JPS596365A - Electroless gold plating method - Google Patents
Electroless gold plating methodInfo
- Publication number
- JPS596365A JPS596365A JP11167582A JP11167582A JPS596365A JP S596365 A JPS596365 A JP S596365A JP 11167582 A JP11167582 A JP 11167582A JP 11167582 A JP11167582 A JP 11167582A JP S596365 A JPS596365 A JP S596365A
- Authority
- JP
- Japan
- Prior art keywords
- gold
- plating
- gold plating
- electroless
- electroless gold
- 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
- C23C18/44—Coating with noble metals using reducing agents
Abstract
Description
【発明の詳細な説明】
〔発明の技術分野〕
本発明は無電解金メツキ方法に係シ、特に高純度の金メ
ッキを被メツキ部材上に行々うことか可能な無電解金メ
ツキ方法に関するものである。[Detailed Description of the Invention] [Technical Field of the Invention] The present invention relates to an electroless gold plating method, and more particularly to an electroless gold plating method that allows high-purity gold plating to be performed on a member to be plated. It is.
例えばIC単体、複数のICに使用される外囲器、L8
I外囲器などの半導体用の外囲器、表面波素子の外囲器
などの所謂電子部品外囲器を製造する場合、セラミック
スやアルミナなどからなる絶縁基板上にタングステンや
モリブデンおよびその合金の金属粉末をペースト状とし
印刷技術を利用して一部に箪布し、絶縁基板と共にこれ
らを加熱焼結して導体部を形成し、この導体部上にメッ
キによシ金層を被着形成して配線や金属ふた部との接続
に使用する方法が知られている。この場合、導体部上に
は通常の電解メッキや無電解メッキで得られるニッケル
メッキ、硼素を含むニッケルメッキなどを行なったのち
、水素炉処理した部材や、シャン金カリ111/l水酸
化ナトリウム1001/lクエン酸ナトリウム100
y/lの液で95℃約5分置換析出した無電解金メッキ
した部材、通常の電解金メッキ液で約0.1μフラツシ
ユメツキした部材上にシアン金カリウム211/l 、
塩化アンモニウム75g/l 、シュウ酸ナトリウム5
0 g/l 、次亜リン酸ナトリウム1ott/lかも
なるpH7〜7.5のメッキ液を使用し90〜95℃で
無電解金メツキ被膜を形成したり、塩化金381//l
、炭酸ナトリウム101/’。For example, a single IC, an envelope used for multiple ICs, L8
When manufacturing so-called electronic component envelopes such as semiconductor envelopes such as I envelopes and envelopes for surface wave devices, tungsten, molybdenum, and their alloys are placed on an insulating substrate made of ceramics, alumina, etc. Metal powder is made into a paste and applied to a portion using printing technology, and then heated and sintered together with an insulating substrate to form a conductor part, and a gold layer is deposited on this conductor part by plating. A known method is to use it for wiring and connection with a metal lid. In this case, after performing nickel plating obtained by ordinary electrolytic plating or electroless plating, nickel plating containing boron, etc. on the conductor part, the parts are treated in a hydrogen furnace, or the parts are treated with 111/l sodium hydroxide 1001/l sodium hydroxide. /l sodium citrate 100
y/l solution for about 5 minutes at 95°C, and on a member that had been flushed by about 0.1 μm with a normal electrolytic gold plating solution, 211/l cyanogen-gold potassium was deposited.
Ammonium chloride 75g/l, sodium oxalate 5
0 g/l and sodium hypophosphite 1 ott/l. An electroless gold plating film is formed at 90-95°C using a plating solution with a pH of 7-7.5, or gold chloride 381//l.
, sodium carbonate 101/'.
37チホルマリン65dllからなるp)(7〜7.5
のメッキ液を使用し、10〜20℃で無電解金メツキ被
膜を形成する々ど多種の無電解金メツキ被膜の形成方法
が行なわれている。p) consisting of 37 formalin and 65 dll (7-7.5
Various methods of forming an electroless gold plating film have been carried out, in which the electroless gold plating film is formed using a plating solution of 10 to 20°C.
然るにこれらのメッキ液は液寿命が短かい、全濃度が高
くないとメッキ速度が遅い、通常90℃以上でメッキ温
度が高い、メッキ膜の純度等の問題があり0.1〜0.
5μと比較的薄い金メッキのみに使用されているのが現
状であシ、このように薄い金メッキ層では電子部品との
接続に使用するボンディング線のボンディング時やリー
ドビンの銀ロウまたは銀−銅ロウ付時にその接続が不充
分であるし、また下地との密着性も悪く更に外観も良く
ない問題点があった。However, these plating solutions have problems such as short service life, slow plating speed unless the total concentration is high, high plating temperature (usually 90°C or higher), and purity of the plating film.
