JPS60502057A - Electroless nickel plating of aluminum - Google Patents
Electroless nickel plating of aluminumInfo
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- JPS60502057A JPS60502057A JP59503212A JP50321284A JPS60502057A JP S60502057 A JPS60502057 A JP S60502057A JP 59503212 A JP59503212 A JP 59503212A JP 50321284 A JP50321284 A JP 50321284A JP S60502057 A JPS60502057 A JP S60502057A
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- nickel
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- protective coating
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- 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
- C23C18/1601—Process or apparatus
- C23C18/1633—Process of electroless plating
- C23C18/1646—Characteristics of the product obtained
- C23C18/165—Multilayered product
- C23C18/1651—Two or more layers only obtained by electroless plating
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- Organic Chemistry (AREA)
- Chemically Coating (AREA)
- Other Surface Treatments For Metallic Materials (AREA)
Abstract
(57)【要約】本公報は電子出願前の出願データであるため要約のデータは記録されません。 (57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.
Description
【発明の詳細な説明】 アルミニウムの＝！解ニッケルめっき 技術分野 本発明は総体的にアルミニウムおよびその合金の無電解ニッケルめっきの方法に 関する。[Detailed description of the invention] = of aluminum! Nickel plating Technical field The present invention generally relates to a method of electroless nickel plating of aluminum and its alloys. related.
技術的背景 無電解ニッケルめっきは、金属仕上げ製造菓においてニウムおよびその合金を含 む多くの金属基質に幅広く採用されている工程である。アルミニウム、マグネシ ウムおよびその合金のようなめつき金属は、しかしながら、１つに関しては、め っきのために表面を番殊な予備めつき処理した状態を必要とする表面ば化コーテ ィングを有するため、電気めっき装置に格別な問題を生起する。本発明はニッケ ル、コバルトおよびニッケルーコノくルト合金のような金属でこのような金属基 質へ無電解めっきを可能にする一方、後述する説明は主として亜鉛コーティング をその表面に付設することによシめつきのために適合されたアルミニウムおよび ゛ｒルミニウム合金の無電解ニッケルめっきに好適であるよう企画されている。Technical background Electroless nickel plating is used in metal finishing products containing nickel and its alloys. This process is widely used for many metal substrates. aluminum, magnesi Plating metals such as aluminum and its alloys, however, are Surface anti-plating coating that requires special pre-plating treatment on the surface for plating. This creates special problems for electroplating equipment. The present invention Metals such as nickel, cobalt, and nickel-conolt alloys Although electroless plating is possible to achieve high quality, the following explanation is mainly for zinc coating. Aluminum and adapted for fastening by attaching to its surface It is designed to be suitable for electroless nickel plating of aluminum alloys.
一般的に、アルミニウム部品はまず有機表面汚染物を浄化され、引続き固形不純 物および混存成分を表面から！ 除去するようエツチングし、酸化膜を取り除くよう生成物除去しく ａ８ｅｍｕ ｔｔｉ’ｎｇ） 、そして浄化済表面の再酸化を防止するよう亜鉛や逮のような 保＠層で被覆する。その部品は通常上述の各工程の後に洗浄されそしてＲ直屏ニ ッケルめっきのために準備される。Typically, aluminum parts are first cleaned of organic surface contaminants, followed by solid impurities. Remove substances and mixed components from the surface! Etch to remove the oxide film and remove the product by removing the oxide film. tti’ng) and contain substances such as zinc and aluminum to prevent re-oxidation of cleaned surfaces. Cover with a protective layer. The part is usually cleaned after each of the steps mentioned above and Prepared for nickel plating.
