JP2002047573A - Pretreatment agent for silver plating and silver plating method - Google Patents
Pretreatment agent for silver plating and silver plating methodInfo
- Publication number
- JP2002047573A JP2002047573A JP2000232782A JP2000232782A JP2002047573A JP 2002047573 A JP2002047573 A JP 2002047573A JP 2000232782 A JP2000232782 A JP 2000232782A JP 2000232782 A JP2000232782 A JP 2000232782A JP 2002047573 A JP2002047573 A JP 2002047573A
- Authority
- JP
- Japan
- Prior art keywords
- silver plating
- pretreatment agent
- plating
- compound
- silane coupling
- 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
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、導電性の低い材料
や鏡面物や粉体などの表面に無電解めっきにより銀めっ
きするための銀めっき前処理剤、およびそれを用いた銀
めっき方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a silver plating pretreatment agent for electroless plating silver on the surface of a material having low conductivity, a mirror-like object or a powder, and a silver plating method using the same. .
【０００２】[0002]
【従来の技術】無電解金属めっき法は導電性のない下地
に金属被膜を形成する方法の一つであり、無電解めっき
の前処理としてパラジウムなどの貴金属を触媒としてあ
らかじめ下地に付着させておく活性化と呼ばれる方法が
一般的である。これまで、ＳｎＣｌ2の塩酸性水溶液で
処理した後ＰｄＣｌ2水溶液に浸漬処理してＰｄを吸着
させたり、ＳｎとＰｄを含んだコロイド溶液によりＰｄ
を表面に担持させる方法が使われてきた。最近、無電解
めっきの触媒であるＰｄなどの貴金属を表面に担持させ
る方法としてこれらの貴金属類と錯体を形成できる官能
基を有するシランカップリング剤を使った方法がいろい
ろと提案されている（特公昭５９−５２７０１、特開昭
６０−１８１２９４、特開昭６１−１９４１８３、特公
平３−４４１４９）。これらの中で、めっき触媒固定剤
とめっき触媒を別々に処理する方法、すなわちカップリ
ング剤を被めっき物に吸着させた後触媒となる貴金属イ
オンを担持させる場合、カップリング剤処理により被め
っき物の表面が改質されたり、貴金属イオンを効率良く
担持できなかったりするためか、被めっき物の素材によ
っては密着性良く均一にめっきすることが困難な場合が
あった。2. Description of the Related Art An electroless metal plating method is one of methods for forming a metal film on a non-conductive base, in which a noble metal such as palladium is previously attached to the base as a catalyst as a pretreatment for electroless plating. A method called activation is common. Previously, or to adsorb Pd was immersed in PdCl 2 solution was treated with hydrochloric acid aqueous solution of SnCl 2, the colloidal solution containing Sn and Pd Pd
Has been used on the surface. Recently, various methods using a silane coupling agent having a functional group capable of forming a complex with such a noble metal have been proposed as a method for supporting a noble metal such as Pd, which is a catalyst for electroless plating, on the surface (see, for example, Japanese Patent Application Laid-Open No. H11-157,055). JP-B-59-52701, JP-A-60-181294, JP-A-61-194183, JP-B-3-44149). Among them, a method of treating the plating catalyst fixing agent and the plating catalyst separately, that is, when supporting the noble metal ion serving as a catalyst after the coupling agent is adsorbed on the plating object, the treatment of the plating object by the coupling agent treatment. In some cases, it was difficult to perform uniform plating with good adhesion depending on the material of the object to be plated, probably because the surface of the substrate was modified or noble metal ions could not be carried efficiently.
【０００３】[0003]
【発明が解決しようとする課題】本発明はこうした実情
の下に従来無電解めっきが適用しにくかった素材に対し
ても、密着力よく無電解銀めっき皮膜を形成することが
できる無電気銀めっきのための前処理剤、およびそれを
用いた無電解銀めっき方法を提供することを目的とする
ものである。SUMMARY OF THE INVENTION Under the above circumstances, the present invention provides an electroless silver plating which can form an electroless silver plating film with good adhesion even to a material to which electroless plating is conventionally difficult to apply. And an electroless silver plating method using the same.
