JP3022978B2 - Electroless plating method - Google Patents
Electroless plating methodInfo
- Publication number
- JP3022978B2 JP3022978B2 JP2121315A JP12131590A JP3022978B2 JP 3022978 B2 JP3022978 B2 JP 3022978B2 JP 2121315 A JP2121315 A JP 2121315A JP 12131590 A JP12131590 A JP 12131590A JP 3022978 B2 JP3022978 B2 JP 3022978B2
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- Prior art keywords
- plating
- plated
- bath
- film
- temperature
- Prior art date
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Description
【発明の詳細な説明】 ［産業上の利用分野］ 本発明は無電解メッキ方法、特に高いメッキ浴温によ
ってメッキ被膜を形成する無電解メッキ方法に関するも
のである。Description: TECHNICAL FIELD The present invention relates to an electroless plating method, and more particularly to an electroless plating method for forming a plating film at a high plating bath temperature.
［従来の技術］ 無電解メッキはメッキ液中の金属イオンを還元して金
属被膜を形成する化学メッキとして知られ、電流を通し
て電解イオンを析出する電気メッキと対比されるが、最
も大きな特長としてどのような形の物にも均一な厚さに
メッキできる点が指摘されている。その他の技術的な優
劣比較は、本発明の要旨とは直接関係しないのでここで
は省略する。なお、無電解メッキにおいては還元剤を含
むメッキ液を容器に入れて、例えばNi（ニッケル）メッ
キの場合のように、メッキ液を所定の温度に昇温してメ
ッキ準備の完了した状態をメッキ浴又は単に浴と称し、
この状態のメッキ浴の温度を浴温と呼んでいる。したが
って、以下の説明においても、適宜メッキ浴（又は浴）
及び浴温の用語を使用する。[Prior art] Electroless plating is known as chemical plating, in which metal ions in a plating solution are reduced to form a metal film, and is compared with electroplating, which deposits electrolytic ions through an electric current. It is pointed out that such a shape can be plated to a uniform thickness. Other technical superiority comparisons are not directly related to the gist of the present invention, and are therefore omitted here. In the case of electroless plating, a plating solution containing a reducing agent is placed in a container, and the plating solution is heated to a predetermined temperature, for example, as in the case of Ni (nickel) plating, and the plating preparation is completed. Called bath or simply bath,
The temperature of the plating bath in this state is called a bath temperature. Therefore, in the following description, a plating bath (or bath) is appropriately used.
And the terms bath temperature.
第２図は従来の無電解メッキ方法の手順を示すフロー
チャート図である。図に示したように、従来の無電解メ
ッキでメッキ薄膜を得るには被メッキ物の表面を、トリ
クレン、クロロセン等の有機溶剤で脱脂を行った後、純
水による洗浄、前処理、水洗を行う。その後即時にまた
は、乾燥して保管後にメッキ浴に投入（浸浴）し必要な
膜厚、もしくは被膜抵抗値が得られる時間メッキを行っ
ていた。この場合、メッキ液の温度を70〜90℃の高温で
使用するメッキ、たとえばNiメッキなどでは、これより
低い温度ではメッキ液に含まれる還元剤が活性化しない
ため、メッキ反応は起きない。このようなメッキ方法に
おいて、均一な、被膜を得るには、浴温を一定に保つこ
と、浴を良くかくはんすること、被メッキ物を回転させ
ることなどの対策が行われていた。FIG. 2 is a flowchart showing the procedure of a conventional electroless plating method. As shown in the figure, to obtain a plating thin film by conventional electroless plating, the surface of the object to be plated is degreased with an organic solvent such as trichlene or chlorocene, and then washed with pure water, pre-treated, and washed with water. Do. Immediately thereafter, or after drying and storing, plating (immersion bath) was performed, and plating was performed for a time to obtain a required film thickness or film resistance value. In this case, in a plating using a plating solution at a high temperature of 70 to 90 ° C., for example, Ni plating, a reducing agent contained in the plating solution is not activated at a temperature lower than this, so that a plating reaction does not occur. In such a plating method, in order to obtain a uniform coating film, measures such as keeping the bath temperature constant, stirring the bath well, and rotating the object to be plated have been taken.