しかしながら、亜鉛酸塩化アルミニウム（Ｚｉｎｃａｊ８ａａ１ｍｉｎｕｍ ） をめっきするのに用いられる無電解ニッケルめっき浴（ｂａｔｈ）は、平板鋼の ようなその他の多くの金属合金をめっきするのに用いられる浴に比べると、不適 当にも相対的に短期な浴寿命である。かくして、例えば通常鋼について約１０回 転（ｔｕｒｎｏＶｅｒ ）利用できる浴が、アルミニウム保−被覆には約５回転 利用できるだけである。この後にニッケルをアルミニウム結晶出する（ ｄｅｐ ｏｓｉｔ ）ことは気泡を生じ始めるので溌莱および交換されねばならない。１ 回転ばめつきされたニッケル金属の量が浴内の形成されるべきニッケルの量と等 しくなる間の期間として定義される。例えば、最初にｆＪ６！７／ｌのニッケル を含有した浴の場合、該浴は通常ニッケルがめつき中に消費される６ｙ／ＩＫ戻 るようニッケル塩を補充される。６ｇ／ｌのニッケルの累加的な補充は１回転を 塊わす。However, aluminum zinc chloride (Zincaj8aa1minum) The electroless nickel plating bath used to plate flat steel Compared to baths used to plate many other metal alloys, such as Indeed, the bath life is relatively short. Thus, for example about 10 times for normal steel A turnoVer bath is available, approximately 5 turns for the aluminum preservation coating. available only. After this, nickel is crystallized from aluminum (dep The oil will begin to form bubbles and must be replaced. 1 The amount of nickel metal rotated is equal to the amount of nickel to be formed in the bath. defined as the period of time between For example, first fJ6!7/l nickel In the case of a bath containing Replenishment with nickel salts will be performed. Cumulative replenishment of 6 g/l nickel takes 1 revolution. It's a lump.
亜鉛酸ｊ化（ｚｉｎｃａｔｉｎｇ ）は、亜鉛酸塩イオンケ含有するアルカリ性 溶液にアルミニウム部品を凝すことのみを必要とする相対的に簡単な工程である ので、アルミ−ニウム表面を予備処理するのに商業上重要な工程である。析出さ れた亜鉛の量は実際には非常に少なくそして使用される浸漬槽、アルミニウム合 金、浴液の温度および予備処理工程の時間および形式に左右され、約ａ１ミクロ ンまでの厚さが通常採用されている。Zincating is an alkaline solution containing zincate ions. It is a relatively simple process that only requires condensing the aluminum parts in a solution. Therefore, it is a commercially important step for pretreating aluminum surfaces. precipitation The amount of zinc used is actually very small and depends on the dipping bath used, the aluminum Depending on the gold, the temperature of the bath and the time and type of pre-treatment step, approximately a1 micro Thicknesses up to 100 mm are usually used.
亜鉛酸塩化工程（ＺｉｎＣａｔｌ；８ ｐｒｏｃθｓｓ）の代りに、Ｗｒｉｇｈ ｔ氏他の米国特許第４６６６．５２９号に示されており、それは、基本的に、ア ルミニウム結晶を絽出しそしてニッケル被覆を析出するよう酸性の塩化ニッケル 溶液でアルミニウムをエツチングし、ニッケル・被覆１ＨＮｏ。Instead of the zincation step (ZinCatl; 8 procθss), Wright No. 4,666,529 to T. et al., which basically Acidic nickel chloride to crystallize the aluminum crystals and deposit the nickel coating. Etch aluminum with solution and nickel coat 1HNo.
（硝酸）で除去し、次亜リン酸イオンを含むアルカリ性浴液で活性化し、そして ニッケルのアルカリ性ストライク被覆（ｑｌｋａｌｉｎ８５ｔｒｉｋｅ Ｃ０ｑ ｔ ）を８０℃〜９０℃でめっきし、引続いて所要のニッケル厚に無電解ニッケ ルめっきを行う、こととからなるアルミニウム表面を処理する方法を開示してい る。(nitric acid), activated with an alkaline bath solution containing hypophosphite ions, and Nickel alkaline strike coating (qlkalin85trike C0q t) at 80°C to 90°C, followed by electroless nickel plating to the required nickel thickness. discloses a method for treating aluminum surfaces consisting of Ru.
Ｂｅｌｌｉｓ氏他の米国特許第３，６７２，９６４号では、弗化水素酸水溶液と 、アルミニウムによシ置き換えられかつ無電解ニッケルめっきに活性的な部材と でアルミニウム表面を予備処理し、その後にアミンポラン（ｑｍｉｎθｂｏｒ５ １ｎｅ ）と−価または二価の虞化化合物を含有するｐＨ６〜７の無電解ニッケ ル浴で処理済アルミニウム表面にめっきすることが開示されている。しかしなが ら、これらの特許は亜鉛酸塩化アルミニウムの無電解ニッケルめっきにおいて遭 遇する問題に対処できず、１曲格の高騰や時間の浪費となる代用工程を徒供する のみである。No. 3,672,964 to Bellis et al. , an active material for electroless nickel plating that can be replaced by aluminum. The aluminum surface was pretreated with 1ne) and an electroless nickel with a pH of 6 to 7 containing a -valent or divalent oxidizing compound The method of plating treated aluminum surfaces in a metal bath is disclosed. But long These patents were encountered in electroless nickel plating of aluminum zinc chloride. Instead of being able to deal with the problems faced, they resort to substitute processes that result in higher prices and a waste of time. Only.