Currently, it is only used for relatively thin gold plating of 5μ, and such a thin gold plating layer is used for bonding of bonding wires used for connection with electronic components, and for silver soldering or silver-copper soldering of lead bins. There are problems in that the connection is sometimes insufficient, the adhesion to the substrate is poor, and the appearance is not good.
本・発明は前記従来の諸問題に鑑みなされたものでア)
、ボンディング特性やリードピンのロウ付特性もよく更
に良好な外観を得ることが可能な無電解金メツキ方法を
提供することを目的としている。This invention was made in view of the above-mentioned conventional problems.
The object of the present invention is to provide an electroless gold plating method that has good bonding properties and brazing properties of lead pins, and can obtain a better appearance.
即ち、本発明は電解メッキや無電解メッキにて得られる
ニッケルメッキ、硼素を含むニッケルメッキを行なった
のち熱処理した部材や鉄やニッケル及びそれらの合金に
金のフラッシュメッキを行なった部材の表面に高純度の
金を無電解金メッキによシ被着形成するに当り、無電解
メッキに少くともシャン金カリウムからなる金化合物と
、クエン酸及びクエン酸ナトリウム、酒石酸、等の有機
酸やその塩類からなる錯化合物と抱水ヒドラジンからな
る還元剤と、塩化アンモン等からなるpH4乃至7の金
メッキ液を使用することを特徴としている。That is, the present invention applies to the surfaces of nickel plating obtained by electrolytic plating or electroless plating, members heat-treated after nickel plating containing boron, and members flash-plated with gold to iron, nickel, or their alloys. When depositing high-purity gold by electroless gold plating, electroless plating is performed using at least a gold compound consisting of gold potassium, and organic acids such as citric acid, sodium citrate, tartaric acid, and their salts. It is characterized by the use of a complex compound consisting of the following, a reducing agent consisting of hydrazine hydrate, and a gold plating solution having a pH of 4 to 7 consisting of ammonium chloride or the like.
次に本発明の無電解金メツキ方法の第1の実施例を説明
する。Next, a first embodiment of the electroless gold plating method of the present invention will be described.
即ち、先ず未焼結のアルミナ基板を用意し、このアルミ
ナ基板の所望部にタングステン粉末またはモリブデン粉
末もしくはタングステンまたはモリブデンを主成分とす
るペーストでスクリーン印刷後、1500℃で焼結して
厚さ約20μの導体部を形成し、50%塩酸501/l
フツ化カリ水溶液を用いて常温で5分浸せき後、水洗す
る。次にこの導体部の表面を活性化したのち、硼素を含
むニッケルメッキ液を使用し、硼素を含むニッケルメッ
キ層を約5μ析出する。次に水洗、乾燥後、水素中で加
熱処理し、この硼素を含むニッケルメッキ層を再結晶化
し、50%塩酸、5011/17ツ化カリ水溶液で浸せ
き後水洗する。That is, first, an unsintered alumina substrate is prepared, and tungsten powder, molybdenum powder, or a paste containing tungsten or molybdenum as a main component is screen-printed on desired parts of the alumina substrate, and then sintered at 1500°C to a thickness of approximately Form a conductor part of 20μ, and add 50% hydrochloric acid 501/l.
After soaking in a potassium fluoride aqueous solution for 5 minutes at room temperature, wash with water. Next, after activating the surface of this conductor part, a nickel plating layer containing boron is deposited using a nickel plating solution containing boron of about 5 μm. Next, after washing with water and drying, heat treatment is performed in hydrogen to recrystallize the nickel plating layer containing boron, immersed in 50% hydrochloric acid and 5011/17 potassium tsulfide aqueous solution, and then washed with water.
次にシアン金カリウム29/l 、クエン酸ナトリウム
501/l、抱水ヒドラジン20m/7、クエン酸や水
酸化ナトリウムにてpH6〜7にした無電解金メッキ液
を45〜50℃でゆるやか々攪拌を行ないながら所望厚
さの無電解金メッキ層を析出させる。Next, an electroless gold plating solution adjusted to pH 6-7 with cyanogen gold potassium 29/l, sodium citrate 501/l, hydrazine hydrate 20 m/7, citric acid and sodium hydroxide was gently stirred at 45-50°C. As the process progresses, an electroless gold plating layer of desired thickness is deposited.
この無電解金メッキ層は0.5〜1,0μ膚位の速度で
厚くすることが可能である。本実施例では60分で約1
.0μ析出させた。This electroless gold plating layer can be thickened at a rate of 0.5 to 1.0 microns. In this example, approximately 1 in 60 minutes
.. 0μ was deposited.