【０００４】[0004]
【課題を解決するための手段】本発明者は、鋭意検討し
た結果、スズ化合物と、含窒素複素環式アゾール化合物
とエポキシシランカップリング剤との反応生成物である
アゾール系シランカップリング剤からなる前処理剤によ
り被めっき物を前処理することが有効であることを知見
し、本発明に至った。Means for Solving the Problems As a result of intensive studies, the present inventor has found that an azole silane coupling agent which is a reaction product of a tin compound, a nitrogen-containing heterocyclic azole compound and an epoxy silane coupling agent is used. The present inventors have found that it is effective to pre-treat an object to be plated with a pre-treatment agent, which has led to the present invention.
【０００５】すなわち、本発明は、（１）金属捕捉能を
持つ置換基を有するシランカップリング剤とスズ化合物
を有効成分とする銀めっき前処理剤、（２）金属捕捉能
を持つ置換基を有するシランカップリング剤が含窒素複
素環式アゾール化合物とエポキシ基含有シラン化合物と
の反応生成物であるアゾール系シランカップリング剤で
あることを特徴とする前記（１）記載の銀めっき前処理
剤、（３）含窒素複素環式アゾール化合物がイミダゾー
ルである前記（２）記載の銀めっき前処理剤、（４）ス
ズ化合物が塩化第１スズである前記（１）、（２）又は
（３）記載の銀めっき前処理剤、（５）被めっき物を前
記（１）、（２）、（３）又は（４）記載の銀めっき前
処理剤で処理した後、無電解銀めっきすることを特徴と
する銀めっき方法、に関する。That is, the present invention provides (1) a silane coupling agent having a substituent having a metal-capturing ability and a pretreatment agent for silver plating containing a tin compound as an active ingredient; and (2) a substituent having a metal-capturing ability. The silver plating pretreatment agent according to the above (1), wherein the silane coupling agent is an azole silane coupling agent which is a reaction product of a nitrogen-containing heterocyclic azole compound and an epoxy group-containing silane compound. (3) the silver plating pretreatment agent according to (2), wherein the nitrogen-containing heterocyclic azole compound is imidazole; and (4) the (1), (2) or (3), wherein the tin compound is stannous chloride. And (5) treating an object to be plated with the silver plating pretreating agent according to (1), (2), (3) or (4), followed by electroless silver plating. Silver plating method characterized by the following On.
【０００６】本発明の前処理剤の一つの有効成分である
アゾール系シランカップリング剤は、含窒素複素環式ア
ゾール化合物とエポキシ基含有シラン化合物との反応生
成物である。前記含窒素複素環式アゾール化合物として
は、イミダゾール、オキサゾール、チアゾール、セレナ
ゾール、ピラゾール、イソオキサゾール、イソチアゾー
ル、トリアゾール、オキサジアゾール、チアジアゾー
ル、テトラゾール、オキサトリアゾール、チアトリアゾ
ール、ベンダゾール、インダゾール、ベンズイミダゾー
ル、ベンゾトリアゾール、インダゾールなどが挙げられ
る。これらに制限されるものではないが、イミダゾール
が特に好ましい。The azole silane coupling agent, one of the active ingredients of the pretreatment agent of the present invention, is a reaction product of a nitrogen-containing heterocyclic azole compound and an epoxy group-containing silane compound. Examples of the nitrogen-containing heterocyclic azole compound, imidazole, oxazole, thiazole, selenazole, pyrazole, isoxazole, isothiazole, triazole, oxadiazole, thiadiazole, tetrazole, oxatriazole, thiatriazole, bendazole, indazole, benzimidazole, Benzotriazole, indazole and the like can be mentioned. Although not limited thereto, imidazole is particularly preferred.
【０００７】また、このような含窒素複素環式アゾール
化合物と反応させるエポキシ基含有シラン化合物として
は、The epoxy group-containing silane compound to be reacted with such a nitrogen-containing heterocyclic azole compound includes:
【０００８】[0008]
【化１】 （式中、Ｒは水素又は炭素数が１〜３のアルキル基）で
示されるエポキシシランカップリング剤が好ましい。Embedded image (Wherein, R is hydrogen or an alkyl group having 1 to 3 carbon atoms).