発明の開示 亜鉛またはその他の保護被覆で前処理されたアルミニウムの無電解ニッケルめっ きは、多様のめつきｔ谷を調整された粂件下で採用することによシ改督されうる 。概説すると、本工程は、例えば、無電解のニッケル浴から亜鉛酸塩化された表 面に薄い第２の床−一覆を適用し、引続いて所要の厚さおよび物理的持回まで該 表面をめっきするよう別のニッケル浴を使用することからなる。本工程はかくし て少なくとも２つのニッケルめつき俗を採用し、その第１浴は亜鉛酸塩化された 表面にニッケルの簿い保腫被覆を通用するよう用いられ、１つまだＵ複数の第２ 浴によって、最終ニッケル被覆をめ′つきするよう用いられる。本工程はその結 果、亜鉛酸塩化アルミニウムを所要厚めつきするのに１つの浴を開用する従来技 術工程と比較して朽２倍の回転埒鮪（ｔｕｒｎｏｖｅｒ １ｉｆｅ ）となる。Disclosure of invention Electroless nickel plating of aluminum pretreated with zinc or other protective coating can be reformed by adopting a variety of methods under adjusted conditions. . In general terms, this process involves, for example, extracting a zincated surface from an electroless nickel bath. Apply a thin second bed-cover to the surface, then apply to the desired thickness and physical coverage. It consists of using a separate nickel bath to plate the surface. This process is hidden At least two nickel plating baths are used, the first of which is zincated. It is used to pass through the nickel surface coating, with one U and a plurality of second The bath is used to plate the final nickel coating. This process is the result As a result, the conventional technique of using one bath to thicken aluminum zinc chloride to the required thickness It becomes a turnover tuna (turnover 1ife) that is twice as long as the process.
篤くべきことに、第１浴は、亜鉛表面に第２保護被覆を直接適用するよう使用さ れているにも掛わらずその通常の回転寿命限界に到達する前に広範に持枕し、亜 鉛酸塩化表面が相対的に刀時間めっき溶液と接触されるのみで所要厚にめっきす る従来技術とは明確に異なった工程である。本発明の工程を使用することによっ て、例えば２つの浴を、順次に通り処理されうる作業量は、浴を別々に使用する 場合よりも実質的に多く（約２倍）なる。Importantly, the first bath is used to apply the second protective coating directly to the zinc surface. Despite the fact that the The lead chloride surface is plated to the required thickness by only being in contact with the plating solution for a relatively short period of time. This process is clearly different from the conventional technology. By using the process of the present invention For example, the amount of work that can be processed through two baths sequentially may be reduced by using the baths separately. substantially more (approximately twice) than in the case of
発明を実施するための様式 無電解ニッケルめっきされるべきアルミニウム部品は、上述の如く、予備処理さ れそして亜鉛、まだは錫のような他の金属のような保護被覆が周知の技術および 工程を用いて設けられる。通常１０チ以下の少量の金属が、とりわけその上に被 覆を析出する％性のような目的のために保護被覆金属と共に析出されうる。コバ ルト、ニッケル、銅および鉄のような多くの金属が使用されうる。Form for carrying out the invention Aluminum parts to be electroless nickel plated are pretreated as described above. Protective coatings such as zinc and other metals such as tin are well known techniques and It is provided using a process. A small amount of metal, usually less than 10 inches, is especially deposited on it. It can be deposited with a protective coating metal for purposes such as the ability to deposit a coating. Koba Many metals can be used such as iron, nickel, copper and iron.