［発明が解決しようとする課題］ 上記のような従来の無電解メッキ方法では、メッキ時
間が短ければ短いほどメッキ被膜抵抗値のばらつきが大
きくなり、均一な薄膜を得るのは非常に困難であった。
その原因としては被メッキ物をメッキ液中に投入してか
ら、実際に被メッキ物表面でメッキ反応が起こるまでの
間に時間のずれが生じることが挙げられ、それは被メッ
キ物の表面温度に起因している。常温の被メッキ物がメ
ッキ液中に投入（浸浴）されると、周囲の高温のメッキ
液に加熱されることになる。そしてメッキ反応が起こる
温度になった部位から優先してメッキ反応が進むことに
なり、その反応は一様ではない。結果としてメッキ被膜
にばらつきが生じることとなる。この点は、浴温を一定
にしても、液のかくはんを行っても、被メッキ物を回転
させても解決できない問題であった。[Problems to be Solved by the Invention] In the conventional electroless plating method as described above, the shorter the plating time, the greater the variation in the plating film resistance value, and it is very difficult to obtain a uniform thin film. Was.
The cause is that there is a time lag between the time when the object to be plated is put into the plating solution and the time when the plating reaction actually occurs on the surface of the object to be plated. Is due. When an object to be plated at normal temperature is put into a plating solution (immersion bath), it is heated by a surrounding high-temperature plating solution. Then, the plating reaction will proceed preferentially from the site where the temperature at which the plating reaction occurs, and the reaction is not uniform. As a result, variations occur in the plating film. This point is a problem that cannot be solved even if the bath temperature is kept constant, the solution is stirred, or the object to be plated is rotated.
本発明は上記のような課題を解決するためになされた
もので、メッキ反応が起こるまでの時間を一定にする工
程を挿入してメッキむら（ばらつき）のないメッキを行
う無電解メッキ方法を提供することを目的とするもので
ある。The present invention has been made in order to solve the above-mentioned problems, and provides an electroless plating method for performing plating without uneven plating (variation) by inserting a step of keeping a time until a plating reaction occurs. It is intended to do so.
［課題を解決するための手段］ 本発明に係る無電解メッキ方法は、メッキ前処理の完
了した被メッキ物を、メッキ直前にメッキ液の浴温以上
の温度に昇温した水に浸漬し、この被メッキ物をメッキ
液の浴温以上の温度とした後、引き続いて、直ちに、浴
温のメッキ液（なお、以下の説明において、浴温のメッ
キ液を、メッキ浴ともいう）に浸浴してメッキするもの
である。[Means for Solving the Problems] In the electroless plating method according to the present invention, the object to be plated, which has been subjected to the plating pretreatment, is immersed in water heated to a temperature equal to or higher than the bath temperature of the plating solution immediately before plating, Immediately after the object to be plated is heated to a temperature equal to or higher than the bath temperature of the plating solution, it is immediately immersed in a bath temperature plating solution (the bath temperature plating solution is also referred to as a plating bath in the following description). To be plated.
［作用］ 本発明においては、メッキ前処理の完了した被メッキ
物を、メッキ直前にメッキ液の浴温以上の温度に昇温し
た水に浸漬し、この被メッキ物をメッキ液の浴温以上の
温度とした後、引き続いて、これを取り出して、直ち
に、浴温のメッキ液に浸浴してメッキを行うようにした
ので、被メッキ物とその表面温度はメッキ浴温以上のも
のとなるため、メッキ反応が起こるまでの時間を一定に
してメッキが行われる。つまり、メッキ反応の開始を早
め、かつすべてのメッキ面に対して一様にすることがで
きるのでメッキ反応が均一にかつスムーズに進行する。
これにより、すべてのメッキ面にメッキむらがなく、均
一な厚みのメッキ皮膜を形成できる。[Operation] In the present invention, the object to be plated, which has been subjected to the plating pretreatment, is immersed in water heated to a temperature equal to or higher than the bath temperature of the plating solution immediately before plating, and the object to be plated is heated to a temperature equal to or higher than the bath temperature of the plating solution. Then, after taking this out, it was immediately immersed in a plating solution at a bath temperature to perform plating, so that the object to be plated and its surface temperature were higher than the plating bath temperature. Therefore, plating is performed with a constant time until a plating reaction occurs. That is, since the start of the plating reaction can be hastened and the plating reaction can be made uniform on all the plating surfaces, the plating reaction proceeds uniformly and smoothly.
This makes it possible to form a plating film having a uniform thickness without plating unevenness on all plating surfaces.
