JP2000144440A - Electroless silver plating solution for electronic parts - Google Patents
Electroless silver plating solution for electronic partsInfo
- Publication number
- JP2000144440A JP2000144440A JP10328373A JP32837398A JP2000144440A JP 2000144440 A JP2000144440 A JP 2000144440A JP 10328373 A JP10328373 A JP 10328373A JP 32837398 A JP32837398 A JP 32837398A JP 2000144440 A JP2000144440 A JP 2000144440A
- Authority
- JP
- Japan
- Prior art keywords
- silver
- plating solution
- silver plating
- electroless
- electroless silver
- 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
Classifications
-
- 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
-
- 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
- H05K3/244—Finish plating of conductors, especially of copper conductors, e.g. for pads or lands
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、電子部品用無電解
銀めっき液に関する。[0001] The present invention relates to an electroless silver plating solution for electronic parts.
【０００２】[0002]
【従来の技術】従前よりプリント配線板などの電子部品
の製造においては、銅パターン上にＮｉ合金層、または
金や銅パターン上にＳｎ−Ｐｂ合金層を設け、これにコ
ンデンサー、抵抗、トランジスター、ＩＣなどの部品を
実装している。しかし近年、環境保全の観点から有害物
質であるＰｂはその使用が中止となり、Ｎｉは使用制限
されつつある。2. Description of the Related Art Conventionally, in the manufacture of electronic parts such as printed wiring boards, a Ni alloy layer is provided on a copper pattern, or an Sn-Pb alloy layer is provided on a gold or copper pattern, and a capacitor, a resistor, a transistor, Components such as IC are mounted. However, in recent years, the use of Pb, which is a harmful substance, has been discontinued from the viewpoint of environmental conservation, and the use of Ni has been restricted.
【０００３】そこで、ＮｉやＰｂを使用せずに、銅パタ
ーン上にＡｇめっき層を設けた電子部品を作る方法が試
みられている。しかしＡｇはマイグレーション（電解移
行）が起こり易いためショートや絶縁破壊の故障を引き
起こすことがしばしばある。マイグレーションとは、一
種の電解腐食であり、吸湿性の比較的大きい絶縁物中で
二つの電極間に電圧がかかると、アノードから電極金属
がイオンとなって溶出し、電解腐食する現象をいう。ア
ノード付近では２ＡｇＯＨ→Ａｇ2 Ｏ＋Ｈ2 Ｏとなり、
Ａｇ2 Ｏのコロイドが生成し、Ａｇ2 Ｏは絶縁物中の還
元性物質、あるいは外的要因により還元されてＡｇイオ
ンとなりカソードに針状結晶として析出して電気的短絡
または絶縁破壊の原因となる。このため外気を完全に遮
断したりあるいはモード外部にＡｇを出さないための多
くの工夫や改善が必要となる。[0003] Therefore, a method of producing an electronic component having an Ag plating layer provided on a copper pattern without using Ni or Pb has been attempted. However, Ag easily causes migration (electrolytic migration), and thus often causes a short circuit or breakdown failure. Migration is a type of electrolytic corrosion, and refers to a phenomenon in which when a voltage is applied between two electrodes in an insulator having relatively high hygroscopicity, the electrode metal is eluted as ions from the anode, resulting in electrolytic corrosion. 2AgOH → Ag 2 O + H 2 O near the anode,
Ag 2 O colloid is generated, and Ag 2 O is reduced by a reducing substance in the insulator or by an external factor to become Ag ions and precipitates as a needle-like crystal on the cathode to cause an electrical short circuit or dielectric breakdown. Become. For this reason, many measures and improvements are required to completely shut off the outside air or to prevent Ag from being emitted outside the mode.
【０００４】しかも、従来の無電解銀めっき浴には、銀
の錯化剤にスルフォン化合物や、エチレンジアミン四酢
酸、ジエチレントリアミン五酢酸、ニトリロ三酢酸など
の多座配位子をもつ化合物を使用しているので、めっき
浴が非常に不安定で経時や光によりＡｇがめっき槽に異
常析出し、その析出片が製品に付着して不良品が発生す
る。In addition, a conventional electroless silver plating bath uses a sulfone compound or a compound having a polydentate ligand such as ethylenediaminetetraacetic acid, diethylenetriaminepentaacetic acid, or nitrilotriacetic acid as a silver complexing agent. Therefore, the plating bath is very unstable, and Ag deposits abnormally in the plating tank due to aging or light, and the deposited pieces adhere to the product, resulting in defective products.