ニッケル被覆を適用するだめの無電解ニッケルめっき組成は周知の技術でありそ してめっき工程および組成は種々の公知文献に述べられている。例えば、無電解 ニッケルを析出するだめの組成は本国特許第２，６９０，４０１号、同第２，６ ９０，４０２号、同第２，７６２，７２３号、同第２，９３５，４２５号、同第 ２，９２９，７４２号および同第３．３３８，７２６号に述べられている。ニッ ケルおよびその合金を析出させるだめのその他の有効な組成はニューｕｔ）１１ ０ｑ１；１ｏｎ８ 、工ｎｃ、社の１９６７年版の６５ ｔｈ Ａｎｎｕ−ａｌ Ｅｄｉｔｉｏｎ Ｏｆ ｔｈｅ Ｍｅｔａｌ Ｆｉｎｉｓｈｉｎｇ Ｇｕｉｄ ｅｂｏｏｋ第４８５Ａ〜第４８６頁に開示されている。前述の各公知文献はここ において参照文献として包括される。The electroless nickel plating composition for applying the nickel coating is a well-known technology and is likely to be used. The plating process and composition are described in various known documents. For example, electroless The composition of the tank in which nickel is deposited is disclosed in Japanese Patent Nos. 2,690,401 and 2,6. No. 90,402, No. 2,762,723, No. 2,935,425, No. 2,935,425, No. No. 2,929,742 and No. 3,338,726. Ni Other effective compositions of tanks for precipitating Kel and its alloys are new) 11 0q1;1on8, 65th Annu-al of the 1967 edition of Engineering NC, Inc. Edition Of the Metal Finishing Guide It is disclosed on pages 485A to 486 of the ebook. Each of the above-mentioned known documents can be found here. Included as a reference in .
概括的に、無電解ニッケル析出浴液は浴媒、典型的には水、に溶解された少なく とも４つの材料からなる。それらは、（１）ニッケルイオン源と、（２）次亜リ ン酸塩またはアミンボランのような還元剤と、（３）所景の、Ｈ度を提供する酸 性まだは水酸化ＰＨ調和剤と、（４）溶液中の金属イオンの沈澱を防止するのに 十分な錯化剤とである。数多くの無電解ニッケル溶液のための好適な錯化剤が上 述した公知文献に述べられている。幾つかの策定において、錯化剤は有用ではお るが必須のものではない。これらの技術的手法によって、ニッケル、または適用 されるその他の金属は、他の金員との合金の形体で通常を中に与えられることは 明らかである。かくして、次亜リン酸塩が還元剤として用いらｎると、析出中に ｎニッケルとリン（ｐｈｏａｐｈｏｒｏｕ８ ）を含有する。同様に、アミンボ ランを採用すると、析出中にはニッケルとボランとを含有する。かくして、ニッ ケルと称する１ものを匝用することは通常それと共に析出される他の要素を包含 する。Generally speaking, an electroless nickel deposition bath solution consists of a small amount of nickel dissolved in a bath medium, typically water. Both are made of four ingredients. They are (1) a nickel ion source and (2) a hypochlorite source. a reducing agent such as a phosphate salt or an amine borane; and (3) an acid that provides the H degree. (4) To prevent the precipitation of metal ions in solution, with sufficient complexing agent. A number of suitable complexing agents for electroless nickel solutions are listed above. It is described in the above-mentioned known documents. In some formulations, complexing agents may not be useful. However, it is not required. By these technical methods, nickel or applied Other metals that are used are usually present in the form of alloys with other metals. it is obvious. Thus, when hypophosphite is used as a reducing agent, during precipitation Contains n-nickel and phosphorus (phoaphorou8). Similarly, aminebo When oran is used, the precipitation contains nickel and borane. Thus, Ni The use of one thing, called Kel, usually includes other elements that are deposited with it. do.
ニッケルイオンは硫酸ニッケル、塩化ニッケル、酢酸ニッケルおよびそれらの混 合物のようないかなる可溶性塩の使用でも提供されうる。溶液中のニッケルの濃 度は非常に広範でありそして約Ｑ、１〜１００！Ｉ／ＶでｈＦ）、約２〜５０ｙ ／ｌが好ましく、例とじ又は、２〜１０！Ｉ／ｌである。Nickel ions include nickel sulfate, nickel chloride, nickel acetate, and mixtures thereof. The use of any soluble salt such as a compound may be provided. Concentration of nickel in solution The degrees are very wide and about Q, 1 to 100! hF at I/V), about 2-50y /l is preferable, for example, 2 to 10! I/l.
還元剤は通常ナトリウム、カリウム、アンモニウムおよび次亜リン酸ニッケルの ようないずれかの好適な源によって浴に次亜リン酸イオンを供給する。アミンボ ラン、水酸化ホウ素（ｂｏｒｏｈｙａｒｉｉθＳ）およびヒドラジンのような他 の還元剤もまた好適に採用されうる。還元剤の濃度は総体的に浴中のニッケルを 減少するのに十分な量を超過している。Reducing agents are usually sodium, potassium, ammonium and nickel hypophosphite. Hypophosphite ions are supplied to the bath by any suitable source, such as. Amimbo Ran, boron hydroxide (borohyariiθS) and others such as hydrazine Reducing agents may also be suitably employed. The concentration of the reducing agent generally reduces the nickel in the bath. in excess of enough to cause a decrease.