次に水洗、乾燥を行なったのち200〜300℃で30
〜60分間加熱し金の再結晶化の熱処理を行ない電子部
品外囲器を完成する。Next, after washing with water and drying, 30 minutes at 200-300℃
The electronic component envelope is completed by heating for ~60 minutes to perform a heat treatment for gold recrystallization.
このよう処して形成した無電解金メッキ層は高純度であ
シ、金メッキ層を再結晶化することによシ良好寿外観と
密着性を有すると共に、例えば電子部品としてのボンデ
ィング特性、ロウ付特性も極めて優れていた。The electroless gold plating layer formed in this way has high purity, and by recrystallizing the gold plating layer, it has a good longevity appearance and adhesion, and also has good bonding and brazing characteristics for electronic components. It was extremely good.
次に本発明の無電解金メツキ方法の第2の実施例を説明
する。Next, a second embodiment of the electroless gold plating method of the present invention will be described.
即ち、硼素を含むニッケルメッキ層を形成する迄は前の
実施例と同様であるが無電解金メッキ液としてシアン゛
全カリウム2 g/l 、酒石酸5og/l、塩化アン
モン501//l 、抱水ヒドラジン30ynl/11
クエン酸ナトリウムまたは水酸化ナトリウムで一6〜7
Kl、たものを使用し45〜50℃でゆるやかな攪拌を
行ないながら無電解金メッキ層を形成す次に本発明の無
電解金メツキ方法の第3の実施例を説明する。That is, the steps up to the formation of the nickel plating layer containing boron were the same as in the previous example, but the electroless gold plating solution was cyanogen (total potassium 2 g/l, tartaric acid 5 og/l, ammonium chloride 501//l, hydrated). Hydrazine 30ynl/11
Sodium citrate or sodium hydroxide
Next, a third embodiment of the electroless gold plating method of the present invention will be described, in which an electroless gold plating layer is formed using Kl, and with gentle stirring at 45 to 50 DEG C.
即ち、本実施例では無電解金メッキ液としてシアン金カ
リウム51/l 、クエン酸751//It 、抱水ヒ
ドラジン401d/l 1クエン酸ナトリウムで…4〜
5にしたものを使用し、45〜50℃でゆるやか々攪拌
を行ないながら無電解金メッキ層を形成する。That is, in this example, the electroless gold plating solution was 51/l of cyanogen-gold potassium, 751//It of citric acid, 401 d/l of hydrazine hydrate, 1 sodium citrate...4~
5, and form an electroless gold plating layer at 45 to 50° C. with gentle stirring.
次に本発明の無電解金メツキ方法の第4の実施例を説明
する。Next, a fourth embodiment of the electroless gold plating method of the present invention will be described.
即ち、本実施例では無電解金メッキ液としてシアン金カ
リウム101/11酒石酸5oy/i10ツセル塩50
1/lで、pH5〜6にしたものを使用し、45〜50
℃でゆるやかな攪拌を行々いながら無電解金メッキ層を
形成する。That is, in this example, as the electroless gold plating solution, cyanogen gold potassium 101/11 tartaric acid 5 oy/i 10 Tuser salt 50
1/l, pH 5-6, 45-50
An electroless gold plating layer is formed with gentle stirring at ℃.
前記実施例の無電解金メッキ液はシアン金カリウムを補
充し、−を調整することで長期間使用でき、また、前記
実施例では硼素を含むニッケルメッキ層を下地にしたが
、これに限定されるものでけなく、ニッケルメッキを行
なったのち熱処理し丸部材や鉄、ニッケル及びそれらの
合金に金のフラッシュメッキを行なった部材でも同様で
あるし、また比較的低温でメッキ出来るため電子部品外
囲器以外にも種々応用出来ることも勿論である。The electroless gold plating solution of the above embodiment can be used for a long period of time by replenishing cyanogen-gold potassium and adjusting -.Also, in the above embodiment, a nickel plating layer containing boron was used as the base, but the present invention is not limited to this. This also applies to round parts that are nickel-plated and then heat-treated, as well as parts that are flash-plated with gold on iron, nickel, and their alloys.Also, since plating can be done at a relatively low temperature, it is possible to apply heat treatment to round parts and parts that are flash-plated with gold on iron, nickel, and their alloys. Of course, it can also be used for various purposes other than vessels.
上述のように本発明の無電解金メツキ方法によれば不純
物を含まず、良好な外観と、下地との密着力が優れた金
メツ午層が得られるのでその工業的価値は極めて大であ
る。As mentioned above, the electroless gold plating method of the present invention provides a gold plating layer that does not contain impurities, has a good appearance, and has excellent adhesion to the base, so its industrial value is extremely large. .