［実施例］ 実施例1; 第１図は本発明による無電解メッキ方法の手順の一実
施例を示すフローチャート図である。まず、被メッキ物
の表面をトリクレン、クロロセン等の有機溶剤で脱脂を
行ったのち、純水による洗浄（水洗）、前処理、水洗を
第２図の従来プロセスと同様に実施する。その後即時に
又は乾燥保管後に、まずメッキ浴温以上の所定温度に昇
温した水（温水）に浸漬させる（温水浸漬）。この浸漬
によって被メッキ物がメッキ浴温以上の温度となった時
点で被メッキ物を水から出し直ちにメッキ浴に浸浴して
メッキを行う。メッキは従来例と同様に時間メッキであ
る。[Example] Example 1; Fig. 1 is a flowchart showing an example of a procedure of an electroless plating method according to the present invention. First, after the surface of the object to be plated is degreased with an organic solvent such as trichlene or chlorocene, washing with pure water (washing with water), pretreatment, and washing with water are performed in the same manner as the conventional process of FIG. Immediately thereafter or after drying and storage, first, it is immersed in water (warm water) heated to a predetermined temperature higher than the plating bath temperature (warm water immersion). When the object to be plated reaches a temperature equal to or higher than the plating bath temperature by this immersion, the object to be plated is taken out of the water and immediately immersed in the plating bath to perform plating. The plating is time plating as in the conventional example.
上記の手順において、例えば被メッキ物がCu（銅）な
どの金属で、Niメッキの場合について説明する。メッキ
液はNiSO4を主成分とし、これに還元剤として次亜リン
酸ソーダ（NaH2PO2）の所定量を加えた組成からなる溶
液である。メッキ浴は酸性浴の場合、pH5.0、温度（浴
温）90゜で使用した。したがって本実施例のメッキ方法
では被メッキ物をメッキ直前に90゜〜100℃の温水に浸
漬したのち、上記の90℃のメッキ浴に浸浴することによ
りメッキが進行する。メッキ被膜は浸浴時間とともに厚
く形成される。そして、このように還元剤としてNaH2PO
2を用いた場合に得られるNi被膜は厳密には耐食性が優
れ、硬さの高いNi−Ｐ合金被膜である。In the above procedure, a case where the object to be plated is a metal such as Cu (copper) and Ni plating is performed will be described. The plating solution is a solution composed of NiSO 4 as a main component and a predetermined amount of sodium hypophosphite (NaH 2 PO 2 ) added thereto as a reducing agent. In the case of an acidic bath, the plating bath was used at pH 5.0 and at a temperature (bath temperature) of 90 °. Therefore, in the plating method of the present embodiment, the plating proceeds by immersing the object to be plated in warm water of 90 ° C. to 100 ° C. immediately before plating, and then immersing it in the plating bath of 90 ° C. The plating film is formed thicker with the immersion time. And thus, NaH 2 PO as a reducing agent
Excellent corrosion resistance Ni film strictly obtained when using a 2, a high hardness Ni-P alloy coating.
以上のように、メッキ直前に被メッキ物を温水中に浸
漬し、被メッキ物とその表面の温度をメッキ浴温以上に
暖めておくことによって、メッキ反応の開始を一様と
し、それによってメッキ被膜の厚さむら、すなわちばら
つきを効果的に抑えることができる。なお、実施例にお
いては、被メッキ物を金属とし、酸性浴におけるNiメッ
キの場合について説明したが、これに限定されるもので
はなく、この発明によるメッキ方法は例えば塩基性浴や
被メッキ物がプラスチック等のNiメッキ以外の金属メッ
キの場合にも十分適用可能である。As described above, the object to be plated is immersed in warm water immediately before plating, and the temperature of the object to be plated and the surface thereof are warmed to the plating bath temperature or higher, so that the start of the plating reaction is uniform, and thereby the plating is performed. The thickness unevenness of the film, that is, the variation can be effectively suppressed. In the examples, the object to be plated was a metal, and the case of Ni plating in an acidic bath was described.However, the present invention is not limited to this, and the plating method according to the present invention may be, for example, a basic bath or an object to be plated. The present invention is sufficiently applicable to metal plating other than Ni plating such as plastic.
実施例2; 本実施例では本発明による無電解メッキ方法で、一例
として絶縁物表面上にNiメッキを行い、併せて得られた
メッキ被膜の評価を行った結果について説明する。Example 2 In this example, a description will be given of a result of performing Ni plating on an insulating material surface by an electroless plating method according to the present invention and evaluating a plating film obtained as an example.