浴は酸性、中性またはアルカリ注であり、そして酸性またはアルカリ性ｐＨ度の 調和剤は水酸化アンモニウム、水酸化す）ＩＪウム、塩酸等のような広範な部材 から選定される。浴のｐＨは約２〜１１．５の範囲であり、第２保護被覆を析出 するにはｐＨ７〜１２、例としてはＰＨ９〜１１の範囲であるのが好ましく、ニ ッケルの最終層を析出するのに用いられる浴にはｐＨ２〜７、例としてはＰＨ４ 〜６の範囲であるのが好ましい０ 錯化剤は、酢酸塩、クエン酸塩、グリコール酸塩（ｇ−１ｙｃＯ１１４ｔθ）、 ピロリン酸塩および同様な部材、そして好適なそれらの混合物のような陰イオン を含む多種の部材から選定される。雇イオンに基礎づけられる錯化剤の範囲は、 例えば、約０〜３００ｙ／ｌ、好ましくは約５〜５０ｙ／ｌと非常に広い。Baths can be acidic, neutral or alkaline, and have an acidic or alkaline pH. Conditioners include a wide range of materials such as ammonium hydroxide, IJ hydroxide, hydrochloric acid, etc. Selected from. The pH of the bath ranges from about 2 to 11.5 to deposit a second protective coating. The pH is preferably in the range of 7 to 12, for example 9 to 11. The bath used to deposit the final layer of nickel has a pH between 2 and 7, e.g. Preferably in the range 0 to 6 Complexing agents include acetate, citrate, glycolate (g-lycO114tθ), Anions such as pyrophosphate and similar members, and suitable mixtures thereof. Selected from a wide variety of materials including. A range of complexing agents based on ions are: For example, it is very wide, about 0 to 300 y/l, preferably about 5 to 50 y/l.
無電解ニッケルめっき浴はまた緩衝剤、浴安定剤、比率活性化剤、光沢剤寺のよ うなその曲の周知の組成成分も含む。Electroless nickel plating baths also contain buffering agents, bath stabilizers, ratio activators, brighteners, etc. It also includes the well-known compositional components of Unaso's song.
好適な浴は水中で組成成分を醒屏しかつＰＨ度を所要範囲に調節することによっ て形成される。Suitable baths are prepared by separating the composition components in water and adjusting the pH level within the required range. It is formed by
亜鉛保護被覆機アルミニウム部品は、板長ニッケルめっきに気泡のない析出を行 うのに好ましい保護被覆を提供するのに十分な厚さ、例えば、約Ｑ、ｌ ｍｉｌ まで、あるいはそれ以上まで、好ましくはＱ、００５〜０．０８旭１、例えば、 Ｑ、０１〜α０５凪１、に無電解ニッケル浴中に部品を浸漬することによる無電 解ニッケルめっきにより第２保禮被覆でめっきされる。１５秒〜１５分の浸漬時 間で、浴パラメータ次第であるが、所要の被覆を通常提供する。約２５℃から沸 騰点、例えｌ−ｆ、、１００″ｃ−１での温度範囲で採用され、好捷しくは約６ ５〜９５１〕である本工程の次の段階は、ニッケルめっきを所要の厚さおよび物 理的％注に完成するよう、約３０〜１００℃、例えば、沸騰点、好ましくは８０ 〜９５℃の温度範囲に保持された別の無電解ニッケルめっき浴にニッケル部品を 浸漬することにより行われる。５ ｍｉｌまで、またはそれ以上の厚さが採用さ れ、般も良好ｆｘ適用としては約０．１〜２ｒｎｉｌの範囲が用いられる。Zinc protective coating machine aluminum parts provides bubble-free deposition on long nickel plated plates. sufficient thickness to provide a desirable protective coating for the seams, e.g., about Q, l mil. up to or above, preferably Q, 005 to 0.08 Asahi 1, e.g. Electroless treatment by immersing the parts in an electroless nickel bath at Q, 01~α05 Calm 1 It is plated with a second protective coating by electrolytic nickel plating. When immersed for 15 seconds to 15 minutes Depending on the bath parameters, the required coverage will usually be provided. Boiling from about 25℃ It is employed in the temperature range of rising point, e.g. l-f, 100"c-1, preferably about 6 The next step in this process is to apply nickel plating to the required thickness and material. about 30-100°C, e.g. boiling point, preferably 80 Nickel parts are placed in a separate electroless nickel plating bath maintained at a temperature range of ~95°C. It is done by immersion. Thicknesses up to 5 mils or thicker may be used. Generally speaking, a range of about 0.1 to 2 rnil is used for good fx applications.
