD-UHFFFAOYSA-N (2,4,5-trichlorophenyl)boronic acid Chemical compound OB(O)C1=CC(Cl)=C(Cl)C=C1Cl FTLYMKDSHNWQKD-UHFFFAOYSA-N 0.000 description 1
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 description 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- 101100257134 Caenorhabditis elegans sma-4 gene Proteins 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- LHIJANUOQQMGNT-UHFFFAOYSA-N aminoethylethanolamine Chemical compound NCCNCCO LHIJANUOQQMGNT-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 238000004453 electron probe microanalysis Methods 0.000 description 1
- 229910001325 element alloy Inorganic materials 0.000 description 1
- 230000005496 eutectics Effects 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- INHCSSUBVCNVSK-UHFFFAOYSA-L lithium sulfate Inorganic materials [Li+].[Li+].[O-]S([O-])(=O)=O INHCSSUBVCNVSK-UHFFFAOYSA-L 0.000 description 1
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 1
- OFNHPGDEEMZPFG-UHFFFAOYSA-N phosphanylidynenickel Chemical compound [P].[Ni] OFNHPGDEEMZPFG-UHFFFAOYSA-N 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 229940085605 saccharin sodium Drugs 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910001379 sodium hypophosphite Inorganic materials 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- RBTVSNLYYIMMKS-UHFFFAOYSA-N tert-butyl 3-aminoazetidine-1-carboxylate;hydrochloride Chemical compound Cl.CC(C)(C)OC(=O)N1CC(N)C1 RBTVSNLYYIMMKS-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/22—Secondary treatment of printed circuits
- H05K3/24—Reinforcing the conductive pattern
Abstract
Description
【発明の詳細な説明】
〔発明の目的、〕
(産業上の利用分野)
本発明は高リン含有ニッケルメッキ法に関するもので、
摺動部を有する電気接点、プリント基板及び半田付部の
ある電気部品、配線部品に利用されるものである。[Detailed Description of the Invention] [Object of the Invention] (Field of Industrial Application) The present invention relates to a high phosphorus-containing nickel plating method,
It is used for electrical contacts with sliding parts, printed circuit boards, electrical parts with soldering parts, and wiring parts.
(従来の技術)
本発明に係る従来の技術としては特開昭6024888
2号の公報がある。(Prior art) As a conventional technology related to the present invention, Japanese Patent Application Laid-Open No. 6024888
There is a 2nd bulletin.
このものは、ニッケル膜中に原子比で20〜25%もの
高い比率でリンを含有させることが可能な無電解メッキ
浴で、この方法に作成された無電解ニッケルリン被膜は
、被膜中に20〜25%のリンを含有しており、耐薬品
性、耐摩耗性に優れている。This is an electroless plating bath that can contain phosphorus at a high atomic ratio of 20 to 25% in the nickel film. Contains ~25% phosphorus and has excellent chemical resistance and wear resistance.
(発明が解決しようとする課り
しかし前記高リン含有ニッケルメッキ法によるメッキ被
膜は摺動部を有する電気接点等の電気部品に応用した場
合に、必ず半田付工程があり、この半田濡れ性が悪いた
めに、電気接点を有する電気部品の製品に使用されない
という問題点がある。(Issues that the invention seeks to solve) However, when the plating film produced by the high phosphorus content nickel plating method is applied to electrical parts such as electrical contacts that have sliding parts, there is always a soldering process, and this solder wettability is There is a problem in that, because of the poor quality, it is not used in products with electrical parts that have electrical contacts.
本発明は前記高リン含有ニッケルメッキ法によるメッキ
被膜に於いて、半田濡れ性の優れた無電解メッキ方法を
技術的課題とするもである。The technical object of the present invention is to provide an electroless plating method that provides excellent solder wettability in the plating film formed by the high phosphorus-containing nickel plating method.