絶縁物が例えばプラスチックである場合は、周知の技
術ではあるが、金属の被メッキ物に対して行う通常の前
処理（第１図参照）とは異る前処理を行う必要がある。
第３図はプラスチックに無電解Niメッキを行う場合に実
施される前処理工程のサブ工程を示すフローチャートで
ある。図示のように、前処理は感受化−水洗−活性化−
水洗の一連のサブ工程を単位とするＡ工程を３回繰り返
して行うことにより前処理終了となる。すなわち、初め
の感受化（センシタイジングとも呼ばれる触媒付与）は
プラスチックを1cc/の塩酸水溶液１中にSnCl21gを
含む溶液中に１分間浸漬する。ついで１分の水洗を行
い、さらに0.1cc/塩酸水溶液１中にPdCl20.1gを含
む溶液中に１分間浸漬して活性化したのち、１分の水洗
を行うことにより１つのＡ工程を終了する。このＡ工程
を３回繰り返すことにより、表面にPd（パラジウム）を
膜状に析出させて前処理が終了するようにしている。When the insulating material is, for example, plastic, it is a well-known technique, but it is necessary to perform a pre-treatment different from a normal pre-treatment (see FIG. 1) performed on a metal object to be plated.
FIG. 3 is a flowchart showing sub-steps of a pretreatment step performed when performing electroless Ni plating on plastic. As shown in the figure, the pretreatment is sensitization-washing-activation-
The pretreatment is completed by repeating Step A, which is a series of sub-steps of washing with water, three times. That is, the first sensitization (providing a catalyst also called sensitizing) involves immersing the plastic in a solution containing 1 g of SnCl 2 in 1 cc / aqueous hydrochloric acid solution 1 for 1 minute. Then, it is washed for 1 minute, and further activated by immersing it in a solution containing 0.1 g of PdCl 2 in 0.1 cc / hydrochloric acid aqueous solution 1 for 1 minute, and then washing for 1 minute to complete one step A. I do. By repeating step A three times, Pd (palladium) is deposited on the surface in the form of a film to complete the pretreatment.
このようにして形成したPd下地を有する被メッキ物を
75゜〜90℃のメッキ液に浸浴してNiの無電解メッキを行
い、表面に形成したPd下地上にNiPのメッキ被膜が形成
される。使用メッキ液はニムエデンHDX（商標：上村工
業社）と称する無電解NiPメッキ液である。この場合、
本発明によるメッキ方法では実施例１の場合と同様に前
処理の終了したプラスチックを浸浴前にメッキ浴温以上
に昇温した水に浸漬し、これを水から取り出して浸浴し
メッキを行うことによりばらつきの小さい強固なメッキ
被膜が得られる。An object to be plated having a Pd underlayer formed in this manner is
Electroless plating of Ni is performed by bathing in a plating solution at 75 ° to 90 ° C., and a NiP plating film is formed on the Pd base formed on the surface. The plating solution used is an electroless NiP plating solution called Nime Eden HDX (trademark: Uemura Kogyo KK). in this case,
In the plating method according to the present invention, as in the case of Example 1, the pretreated plastic is immersed in water heated to a temperature higher than the plating bath temperature before immersion, taken out of the water, and immersed in the bath for plating. As a result, a strong plating film with small variations can be obtained.
第４図はプラスチック上のメッキ被膜の評価として膜
質のばらつきについて検討した確認実験の結果を示す線
図である。図において、横軸はメッキ（浸浴）時間、縦
軸は得られたNi被膜のシート抵抗（Ω／□）の｜最大値
−最小値｜をばらつきとして示している。この場合、被
メッキ物（プラスチック）は同一形状のものを対象とし
従来のメッキ方法（データ●印）と本発明のメッキ方法
（データ■印）についての実験結果を示した。この場
合、メッキ被膜のシート抵抗のばらつきは直接メッキ被
膜の厚さのばらつきに対応するものである。メッキ被膜
の評価方法としては、従来方式（第２図）による常温乾
燥状態の被メッキ物と本発明方式（第１図・第３図）に
よる被メッキ物をメッキ浴温以上に加熱したものとをそ
れぞれ一定時間浸浴してメッキを行い、得られた被膜の
シート抵抗値のばらつきを求めて比較を行った。FIG. 4 is a diagram showing the results of a confirmation experiment in which a variation in film quality was examined as an evaluation of a plating film on plastic. In the figure, the horizontal axis represents the plating (immersion bath) time, and the vertical axis represents the | maximum value−minimum value | of the sheet resistance (Ω / □) of the obtained Ni film as a variation. In this case, the object to be plated (plastic) has the same shape, and the experimental results of the conventional plating method (data mark) and the plating method of the present invention (data mark) are shown. In this case, the variation in the sheet resistance of the plating film directly corresponds to the variation in the thickness of the plating film. The method for evaluating the plating film includes a method in which the object to be plated in a normal temperature dried state by the conventional method (FIG. 2) and a method in which the object to be plated by the method of the present invention (FIGS. 1 and 3) are heated to a plating bath temperature or higher. Were subjected to plating for a certain period of time, and the sheet resistance of the obtained coating film was measured for variation.