めっきの程度は多くの要因によって左右され、それらの要因は（１）めっき溶液 のＰＨと、（２）還元剤の一度と、（３）めっき浴の温度と、（４）可溶性ニッ ケルの一度と、（５）浴の一着／めっきされる一面積の比率と、（６）可溶性塩 フッ化物（ｆｌｕｏｒｉｄｅ ５ａｌｔｓ ） （比率活性化剤）のび在と（力 は着剤（ｗｅｔｔｉｎｇ ａｇｅｎｔ ）および／または浸ａＪＩＩ （ａｇｉ −ｔａｔｉＯｎ ）のσ在、とを含むことはこれらの技術分野で明らかであυ、 そして上述のパラメータは本発明を実施するのに一般的な事例を与えるよう提示 されているのみであることもまた明らかであり、本発明は効果的なめつき工程を 提供するよう上述したような複数の浴を使用することにある。The degree of plating depends on many factors, including (1) plating solution; (2) the temperature of the reducing agent, (3) the temperature of the plating bath, and (4) the soluble nitrogen. (5) the ratio of one piece of bath/one area plated, and (6) the soluble salt. Fluoride 5 alts (ratio activator) and (power) is a wetting agent and/or aJII (agi It is clear in these technical fields that σ exists in -tatiOn), υ, and the above parameters are presented to give a general case for implementing the invention. It is also clear that the present invention provides an effective plating process. The solution lies in the use of multiple baths as described above.
実施されうる工程での種々のめつき浴および条件を示す例を以下に述べる。Examples are provided below showing various plating baths and conditions in the process that may be carried out.
例 Ｉ Ａｌｕｍｉｎｕｍ Ａ３８０Ｃ１ａ１：ｉｏｎ Ｎｕｍｂｅｒ ６Ｑ Ｑ ３の ２１／２×４のアルミニウムパネルをアルカリ洗浄し、水洗いし、酸エツチング し、水洗いし、汚れ除去（ｄｅｓｍｕｔ ）し、そして水洗いした。欠いて該パ ネルは１００ｙ／４のＺｎＯと５００ｇ／ｌのＮａＯＨと１ｙ／ｌのＦｔＣｌｓ と１０ｓｌｌのロッシェル塩とをき有した水成浴を用いて室温で５０秒間亜鉛酸 塩化された。パネルは水洗いされそしていくつかのパネルは約９０℃に保持され た商品名ＥＮＰ −ＬＡＴＩＢ Ｎニー４６１としてＥｎｔｈｏｎｅ、■ｎｃｏ ｒｐｏｒａｔｅａ社によって販売されている無電解ニッケルめっき心中に約３０ 分間浸漬することによりめっきされた。ボ’Ｉ （ｌ１４ ｒ７！ｉｌの被覆が 各パネルに得られた。ニッケルおよび次亜リン酸塩濃度は約４１／ｌのニッケル 一度に低下したときに補充された。ニッケルめっきに気泡が生じ始めるまでに合 計５回転できた。浴は通常亜鉛酸塩化されたアルミニウムをめっきするよう更に 使用することができずそして廃棄しなければならないことがここにおける要点で ある。Example I Aluminum A380C1a1:ion Number 6Q Q3 Alkaline cleaning, water washing, and acid etching of 21/2 x 4 aluminum panels washed, desmuted, and rinsed with water. Lacking the pa The flannel is made of 100y/4 ZnO, 500g/l NaOH, and 1y/l FtCls. and 10 sll of Rochelle's salt for 50 seconds at room temperature. Chlorinated. The panels were washed with water and some panels were held at about 90°C. Product name ENP-LATIB N knee 461 as Enthone, nco Approximately 30% electroless nickel plated core sold by Rporatea Plated by dipping for minutes. B’I (l14 r7!il’s coating is obtained in each panel. Nickel and hypophosphite concentration is approximately 41/l nickel It was replenished when it was low at once. Until the nickel plating begins to form bubbles, I was able to do a total of 5 rotations. The bath is typically further plated with zincated aluminum. The point here is that it cannot be used and must be discarded. be.