【０００５】[0005]
【発明が解決しようとする課題】本発明は、マイグレー
ション防止効果を有し、めっき浴寿命の長い電子部品用
無電解銀めっき液を提供することを目的としている。SUMMARY OF THE INVENTION An object of the present invention is to provide an electroless silver plating solution for electronic parts having a migration preventing effect and a long plating bath life.
【０００６】[0006]
【課題を解決するための手段】本発明は、下記の事項を
その特徴としている。 （１）銀塩と、銀の錯化剤と、フッ素系界面活性剤と、
ＰＨバッファー塩とからなることを特徴とする電子部品
用無電解銀めっき液。 （２）銀塩が硝酸銀、銀の錯化剤がピロリドン化合物で
ある前記（１）に記載の無電解銀めっき液。 （３）銀イオン０．０５〜３０ｇ／ｌ、ピロリドン化合
物０．１〜２００ｇ／ｌ、フッ素系界面活性剤０．０１
〜１０ｇ／ｌ含有し、ＰＨバッファー塩として無機酸ま
たは有機酸若しくは両方を含むことを特徴とする電子部
品用無電解銀めっき液。The present invention has the following features. (1) a silver salt, a silver complexing agent, a fluorine-based surfactant,
An electroless silver plating solution for electronic components, comprising a pH buffer salt. (2) The electroless silver plating solution according to (1), wherein the silver salt is silver nitrate and the silver complexing agent is a pyrrolidone compound. (3) 0.05-30 g / l of silver ions, 0.1-200 g / l of a pyrrolidone compound, 0.01 of a fluorine-based surfactant
An electroless silver plating solution for an electronic component, comprising 10 to 10 g / l and containing an inorganic acid or an organic acid or both as a PH buffer salt.
【０００７】（４）ピロリドン化合物が、２−ピロリド
ン、３−ピロリドンおよび２−ピロリドン−５−カルボ
ン酸のうち少なくとも１種である前記（２）または
（３）に記載の電子部品用無電解銀めっき液。 （５）フッ素系界面活性剤が、パーフルオロアルキルス
ルホン酸塩、パーフルオロアルキルカルボン酸塩、パー
フルオロアルキルリン酸エステル、パーフルオロアルキ
ルアンモニウムヨウ化物、パーフルオロアルキルアミン
オキサイド、パーフルオロアルキルトリメチルアンモニ
ウム塩のうち少なくとも１種である前記（１）または
（３）に記載の電子部品用無電解銀めっき液。(4) The electroless silver for electronic parts according to (2) or (3), wherein the pyrrolidone compound is at least one of 2-pyrrolidone, 3-pyrrolidone and 2-pyrrolidone-5-carboxylic acid. Plating solution. (5) The fluorine surfactant is a perfluoroalkyl sulfonate, a perfluoroalkyl carboxylate, a perfluoroalkyl phosphate, a perfluoroalkylammonium iodide, a perfluoroalkylamine oxide, a perfluoroalkyltrimethylammonium salt The electroless silver plating solution for electronic components according to (1) or (3), which is at least one of the following.
【０００８】以下に、本発明について詳細に説明する。
本発明の電子部品用無電解銀めっき液は、銀塩、銀の錯
化剤、フッ素系界面活性剤およびＰＨバッファー塩とか
らなっている。銀塩としては硝酸銀、銀の錯化剤として
はピロリドン化合物が適当である。ピロリドン化合物と
しては、２−ピロリドン、３−ピロリドン、２−ピロリ
ドン−５−カルボン酸が使用される。Hereinafter, the present invention will be described in detail.
The electroless silver plating solution for an electronic component of the present invention comprises a silver salt, a silver complexing agent, a fluorine-based surfactant, and a PH buffer salt. Silver nitrate is suitable as a silver salt, and a pyrrolidone compound is suitable as a silver complexing agent. As the pyrrolidone compound, 2-pyrrolidone, 3-pyrrolidone, or 2-pyrrolidone-5-carboxylic acid is used.