【０００９】前記アゾール化合物と前記エポキシ基含有
シラン化合物との反応は、特開平６−２５６３５８号公
報に説示されている条件で行うことができる。例えば、
８０〜２００℃でアゾール化合物１モルに対して０．１
〜１０モルのエポキシ基含有シラン化合物を滴下して５
分〜２時間反応させる。その際、溶媒は特に不要である
が、クロロホルム、ジオキサンメタノール、エタノール
等の有機溶媒を用いてもよい。The reaction between the azole compound and the epoxy group-containing silane compound can be carried out under the conditions described in JP-A-6-256358. For example,
0.1 to 0.1 mol of the azole compound at 80 to 200 ° C.
5 to 10 moles of an epoxy group-containing silane compound are added dropwise.
Allow to react for minutes to 2 hours. At this time, a solvent is not particularly necessary, but an organic solvent such as chloroform, dioxanemethanol, and ethanol may be used.
【００１０】スズ化合物としては、塩化第１スズ、塩化
第２スズ、酸化スズ、しゅう酸スズ、硫酸スズ、臭化ス
ズ、酢酸スズなどを用いることができる。特に塩化第１
スズが望ましい。As the tin compound, stannous chloride, stannic chloride, tin oxide, tin oxalate, tin sulfate, tin bromide, tin acetate and the like can be used. Especially the first chloride
Tin is preferred.
【００１１】本発明の銀めっき前処理剤は、前記のアゾ
ール系シランカップリング剤と塩化第１スズとを有効成
分とするが、アゾール系シランカップリング剤とスズ化
合物との割合（モル比）は０．００１〜５０で用いら
れ、好ましくは０．１〜２０である。The silver plating pretreatment agent of the present invention contains the above azole-based silane coupling agent and stannous chloride as active ingredients, and the ratio (molar ratio) of the azole-based silane coupling agent to the tin compound is used. Is used in the range of 0.001 to 50, preferably 0.1 to 20.
【００１２】本発明の銀めっき前処理剤は、水溶液の形
態で使用するのが好ましく、溶液中のアゾール系シラン
カップリング剤の濃度は、０．００１〜１０重量％が使
いやすい。０．００１重量％未満の場合、被めっき物の
表面に付着する量が低くなりめっきが均一にされない。The pretreatment agent for silver plating of the present invention is preferably used in the form of an aqueous solution, and the concentration of the azole silane coupling agent in the solution is preferably 0.001 to 10% by weight. If the amount is less than 0.001% by weight, the amount of adhesion to the surface of the object to be plated is low, and the plating is not uniform.
【００１３】また、１０重量％を超えると付着量が多す
ぎて乾燥しにくかったり、被めっき物が粉末の場合、凝
集を起こしやすくなる。On the other hand, if the content exceeds 10% by weight, the amount of adhesion is too large to be dried easily, and when the object to be plated is a powder, aggregation tends to occur.
【００１４】本発明の前処理剤の作用について述べる
と、上記のようにアゾール系シランカップリング剤成分
が被めっき物の表面に付着し、その付着したアゾール系
シランカップリング剤に塩化第１スズが担持されてこれ
がめっき触媒として作用し、後続の無電解銀めっきを促
進する。The function of the pretreatment agent of the present invention is as follows. As described above, the azole-based silane coupling agent component adheres to the surface of the object to be plated, and stannous chloride is added to the adhered azole-based silane coupling agent. Which acts as a plating catalyst and promotes subsequent electroless silver plating.