(課題を解決するための手段)
前記技術的課題を解決するために講じた技術的手段は次
のようである。すなわち、
被メッキ物のメッキ膜中に原子比20〜25%の高い比
率でリンを含有することが可能な無電解メッキ浴でメッ
キ後、被メッキ物を前記メッキ浴から出すことなく、連
続に同じメッキ浴に浸漬させたまま、1〜IOA/dm
”の電流密度の電流を1−10分又はそれ以上の間流し
、被メッキ物の表面上に電気メッキ層を薄く積層する高
リン含有ニッケルメッキ無電解メッキ方法である。(Means for solving the problem) The technical means taken to solve the above technical problem are as follows. That is, after plating with an electroless plating bath capable of containing phosphorus at a high atomic ratio of 20 to 25% in the plating film of the object to be plated, the object to be plated is continuously coated without taking it out of the plating bath. 1 to IOA/dm while immersed in the same plating bath
This is an electroless plating method for high phosphorus-containing nickel plating, in which a current with a current density of 1 to 10 minutes or more is passed for 1 to 10 minutes or more to form a thin electroplating layer on the surface of the object to be plated.
耐薬品性1、耐摩耗性に優れた無電解ニッケルリン被膜
上に、電気メッキにより被膜の最上部のみにリン含有率
を強制的に低下させたメッキ膜を設けたもので、半田濡
れ性が大幅に向上するものである。On top of the electroless nickel phosphorus coating, which has chemical resistance 1 and excellent wear resistance, a plating film with a forced reduction in phosphorus content is applied only to the top of the coating by electroplating, resulting in improved solder wettability. This is a significant improvement.
無電解メッキと電解メッキについては、(1)Nt”→
Ni’ −2e−、(2)3PO”→P0+2PO!−
+2e−で、無電解メッキ、電気メッキ共メッキ浴中に
て上記(1)、 (2)の反応が起こっているが、電
気メッキの場合前記(1)の反応は電流密度の大きさに
支配されており、それに比べ(2)の反応はほとんど一
定である。Regarding electroless plating and electrolytic plating, (1) Nt”→
Ni' -2e-, (2) 3PO"→P0+2PO!-
+2e-, the reactions (1) and (2) above occur in both electroless plating and electroplating baths, but in the case of electroplating, the reaction (1) above is dominated by the magnitude of the current density. In comparison, the reaction in (2) is almost constant.
従って、電流密度をかえることにより被膜中のリン含有
率をコントロールすることが可能である。Therefore, it is possible to control the phosphorus content in the coating by changing the current density.
本発明は高リン含有の無電解メッキ膜の最上部層に原子
比で最大25%までの範囲でリン含有率を制御したニッ
ケル膜を積層させることにより耐薬品性、耐摩耗性の特
性にさらに半田濡れ性を向上したものである。The present invention further improves chemical resistance and abrasion resistance by laminating a nickel film with a controlled phosphorus content within a range of up to 25% in atomic ratio on the top layer of a high phosphorus-containing electroless plated film. It has improved solder wettability.
(実施例) 以下実施例について説明する。(Example) Examples will be described below.
第1図は摺動部Aをする電気接点で、1はエポキシ板で
、前記摺動部は銅箔2及びメッキ膜3よりなり、4は6
元系元金ブラシである。Figure 1 shows an electrical contact with a sliding part A, where 1 is an epoxy plate, the sliding part is made of copper foil 2 and a plating film 3, and 4 is 6
It is a Genkin Genkin brush.
ガラスエボキン銅張り積層板(CEM3.銅箔厚み35
μm)に所定形状パターンがエツチング法により形成さ
れた基板1の銅箔部2に高リン含有無電解ニッケルメッ
キ3 くアモルファスメッキ)を施すものである。Glass Evokin copper clad laminate (CEM3. Copper foil thickness 35
High phosphorus-containing electroless nickel plating (amorphous plating) is applied to the copper foil portion 2 of the substrate 1, on which a predetermined pattern (μm) has been formed by etching.
メッキの前処理としては、
(1)脱脂・・・opcクリーン91 (奥野製薬)、
50cc/l (イオン交換水)30℃、2分浸漬、
(2)ソフトエツチング・・・渦流酸ナトリウム(Na
z sz ol )100g/I! (イオン交換水3
0℃2分、
(3)酸洗・・・硫酸100”/j’ (イオン交換水
)30℃1分浸漬、
の3工程で処理した。Pretreatment for plating includes: (1) Degreasing: OPC Clean 91 (Okuno Pharmaceutical);
50cc/l (ion-exchanged water) 30℃, 2 minute immersion, (2) Soft etching...sodium sulfate (Na
z sz ol ) 100g/I! (Ion exchange water 3
The treatment was carried out in three steps: 0°C for 2 minutes, (3) Pickling: immersion in sulfuric acid 100''/j' (ion-exchanged water) at 30°C for 1 minute.