【０００９】フッ素系界面活性剤としては、パーフルオ
ロアルキルスルホン酸塩、パーフルオロアルキルカルボ
ン酸塩、パーフルオロアルキルリン酸エステル、パーフ
ルオロアルキルアンモニウムヨウ化物、パーフルオロア
ルキルアミンオキサイド、パーフルオロアルキルトリメ
チルアンモニウム塩が使用される。ＰＨバッファー塩と
しては、リン酸化合物、ホウ酸化合物、カルボン酸化合
物、オキシ酸化合物、炭水化物などの無機酸または有機
酸若しくは両方の化合物を用いる。[0009] Fluorinated surfactants include perfluoroalkyl sulfonates, perfluoroalkyl carboxylates, perfluoroalkyl phosphates, perfluoroalkylammonium iodides, perfluoroalkylamine oxides, perfluoroalkyltrimethylammonium Salt is used. As the PH buffer salt, a phosphate compound, a boric acid compound, a carboxylic acid compound, an oxyacid compound, an inorganic acid such as a carbohydrate, or an organic acid or both compounds are used.
【００１０】本発明の無電解銀めっき液には銀の錯化剤
を用いるものが一般的であるが、下地銅材が溶け込んだ
場合には銅の錯化剤を添加しても良い。この銅の錯化剤
としては、エチレンジアミン四酢酸塩、ニトリロ三酢酸
塩、ジエチレントリアミン五酢酸塩が一般に使用され
る。Although the electroless silver plating solution of the present invention generally uses a silver complexing agent, a copper complexing agent may be added when the underlying copper material is dissolved. As the copper complexing agent, ethylenediaminetetraacetate, nitrilotriacetate, and diethylenetriaminepentaacetate are generally used.
【００１１】本発明の無電解銀めっき液は、銀イオン
０．０５〜３０ｇ／ｌ、ピロリドン化合物０．１〜２０
０ｇ／ｌ、フッ素系界面活性剤０．０１〜１０ｇ／ｌを
含有していることが好ましい。The electroless silver plating solution of the present invention contains 0.05 to 30 g / l of silver ions and 0.1 to 20 of a pyrrolidone compound.
0 g / l, and preferably 0.01 to 10 g / l of a fluorinated surfactant.
【００１２】[0012]
【実施例】以下に、本発明の電子部品用無電解銀めっき
液を実施例および比較例により説明する。電子部品とし
てプリント配線板を挙げ、その製造に本発明の無電解銀
めっき液を用いた例について述べる。各種の無電解銀め
っき液を用いて下記の製造工程によりプリント配線板を
製作した。すなわち、銅めっきまたはエッチングにより
パターン形成された有機材プリント基板を常法により脱
脂、化学研磨、酸浸漬後、表１に示す組成からなる各種
無電解銀めっき液に、３５℃で３〜８分間浸漬して０．
１０μｍの銀めっき厚を有するプリント配線板を製作し
た。EXAMPLES Hereinafter, the electroless silver plating solution for electronic parts of the present invention will be described with reference to Examples and Comparative Examples. An example in which a printed wiring board is used as an electronic component and the electroless silver plating solution of the present invention is used for the production thereof will be described. Using various electroless silver plating solutions, printed wiring boards were manufactured by the following manufacturing steps. That is, the organic printed circuit board patterned by copper plating or etching is degreased, chemically polished, and immersed in an acid by a conventional method, and is then placed in various electroless silver plating solutions having the compositions shown in Table 1 at 35 ° C. for 3 to 8 minutes. Immerse 0.
A printed wiring board having a silver plating thickness of 10 μm was manufactured.
【００１３】表１に示す組成からなる各種無電解銀めっ
き液を用いて得られたプリント配線板の銀層について
（１）マイグレーション性テスト、（２）半田濡れテス
トを行った。また各種無電解銀めっき液の浴安定性を調
査するために（３）めっき浴寿命テストを行った。前記
（１）〜（３）の各性能テストの要領は下記の通りであ
る。The silver layers of the printed wiring boards obtained by using various electroless silver plating solutions having the compositions shown in Table 1 were subjected to (1) a migration test and (2) a solder wetting test. Further, (3) plating bath life test was conducted to investigate the bath stability of various electroless silver plating solutions. The points of the performance tests (1) to (3) are as follows.