上述の如く準備された亜鉛酸塩化されたアルミニウムパネルは下記の無電Ｓニッ ケルめっき浴中で４０℃で６分１ｉＪ］ ニッケルの薄い第２保護被覆（朽ｏ、 ０２ｍ１ｌ＞ｋメっきされた。The galvanized aluminum panels prepared as described above were coated with the following electroless S-Ni 1 iJ for 6 minutes at 40°C in a Kel plating bath] Thin second protective coating of nickel (decay, 02ml1l>k plated.
ｍ酸ニッケ＃ （Ｎ１ｃｋｅｌ ＳｕｌｆａｍＢｔｅ ） ２４ ｇ ／ ｌピ ロリン酸テトラカリウム ｂ、Ｇｙ／１次亜リン酸ナトリウム ２７．ｙ／ｌ ｐＨ１０に保持するためのＮＨ４ＯＨ 欠いて５回転を有するめっき浴に浸漬されて気泡のないニッケル析出を得られた 。約６０分間の浸漬時間が約Ｑ、４ ｍｉｌのニッケル厚を作成した。めっきさ れた／くネルを取り外して、亜鉛酸塩化されたにニッケル第２保護被覆のない） パネルを同じ浴に浸漬したところ、被覆に気泡を生じた。上述の手順が複数回繰 返され、第２保護ニツケル被覆を有する亜鉛酸塩化アルミニウムパネルは亜鉛酸 塩化アルミニウム（薄い第２保護ニツケル被覆を有していない）に得られた気泡 を生じた析出に比べて気泡のない析出を得た。別の４回転が得られその結果浴に 対し合計約９回転であった。浴は通常約９〜１０回転した時点においても第２保 護被覆パネルにめっきするのに有効であったがそのめっき速度は非常に遅かった 。Nickel m acid # (N1ckel SulfamBte) 24 g / l pi Tetrapotassium rophosphate b, Gy/1 Sodium hypophosphite 27. y/l NH4OH to maintain pH 10 It was immersed in a plating bath with 5 rotations to obtain bubble-free nickel deposition. . A soak time of about 60 minutes produced a 4 mil nickel thickness of about Q. Plating (Without the nickel secondary protective coating on the galvanized surface) When the panel was immersed in the same bath, the coating developed bubbles. The above steps are repeated multiple times. Zincified aluminum panels with a second protective nickel coating are Air bubbles obtained in aluminum chloride (without a thin second protective nickel coating) A bubble-free precipitation was obtained compared to the precipitation that produced bubbles. Another quadruple is obtained resulting in a bath In contrast, the total number of rotations was approximately 9. The bath usually remains in the second protection state even after about 9 to 10 revolutions. It was effective for plating protective coating panels, but the plating speed was very slow. .
この例は、亜鉛酸塩化アルミニウムをめっきするのに使用される無電解ニッケル めっき浴の寿命が亜鉛酸塩化アルミニウムを浴に浸漬する前に薄い第２保護ニツ ケル被覆を行う場合に増長されることを実証している。An example of this is electroless nickel used to plate aluminum zinc chloride. The life of the plating bath is limited by the use of a thin second protective coating before dipping the aluminum zinc chloride into the bath. It has been demonstrated that the growth is increased when a Kel coating is applied.
前述のようにして亜鉛酸塩化されたアルミニウムパネルに下記の組成成分を含有 しＨＥ、ＯＲでｐＨ’ ７．５に調節された無電解めっき浴中で６５℃で５分間 、ニッケルの薄い第２保護被覆（約０．０２ｍ１ｌ ）をめっきした。The zincated aluminum panel as described above contains the following composition components. 5 minutes at 65℃ in an electroless plating bath adjusted to pH'7.5 with HE and OR. , a thin second protective coating of nickel (approximately 0.02 ml) was plated.
Ｎ１Ｅ３０、−６Ｈρ ４ｙ／１ ｃｓｏ４．７Ｈｐ ２８ ｙ／１ クエン酸ナトリウム・２Ｅ＊Ｏ７５ダ／ｌＮｍ、ｃｔ ４２ ｙ／ １ このパネルを例１のめっき浴（５回転されている）に浸漬したところ、気泡のな いニッケル析出を得られた。N1E30, -6Hρ 4y/1 cso4.7Hp 28y/1 Sodium citrate・2E*O75 da/lNm, ct 42 y/1 When this panel was immersed in the plating bath of Example 1 (which had been rotated 5 times), no air bubbles were observed. A thick nickel deposit was obtained.