【００１５】本発明の銀めっき方法によれば、被めっき
材はその性状に制限されない。例えば、ガラス、セラミ
ックなどの無機材料、ポリエステル、ポリアミド、ポリ
イミド、フッ素樹脂などのプラスチック材料、そのフィ
ルム、シート、繊維、必要によりガラス布基材などで補
強されたエポキシ樹脂などの絶縁板などの絶縁物やＳｉ
ウエハーなどの半導体などの導電性の低い被めっき物に
適用されるが、被めっき物は透明ガラス板、Ｓｉウエハ
ー、その他半導体基板のような鏡面物であっても、また
粉体であっても本発明の方法を好ましく適用することが
できる。このような粉体としては、例えばガラスビー
ズ、二硫化モリブデン粉末、酸化マグネシウム粉末、黒
鉛粉末、ＳｉＣ粉末、酸化ジルコニウム粉末、アルミナ
粉末、酸化ケイ素粉末、マイカフレーク、ガラス繊維、
窒化ケイ素、テフロン（登録商標）粉末などが挙げられ
る。According to the silver plating method of the present invention, the material to be plated is not limited in its properties. For example, insulating materials such as inorganic materials such as glass and ceramics, plastic materials such as polyester, polyamide, polyimide and fluororesin, films, sheets, fibers thereof, and insulating plates such as epoxy resins reinforced with glass cloth base materials as necessary. Things and Si
It is applied to low conductive objects such as semiconductors such as wafers, but the object to be plated may be a mirror-like object such as a transparent glass plate, a Si wafer, or other semiconductor substrate, or may be a powder. The method of the present invention can be preferably applied. Examples of such powders include glass beads, molybdenum disulfide powder, magnesium oxide powder, graphite powder, SiC powder, zirconium oxide powder, alumina powder, silicon oxide powder, mica flake, glass fiber,
Examples include silicon nitride and Teflon (registered trademark) powder.
【００１６】無電解めっきをする被めっき材を本発明の
前処理剤で処理する場合、すでに述べたとおり、前処理
剤を水溶液で用いることが好ましいが、例えば、メチル
アルコール、エチルアルコール、２−プロパノール、エ
チレングリコール、ポリエチレングリコールなどやこれ
らを混合した溶媒などに溶解させた溶液も使用できる。
特に水溶液を用いる際は、ｐＨがめっき性を大きく左右
する。めっき触媒（スズ化合物）を固定する窒素の錯体
形成能力からはｐＨは高い方が良いが溶液の安定性が低
下するため、一般にｐＨ１．５〜７が好ましい。When the material to be subjected to electroless plating is treated with the pretreatment agent of the present invention, as described above, it is preferable to use the pretreatment agent in an aqueous solution. A solution in which propanol, ethylene glycol, polyethylene glycol, or the like is dissolved, or a mixed solvent thereof can also be used.
Particularly when an aqueous solution is used, the pH greatly affects the plating property. From the viewpoint of the ability of nitrogen to form a plating catalyst (tin compound) to form a complex with nitrogen, the higher the pH, the better the stability of the solution. Therefore, the pH is generally preferably from 1.5 to 7.
【００１７】本発明の前処理剤には、前記有効成分の
他、必要に応じてｐＨ調整剤、界面活性剤、ｐＨ緩衝剤
などを添加することができる。[0017] In addition to the above-mentioned active ingredients, a pH adjuster, a surfactant, a pH buffer, and the like can be added to the pretreatment agent of the present invention, if necessary.
【００１８】被めっき物を本発明の前処理剤で処理する
方法としては、浸漬、刷毛塗り、スピンコートなどの方
法が一般的であるが、これに限定されるものではない。
その際３０〜８０℃の雰囲気下で処理すると薬剤の付着
性を向上させる上で有効である。As a method of treating the object to be plated with the pretreatment agent of the present invention, a method such as immersion, brush coating, or spin coating is generally used, but is not limited thereto.
At this time, treatment in an atmosphere at 30 to 80 ° C. is effective in improving the adhesiveness of the drug.
【００１９】本発明の前処理剤を用いて銀めっきされた
被めっき物は、銀の密着性に優れているので、銀の殺菌
性を持続的に利用することができ、さまざまな抗菌性製
品に応用することができる。例えば、銀めっきした繊維
から抗菌性衣料などの抗菌性繊維製品を製造することが
できる。The silver-plated object using the pretreatment agent of the present invention has excellent silver adhesion, so that the bactericidal properties of silver can be continuously used and various antibacterial products can be used. It can be applied to For example, antibacterial textile products such as antibacterial clothing can be manufactured from silver-plated fibers.