【００１４】（１）マイグレーション性テスト 極間０．３ｍｍのクシ型テストパターンを有する銀めっ
きプリント配線板を使用し、環境加速テスト条件として
湿度９０〜９５％ＲＨ、極間に直流電圧５０Ｖを付加
し、４８時間後および４８０時間後のマイグレーション
発生状況を顕微鏡で観察評価した。(1) Migration property test A silver-plated printed wiring board having a comb-shaped test pattern with a gap of 0.3 mm is used, and a humidity of 90 to 95% RH and a DC voltage of 50 V are applied between the poles as environmental acceleration test conditions. Then, the occurrence of migration after 48 hours and 480 hours was observed and evaluated with a microscope.
【００１５】（２）半田濡れ性テスト 銀めっきプリント配線板のパッドパターン上に直径０．
５ｍｍの半田ボールをのせ、非活性ロジン系フラック
（商品名Ｒ−１００：αメタル社製）を用いて２３０
℃、３０秒間加熱後の半田濡れ性を観察評価した。(2) Solder wettability test: The solder wettability test was performed on a pad pattern of a silver-plated printed wiring board with a diameter of 0.3 mm.
Place a 5 mm solder ball and use an inactive rosin-based flux (trade name: R-100: manufactured by α Metal Co., Ltd.) for 230
The solder wettability after heating at 30 ° C. for 30 seconds was observed and evaluated.
【００１６】（３）めっき浴寿命テスト 表１に示す各種組成からなる無電解銀めっき液を６０℃
で１２時間恒温槽にて放置し、銀めっき液中の銀析出有
無を観察評価した。(3) Plating bath life test An electroless silver plating solution having various compositions shown in Table 1 was heated to 60 ° C.
For 12 hours in a constant temperature bath, and the presence or absence of silver precipitation in the silver plating solution was observed and evaluated.
【００１７】性能評価テストの結果を、表２に示す。表
２においてＡ：優れている、Ｂ：やや優れている、Ｃ：
やや劣っている、Ｄ：劣っている、を表わす。Table 2 shows the results of the performance evaluation test. In Table 2, A: excellent, B: slightly excellent, C:
Inferior, D: Inferior.
【００１８】表２に示す結果からわかるように、本発明
範囲内に含まれる試料番号１〜１０については、マイグ
レーション性テストにおいて４８時間および４８０時間
後のマイグレーションの発生はなく、環境加速試験なし
の半田濡れおよびＨ2 Ｓ ０．１ｐｐｍ １時間試験後
の半田濡れはともに良好であり、さらにめっき浴寿命テ
ストにおいてめっき浴の分解がなく、総合評価において
もＡランクの評価が得られている。As can be seen from the results shown in Table 2, with respect to Sample Nos. 1 to 10 included in the scope of the present invention, migration did not occur after 48 hours and 480 hours in the migration test, and no environmental acceleration test was performed. Both the solder wettability and the solder wettability after the H 2 S 0.1 ppm 1 hour test were good, and the plating bath life test did not decompose the plating bath, and the rank A was obtained in the overall evaluation.
【００１９】これに対し本発明範囲外の試料番号１１〜
１４については、マイグレーション性テスト、半田濡れ
性テスト、めっき浴寿命テストのいずれにおいても低い
評価であり、総合評価においてもＣまたはＤの評価しか
得られていない。On the other hand, sample numbers 11 to 11 outside the scope of the present invention
14 was a low evaluation in any of the migration test, the solder wettability test, and the plating bath life test, and only C or D was obtained in the overall evaluation.
【００２０】[0020]
【表１】 [Table 1]
【００２１】[0021]
【表２】 [Table 2]
【００２２】[0022]
【発明の効果】本発明によれば、マイグレーション防止
効果に優れた、半田濡れ性に良い、かつ、めっき浴寿命
の長い電子部品用無電解銀めっき液が得られた。According to the present invention, an electroless silver plating solution for electronic parts having an excellent effect of preventing migration, good solder wettability, and a long plating bath life was obtained.
Claims (5)
剤と、ＰＨバッファー塩とからなることを特徴とする電
子部品用無電解銀めっき液。1. An electroless silver plating solution for electronic components, comprising a silver salt, a silver complexing agent, a fluorine-based surfactant, and a PH buffer salt.