第４図の実験結果から、本発明による無電解メッキ方
法の方が従来方法よりメッキ被膜のばらつきが小さいこ
とがわかる。特に、メッキ時間が２分以内のメッキ薄膜
形成に対してこの傾向は著るしく、本発明による方法の
効果を裏付けするものということができる。From the experimental results shown in FIG. 4, it can be understood that the electroless plating method according to the present invention has a smaller variation in plating film than the conventional method. In particular, this tendency is remarkable for the formation of a plating thin film having a plating time of 2 minutes or less, and can be said to support the effect of the method according to the present invention.
［発明の効果］ 以上のように、本発明によれば、メッキ前処理の完了
した被メッキ物を、メッキ直前にメッキ液の浴温以上の
温度に昇温した水に浸漬し、この被メッキ物をメッキ液
の浴温以上の温度とした後、引き続いて、直ちに、メッ
キ浴に浸浴してメッキするようにしたので、被メッキ物
の全てのメッキ面において、メッキ反応が一様に開始さ
れ、かつメッキ浴に浸浴してすぐに反応が開始されるた
め、メッキ面にばらつきなく均一な厚みのメッキ皮膜が
形成でき、またバラツキのない皮膜抵抗値のメッキ皮膜
を形成でき、しかもメッキ皮膜をメッキ時間で正確に制
御して精度良く形成することができるという効果を有す
る。[Effects of the Invention] As described above, according to the present invention, the object to be plated, which has been subjected to the plating pretreatment, is immersed in water heated to a temperature equal to or higher than the bath temperature of the plating solution immediately before plating. After the product was heated to a temperature equal to or higher than the bath temperature of the plating solution, it was immediately immersed in the plating bath for plating, so that the plating reaction started uniformly on all the plating surfaces of the object to be plated. The reaction starts immediately after being immersed in the plating bath, so that a plating film having a uniform thickness can be formed on the plating surface without variation, and a plating film having a uniform film resistance can be formed. This has the effect that the film can be accurately formed by accurately controlling the film by the plating time.
第１図は本発明の無電解メッキ方法の手順の一実施例を
示すフローチャート図、第２図は従来の無電解メッキ方
法の手順を示すフローチャート図、第３図はプラスチッ
クに無電解メッキを行う場合の前処理工程のサブ工程を
示すフローチャート図、第４図はメッキ被膜の評価をメ
ッキ時間に対するメッキ膜質のばらつきについて比較実
験した結果を示す線図である。FIG. 1 is a flowchart showing one embodiment of the procedure of the electroless plating method of the present invention, FIG. 2 is a flowchart showing the procedure of a conventional electroless plating method, and FIG. FIG. 4 is a flowchart showing the sub-steps of the pretreatment step in the case, and FIG. 4 is a diagram showing the results of a comparison experiment of the evaluation of the plating film with respect to the variation in the quality of the plating film with respect to the plating time.
───────────────────────────────────────────────────── フロントページの続き (58)調査した分野(Int.Cl.7，ＤＢ名) C23C 18/18 ──────────────────────────────────────────────────続 き Continued on front page (58) Field surveyed (Int.Cl. 7 , DB name) C23C 18/18
Claims (1)
ッキ直前にメッキ液の浴温以上の温度に昇温した水に浸
漬し、当該被メッキ物をメッキ液の浴温以上の温度とし
た後、引き続いて、直ちに、前記メッキ液に浸浴してメ
ッキすることを特徴とする無電解メッキ方法。An object to be plated, which has been subjected to a plating pretreatment, is immersed in water heated to a temperature equal to or higher than the bath temperature of the plating solution immediately before plating, and the object to be plated is heated to a temperature equal to or higher than the bath temperature of the plating solution. And thereafter immediately immersing in the plating solution for plating.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2121315A JP3022978B2 (en) | 1990-05-14 | 1990-05-14 | Electroless plating method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2121315A JP3022978B2 (en) | 1990-05-14 | 1990-05-14 | Electroless plating method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0421786A JPH0421786A (en) | 1992-01-24 |
| JP3022978B2 true JP3022978B2 (en) | 2000-03-21 |
Family
ID=14808202
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2121315A Expired - Fee Related JP3022978B2 (en) | 1990-05-14 | 1990-05-14 | Electroless plating method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3022978B2 (en) |
-
1990
- 1990-05-14 JP JP2121315A patent/JP3022978B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0421786A (en) | 1992-01-24 |
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