【００２０】[0020]
【実施例】液の安定性は塩化第一スズを添加し、室温で
一昼夜放置後の沈殿物や生成物の存在を目視により判断
した。めっき付きは、めっきの被覆率および密着性によ
り判断した。めっき前処理剤処理はすべて７０℃に加熱
して行った。なお、ｐＨ調整は塩酸水溶液を用いて行っ
た。EXAMPLES The stability of the solution was determined by adding stannous chloride and leaving it overnight at room temperature to determine the presence of precipitates and products. The case with plating was judged based on the plating coverage and adhesion. All plating pretreatment agent treatments were performed by heating to 70 ° C. The pH was adjusted using an aqueous hydrochloric acid solution.
【００２１】実施例１ イミダゾールとγ−グリシドキシプロピルトリメトキシ
シランとの等モル反応生成物０．０５ｗｔ％水溶液へ室
温で攪拌しながら塩化第一スズを添加し、塩化スズ濃度
が８０ｍｇ／Ｌの溶液を調製した。なお、溶液調製の際
ｐＨは塩酸水溶液により２．０にした。安定性は一昼夜
放置し、液が安定であることを確認した。この溶液にＳ
ｉＯ2粉を加え、１時間室温攪拌し、十分に水洗後、ム
デンシルバー（奥野製薬製）を用いて１５℃で無電解銀
めっきを行った。ＳｉＯ2粉全体に密着性良く銀めっき
された。めっき後の色は黒灰色であった。EXAMPLE 1 Stannous chloride was added to a 0.05 wt% aqueous solution of an equimolar reaction product of imidazole and γ-glycidoxypropyltrimethoxysilane while stirring at room temperature to obtain a tin chloride concentration of 80 mg / L. Was prepared. At the time of preparing the solution, the pH was adjusted to 2.0 with an aqueous hydrochloric acid solution. Stability was allowed to stand overnight, and it was confirmed that the solution was stable. S
The iO 2 powder was added, the mixture was stirred at room temperature for 1 hour, washed thoroughly with water, and then subjected to electroless silver plating at 15 ° C. using Muden Silver (Okuno Pharmaceutical). Silver plating was performed on the entire SiO 2 powder with good adhesion. The color after plating was black-gray.
【００２２】実施例２ 実施例１と同様に、イミダゾールとγ−グリシドキシプ
ロピルトリメトキシシランとの等モル反応生成物と塩化
第１スズとから調製しためっき前処理剤に、ポリエステ
ル繊維を４０℃で５分間浸漬後、十分に水洗した。次
に、ムデンシルバー（奥野製薬製）を用いて１５℃で無
電解銀めっきを行った。ポリエステル繊維全体に密着性
良く銀めっきされた。めっき後の色は淡黄色であった。
テープ引き剥がしテストにより密着性を測定した結果、
テープに銀めっきが付着しなかった。Example 2 As in Example 1, 40 polyester fibers were added to a plating pretreatment agent prepared from an equimolar reaction product of imidazole and γ-glycidoxypropyltrimethoxysilane and stannous chloride. After immersion at 5 ° C. for 5 minutes, it was sufficiently washed with water. Next, electroless silver plating was performed at 15 ° C. using Muden Silver (manufactured by Okuno Pharmaceutical). Silver plating was performed on the entire polyester fiber with good adhesion. The color after plating was pale yellow.
As a result of measuring the adhesion by the tape peeling test,
Silver plating did not adhere to the tape.
【００２３】比較例１ ポリエステル繊維を１０ｇ／Ｌの塩化第一スズの水溶液
に浸漬し、十分に水洗後、ムデンシルバー（奥野製薬
製）を用いて１５℃で無電解銀めっきを行った。ポリエ
ステル繊維全体に密着性良く銀めっきされた。めっき後
の色は淡黄色であった。テープ引き剥がしテストにより
密着性を測定した結果、テープに銀めっきが付着した。Comparative Example 1 A polyester fiber was immersed in a 10 g / L aqueous solution of stannous chloride, washed thoroughly with water, and subjected to electroless silver plating at 15 ° C. using Muden Silver (Okuno Pharmaceutical). Silver plating was performed on the entire polyester fiber with good adhesion. The color after plating was pale yellow. As a result of measuring the adhesiveness by a tape peeling test, silver plating was adhered to the tape.