合物である、請求項１に記載の無電解銀めっき液。2. The electroless silver plating solution according to claim 1, wherein the silver salt is silver nitrate and the silver complexing agent is a pyrrolidone compound.
ン化合物０．１〜２００ｇ／ｌ、フッ素系界面活性剤
０．０１〜１０ｇ／ｌ含有し、ＰＨバッファー塩として
無機酸または有機酸若しくは両方を含むことを特徴とす
る電子部品用無電解銀めっき液。3. The composition contains 0.05 to 30 g / l of silver ions, 0.1 to 200 g / l of a pyrrolidone compound, and 0.01 to 10 g / l of a fluorinated surfactant. An electroless silver plating solution for electronic parts, characterized by containing both.
−ピロリドン、および２−ピロリドン−５−カルボン酸
のうち少なくとも１種である請求項２または３に記載の
電子部品用無電解銀めっき液。4. The method of claim 1, wherein the pyrrolidone compound is 2-pyrrolidone, 3
The electroless silver plating solution for an electronic component according to claim 2 or 3, wherein the electroless silver plating solution is at least one of -pyrrolidone and 2-pyrrolidone-5-carboxylic acid.
キルスルホン酸塩、パーフルオロアルキルカルボン酸
塩、パーフルオロアルキルリン酸エステル、パーフルオ
ロアルキルアンモニウムヨウ化物、パーフルオロアルキ
ルアミンオキサイド、パーフルオロアルキルトリメチル
アンモニウム塩のうち少なくとも１種である請求項１ま
たは３に記載の電子部品用無電解銀めっき液。5. A fluorosurfactant comprising a perfluoroalkyl sulfonate, a perfluoroalkyl carboxylate, a perfluoroalkyl phosphate, a perfluoroalkylammonium iodide, a perfluoroalkylamine oxide, a perfluoroalkyltrimethyl. 4. The electroless silver plating solution for electronic components according to claim 1, wherein the electroless silver plating solution is at least one of ammonium salts.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10328373A JP2000144440A (en) | 1998-11-18 | 1998-11-18 | Electroless silver plating solution for electronic parts |
| PCT/JP1999/006453 WO2000029638A1 (en) | 1998-11-18 | 1999-11-18 | Electroless silver plating solution for electronic parts |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10328373A JP2000144440A (en) | 1998-11-18 | 1998-11-18 | Electroless silver plating solution for electronic parts |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JP2000144440A true JP2000144440A (en) | 2000-05-26 |
Family
ID=18209531
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP10328373A Pending JP2000144440A (en) | 1998-11-18 | 1998-11-18 | Electroless silver plating solution for electronic parts |
Country Status (2)
| Country | Link |
|---|---|
| JP (1) | JP2000144440A (en) |
| WO (1) | WO2000029638A1 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013010858A1 (en) * | 2011-07-18 | 2013-01-24 | Technische Universität Dresden | Method for producing thin electrically conductive layers of silver, a silver layer, a silver complex, the solution of said silver complex, and the use of the silver complex in a solution |
| CN110484901A (en) * | 2018-05-15 | 2019-11-22 | 上海新阳半导体材料股份有限公司 | A kind of chemical plating liquid, preparation method and application |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB9425030D0 (en) * | 1994-12-09 | 1995-02-08 | Alpha Metals Ltd | Silver plating |
| JP3532046B2 (en) * | 1996-10-25 | 2004-05-31 | 株式会社大和化成研究所 | Non-cyanated silver plating bath |
-
1998
- 1998-11-18 JP JP10328373A patent/JP2000144440A/en active Pending
-
1999
- 1999-11-18 WO PCT/JP1999/006453 patent/WO2000029638A1/en active Application Filing
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013010858A1 (en) * | 2011-07-18 | 2013-01-24 | Technische Universität Dresden | Method for producing thin electrically conductive layers of silver, a silver layer, a silver complex, the solution of said silver complex, and the use of the silver complex in a solution |
| CN110484901A (en) * | 2018-05-15 | 2019-11-22 | 上海新阳半导体材料股份有限公司 | A kind of chemical plating liquid, preparation method and application |
| CN110484901B (en) * | 2018-05-15 | 2022-11-01 | 上海新阳半导体材料股份有限公司 | Chemical silver plating solution, preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| WO2000029638A1 (en) | 2000-05-25 |
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