次に高リンニッケルメッキについては特願昭60−24
8882号公報に記載のように、塩化ニッケル・・・2
0g/I!、次亜リン酸ナトリウム・・・100g/l
、 リエン酸3ナトリウム・・・50g/j!、 サ
ッカリンナトリウム・・・2gIC硫酸リチウム・・・
25g/1.※C3゜H1sNa30.・・・3g/L
※(N−2ヒドロキシエチルエチレンジアミンNN’
N”酢酸3ナトリウム)
よりなるメ・ンキン夜にて行う。Next, regarding high phosphorous nickel plating, a patent application was filed in 1986-24.
As described in Publication No. 8882, nickel chloride...2
0g/I! , Sodium hypophosphite...100g/l
, Trisodium lienoate...50g/j! , Saccharin sodium...2g IC lithium sulfate...
25g/1. *C3゜H1sNa30. ...3g/L *(N-2 hydroxyethylethylenediamine NN'
N"trisodium acetate)
メッキ液は90℃、PHは4.6に調整し、前処理の終
了した基板をこのメッキ液に浸漬し、1分間、1■の通
電を行う。The plating solution was adjusted to 90° C. and pH 4.6, and the pretreated substrate was immersed in the plating solution, and a current of 1× was applied for 1 minute.
このとき基板は陰極であり、陽極としてステンレス板又
はニッケル板を使用してもよい。At this time, the substrate is a cathode, and a stainless steel plate or a nickel plate may be used as an anode.
1分後通電をやめ80分無電解メッキを行うと、約7μ
mのメッキ膜が形成される。After 1 minute, the current was turned off and electroless plating was performed for 80 minutes.
m plating films are formed.
その後前記基板をメッキ沿から出さすに、2.5A/d
m”の大きさの電流を流すと(このとき基板は陰極、陽
極はニッケル板)、5分で約1.5μmの電気メッキ被
膜が無電解被膜に形成される。このときの最表面のリン
含有率はEPMA分析により、原子比で10%である。After that, when the board was taken out from the plating side, it was 2.5A/d.
When a current with a magnitude of 1.5 m is applied (at this time, the substrate is the cathode and the anode is a nickel plate), an electroplated film of about 1.5 μm is formed on the electroless film in 5 minutes. The content is 10% in atomic ratio according to EPMA analysis.
次に第2図〜第4図にメッキ被膜の断面を示す、第3図
に示す高すン含有無電解+低リン含有電解によるニッケ
ルメッキ被膜と、第2図に示す従来の高リン含有無電解
ニッケル被膜及び第4図に示す電気メッキのみのニッケ
ル被膜との半田濡れ性、耐薬品性、耐摩耗性についての
比較を第1表に示す、第2図〜第4図に於いて5はガラ
スエボキン6は銅箔、7は無電解メッキ膜、8は電解メ
ッキ膜である。Next, Figures 2 to 4 show the cross-sections of the plated coatings; Figure 3 shows the electroless nickel plating with high phosphorus content and electrolytic low phosphorus content, and the conventional non-electrolytic high phosphorus coating shown in Figure 2. Table 1 shows a comparison of solder wettability, chemical resistance, and abrasion resistance between the electrolytic nickel coating and the electroplated nickel coating shown in Figure 4. Glass Evokin 6 is a copper foil, 7 is an electroless plating film, and 8 is an electrolytic plating film.
注1.濡れ面積において、テストピースにレジン系フラ
ックスを塗布後乾燥させ、230±3℃に温調された共
晶半田の槽へ5±0.5秒浸漬、注2.耐薬品性につい
ては塩化第2鉄300g/l、30℃、1分間浸漬、
注3.耐摩耗性について6元素合金(Pt、 Au。Note 1. In the wet area, apply resin-based flux to the test piece, dry it, and immerse it in a eutectic solder bath temperature-controlled at 230 ± 3°C for 5 ± 0.5 seconds. Note 2. Regarding chemical resistance, immersion in ferric chloride 300g/l, 30°C, 1 minute, Note 3. Regarding wear resistance, six element alloys (Pt, Au.
Pd、他元素)ブラシにて、テストピースに9gの荷重
を加え200万回往復、
上記の結果より、従来の優れた特性(耐薬品性、耐摩耗
性)を損なうことなく、又欠点とされていた半田1濡れ
性を大きく向上させることができた。A load of 9g was applied to the test piece using a brush (Pd, other elements), and the test piece was reciprocated 2 million times. From the above results, it was found that the previous excellent properties (chemical resistance, abrasion resistance) were not impaired, and no defects were identified. It was possible to greatly improve the wettability of solder 1, which had been previously used.