【００２４】[0024]
【発明の効果】以上説明したように、本発明の前処理剤
を用いることにより、被めっき物に密着性よく銀めっき
を形成することができる。As described above, by using the pretreatment agent of the present invention, silver plating can be formed on an object to be plated with good adhesion.
Claims (5)
カップリング剤とスズ化合物を有効成分とする銀めっき
前処理剤。1. A silver plating pretreatment agent comprising a silane coupling agent having a substituent capable of trapping metal and a tin compound as active ingredients.
カップリング剤が含窒素複素環式アゾール化合物とエポ
キシ基含有シラン化合物との反応生成物であるアゾール
系シランカップリング剤であることを特徴とする請求項
１記載の銀めっき前処理剤。2. The silane coupling agent having a substituent having a metal-capturing ability is an azole silane coupling agent which is a reaction product of a nitrogen-containing heterocyclic azole compound and an epoxy group-containing silane compound. The silver plating pretreatment agent according to claim 1, wherein
ゾールである請求項２記載の銀めっき前処理剤。3. The silver plating pretreatment agent according to claim 2, wherein the nitrogen-containing heterocyclic azole compound is imidazole.
特徴とする請求項１、２又は３記載の銀めっき前処理
剤。4. The silver plating pretreatment agent according to claim 1, wherein the tin compound is stannous chloride.
載の銀めっき前処理剤で処理した後、無電解銀めっきす
ることを特徴とする銀めっき方法。5. A silver plating method, comprising: treating an object to be plated with the silver plating pretreatment agent according to claim 1, followed by electroless silver plating.
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| JP2000232782A JP4836312B2 (en) | 2000-08-01 | 2000-08-01 | Silver plating pretreatment agent and silver plating method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7867564B2 (en) | 2002-09-10 | 2011-01-11 | Nippon Mining & Metals Co., Ltd. | Metal plating method and pretreatment agent |
| JP2013001935A (en) * | 2011-06-15 | 2013-01-07 | Adeka Corp | Organic silicon compound and pretreatment method for electroless plating using organic silicon compound |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63227784A (en) * | 1987-03-16 | 1988-09-22 | Toyobo Co Ltd | Method for providing electroless plating catalyst |
| JPH11335858A (en) * | 1998-05-27 | 1999-12-07 | Yuji Shikamata | Formation of silver plating surface and solution used therefor |
| WO2000001862A1 (en) * | 1998-07-07 | 2000-01-13 | Japan Energy Corporation | Pretreating agent for metal plating, and method for metal plating using the same |
| JP2000104175A (en) * | 1998-09-30 | 2000-04-11 | Inoac Corp | Vessel and its production |
| JP2000129452A (en) * | 1998-10-23 | 2000-05-09 | Inoac Corp | Electroless plating primer agent, laminate provided with electroless plating layer and its production |
-
2000
- 2000-08-01 JP JP2000232782A patent/JP4836312B2/en not_active Expired - Lifetime
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63227784A (en) * | 1987-03-16 | 1988-09-22 | Toyobo Co Ltd | Method for providing electroless plating catalyst |
| JPH11335858A (en) * | 1998-05-27 | 1999-12-07 | Yuji Shikamata | Formation of silver plating surface and solution used therefor |
| WO2000001862A1 (en) * | 1998-07-07 | 2000-01-13 | Japan Energy Corporation | Pretreating agent for metal plating, and method for metal plating using the same |
| JP2000104175A (en) * | 1998-09-30 | 2000-04-11 | Inoac Corp | Vessel and its production |
| JP2000129452A (en) * | 1998-10-23 | 2000-05-09 | Inoac Corp | Electroless plating primer agent, laminate provided with electroless plating layer and its production |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7867564B2 (en) | 2002-09-10 | 2011-01-11 | Nippon Mining & Metals Co., Ltd. | Metal plating method and pretreatment agent |
| JP2013001935A (en) * | 2011-06-15 | 2013-01-07 | Adeka Corp | Organic silicon compound and pretreatment method for electroless plating using organic silicon compound |
Also Published As
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|---|---|
| JP4836312B2 (en) | 2011-12-14 |
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