代理人 弁理士 井 上 −男Agent Patent Attorney Inoue - Male
Claims (2)
キを行なったのち熱処理した部材や金のフラッシュメッ
キを行なった部材の表面に高純度の金を無電解金メッキ
によシ被着形成するに当シ、前記無電解金メッキに少く
と亀シャン金カリウムからなる金化合物と、クエン酸及
びクエン酸ナトリウム、酒石酸、等の有機酸やその塩類
からなる錯化合物と、抱水ヒドラジンからなる還元剤と
、塩化アンモン、等からカるpH4乃至7の金メッキ液
を使用することを特徴とする無電解金メツキ方法。(1) When depositing high-purity gold by electroless gold plating on the surface of a member that has been heat-treated after nickel plating or nickel plating containing boron, or a member that has been flash plated with gold, the above-mentioned method is used. For electroless gold plating, a gold compound consisting of at least Kamechan gold potassium, a complex compound consisting of organic acids and their salts such as citric acid, sodium citrate and tartaric acid, a reducing agent consisting of hydrazine hydrate, ammonium chloride, An electroless gold plating method characterized by using a gold plating solution with a pH of 4 to 7.
ないながら無電解金メッキを行なうことを特徴とする特
許請求の範囲第1項記載の無電解金メツキ方法。(2) The electroless gold plating method according to claim 1, characterized in that electroless gold plating is performed while gently stirring the gold plating solution at a temperature of about 50°C.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP11167582A JPS596365A (en) | 1982-06-30 | 1982-06-30 | Electroless gold plating method |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP11167582A JPS596365A (en) | 1982-06-30 | 1982-06-30 | Electroless gold plating method |
Publications (1)
Publication Number | Publication Date |
---|---|
JPS596365A true JPS596365A (en) | 1984-01-13 |
Family
ID=14567332
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP11167582A Pending JPS596365A (en) | 1982-06-30 | 1982-06-30 | Electroless gold plating method |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPS596365A (en) |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS6452082A (en) * | 1987-06-22 | 1989-02-28 | Gen Electric | Electroless gold plating composition and method |
US5838069A (en) * | 1996-04-11 | 1998-11-17 | Ngk Spark Plug Co., Ltd. | Ceramic substrate having pads to be attached to terminal members with Pb-Sn solder and method of producing the same |
EP1026285A2 (en) * | 1999-01-27 | 2000-08-09 | Shipley Company LLC | Electroless gold plating solution and process |
US6486551B1 (en) | 1998-01-28 | 2002-11-26 | Ngk Spark Plug Co., Ltd. | Wired board and method of producing the same |
JP2008214703A (en) * | 2007-03-05 | 2008-09-18 | Rohm & Haas Electronic Materials Llc | Electroless gold plating liquid |
EP2143820A1 (en) | 2008-07-11 | 2010-01-13 | Rohm and Haas Electronic Materials LLC | An electroless gold plating solution |
-
1982
- 1982-06-30 JP JP11167582A patent/JPS596365A/en active Pending
Cited By (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS6452082A (en) * | 1987-06-22 | 1989-02-28 | Gen Electric | Electroless gold plating composition and method |
US5838069A (en) * | 1996-04-11 | 1998-11-17 | Ngk Spark Plug Co., Ltd. | Ceramic substrate having pads to be attached to terminal members with Pb-Sn solder and method of producing the same |
US6486551B1 (en) | 1998-01-28 | 2002-11-26 | Ngk Spark Plug Co., Ltd. | Wired board and method of producing the same |
EP1026285A2 (en) * | 1999-01-27 | 2000-08-09 | Shipley Company LLC | Electroless gold plating solution and process |
EP1026285A3 (en) * | 1999-01-27 | 2001-12-12 | Shipley Company LLC | Electroless gold plating solution and process |
US6383269B1 (en) * | 1999-01-27 | 2002-05-07 | Shipley Company, L.L.C. | Electroless gold plating solution and process |
KR100712261B1 (en) * | 1999-01-27 | 2007-04-26 | 롬 앤드 하스 일렉트로닉 머트어리얼즈, 엘.엘.씨 | Electroless gold plating solution and process |
JP2008214703A (en) * | 2007-03-05 | 2008-09-18 | Rohm & Haas Electronic Materials Llc | Electroless gold plating liquid |
EP2143820A1 (en) | 2008-07-11 | 2010-01-13 | Rohm and Haas Electronic Materials LLC | An electroless gold plating solution |
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