第5図は本実施例の場合の無電解メッキ膜+電気メッキ
膜の厚み方向のリン含有率を表したもので、第6図は本
実施例の電流と時間との関係を表したものである。Figure 5 shows the phosphorus content in the thickness direction of the electroless plated film + electroplated film in this example, and Figure 6 shows the relationship between current and time in this example. be.
本発明は次の効果を有する。すなわち、従来技術に比較
して半田濡れ性が良く、半田付作業についてロボット等
により自動化する場合には極めて有効なものである。The present invention has the following effects. That is, the solder wettability is better than that of the conventional technology, and it is extremely effective when automating soldering work using a robot or the like.
第1図の(イ)は摺動部を有する電気接点の説明図、(
ロ)は(イ)の要部の断面図、第2図〜ヰ
第9図は各メッキ層の断面説明図、第5図はメッキ層の
厚みとリン含有率との関係図、第6図は本実施例の電流
と時間の関係図である。
A・・・電気的摺動部。
■・・・基板。
2.6・・・銅箔。
3・・・メッキ膜。
7・・・無電解メッキ膜
8・・・電解メッキ膜。Figure 1 (a) is an explanatory diagram of an electrical contact having a sliding part;
b) is a sectional view of the main part of (a), Figs. 2 to 9 are explanatory cross-sectional views of each plating layer, Fig. 5 is a relationship between the thickness of the plating layer and the phosphorus content, and Fig. 6 is a diagram showing the relationship between current and time in this embodiment. A...Electrical sliding part. ■... Board. 2.6...Copper foil. 3... Plating film. 7... Electroless plating film 8... Electrolytic plating film.
Claims (1)
比率でリンを含有することが可能な無電解メッキ浴でメ
ッキ後、前記被メッキ物を前記メッキ浴から出すことな
く、連続的にメッキ浴中に浸漬させたまま、1〜10A
/dm^2の電流密度の電流を1〜10分又はそれ以上
の間流し、被メッキ物の表面上に電気メッキ層を薄く積
層する高リン含有ニッケルメッキ方法。After plating with an electroless plating bath capable of containing phosphorus at a high atomic ratio of 20 to 25% in the plating film of the object to be plated, the object to be plated is continuously coated without taking it out of the plating bath. 1 to 10 A while immersed in the plating bath.
A high phosphorus-containing nickel plating method in which a current with a current density of /dm^2 is passed for 1 to 10 minutes or more to deposit a thin electroplating layer on the surface of the object to be plated.
Priority Applications (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP28848088A JPH02138484A (en) | 1988-11-15 | 1988-11-15 | High phosphorus-content nickel plating method |
US07/436,647 US4994329A (en) | 1988-11-15 | 1989-11-15 | Article having nickel plated film comprising a varying content of phosphorus |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP28848088A JPH02138484A (en) | 1988-11-15 | 1988-11-15 | High phosphorus-content nickel plating method |
Publications (1)
Publication Number | Publication Date |
---|---|
JPH02138484A true JPH02138484A (en) | 1990-05-28 |
Family
ID=17730753
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP28848088A Pending JPH02138484A (en) | 1988-11-15 | 1988-11-15 | High phosphorus-content nickel plating method |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPH02138484A (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2000015876A1 (en) * | 1998-09-11 | 2000-03-23 | Nippon Mining & Metals Co., Ltd. | Metal material |
JP2015170575A (en) * | 2014-03-10 | 2015-09-28 | セイコーインスツル株式会社 | Substrate unit, electrochemical cell unit and manufacturing method for electrochemical cell unit |
-
1988
- 1988-11-15 JP JP28848088A patent/JPH02138484A/en active Pending
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2000015876A1 (en) * | 1998-09-11 | 2000-03-23 | Nippon Mining & Metals Co., Ltd. | Metal material |
US6613451B1 (en) | 1998-09-11 | 2003-09-02 | Nippon Mining & Metals Co., Ltd. | Metallic material |
JP2015170575A (en) * | 2014-03-10 | 2015-09-28 | セイコーインスツル株式会社 | Substrate unit, electrochemical cell unit and manufacturing method for electrochemical cell unit |
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