薄いニッケル被覆のない亜鉛酸塩化パネルを同じ蔭に浸漬したところ、気泡を生 じた析出であった。When a galvanized panel without a thin nickel coating was immersed in the same shade, air bubbles formed. There was a slight precipitation.
例 ■ 例■がＥｎｔｈｏｎｅ、■ｎｃＯｒｐｏｒｆｉｔｅｄ社の販売するＥＮＰ−ＬＡ ＴＥ Ｎニー４５１を使用して薄いニッケル第２保護被覆を無電解めっきするよ う繰返され、それにょシ同様な結果を得た。すなわち、第２保護被覆付きパネル は気泡のない析出でありそして亜鉛被覆パネルは気泡を生じた析出であった。Example ■ Example ■ is Enthone, ■ ENP-LA sold by ncOrporfited Electroless plating a thin nickel second protective coating using TE N-451. It was repeated with similar results. i.e. a panel with a second protective coating was a bubble-free deposit and the zinc coated panel was a bubble-filled deposit.
ここにおいて本発明の好適実施例についての考察を叙述したが、種々の応用がそ こにおいて遂行しえることは理解されよう、そして従属の請求の範囲に２いて本 発明の真の主意および範囲内にあるような全ての応用を包括することを意図して いる。Although a discussion of preferred embodiments of the invention has been described herein, various applications may be found therein. It will be understood that this may be accomplished in this context, and that the dependent claims include two main claims. Intended to cover all such applications as fall within the true spirit and scope of the invention. There is.
国際調査報告international search report
Claims (1)
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US52535883A | 1983-08-22 | 1983-08-22 | |
| US525358 | 1983-08-22 | ||
| HK98105637A HK1006860A1 (en) | 1983-08-22 | 1998-06-18 | Electroless nickel plating of aluminum |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS60502057A true JPS60502057A (en) | 1985-11-28 |
| JPH0319302B2 JPH0319302B2 (en) | 1991-03-14 |
Family
ID=26316726
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP59503212A Granted JPS60502057A (en) | 1983-08-22 | 1984-08-08 | Electroless nickel plating of aluminum |
Country Status (9)
| Country | Link |
|---|---|
| EP (1) | EP0153369B1 (en) |
| JP (1) | JPS60502057A (en) |
| AU (1) | AU558946B2 (en) |
| BR (1) | BR8407027A (en) |
| CA (1) | CA1220101A (en) |
| DE (1) | DE3486228T2 (en) |
| HK (1) | HK1006860A1 (en) |
| MX (1) | MX167978B (en) |
| WO (1) | WO1985001070A1 (en) |
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| KR20160132775A (en) * | 2015-05-11 | 2016-11-21 | 도쿄엘렉트론가부시키가이샤 | Plating method and recording medium |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US5476688A (en) * | 1988-08-29 | 1995-12-19 | Ostolski; Marian J. | Process for the preparation of noble metal coated non-noble metal substrates, coated materials produced in accordance therewith and compositions utilizing the coated materials |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5345787A (en) * | 1976-10-08 | 1978-04-24 | Shiguma Ruutein Narodoni Podon | Method of working nonncircular functional hole of drawing die |
| US4346128A (en) * | 1980-03-31 | 1982-08-24 | The Boeing Company | Tank process for plating aluminum substrates including porous aluminum castings |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US366529A (en) * | 1887-07-12 | James timms | ||
| US4169171A (en) * | 1977-11-07 | 1979-09-25 | Harold Narcus | Bright electroless plating process and plated articles produced thereby |
| JPS6015706B2 (en) * | 1977-12-19 | 1985-04-20 | 株式会社東芝 | Surface treatment method of Al and Al alloy for soldering |
| US4358923A (en) * | 1980-04-10 | 1982-11-16 | Surface Technology, Inc. | Composite coatings for open-end machinery parts |
| SU926064A1 (en) * | 1980-07-15 | 1982-05-07 | Алтайский Сельскохозяйственный Институт | Aqueous solution for preparing metal surface to chemical nickel plating |
-
1984
- 1984-08-08 AU AU32178/84A patent/AU558946B2/en not_active Ceased
- 1984-08-08 DE DE84903142T patent/DE3486228T2/en not_active Expired - Lifetime
- 1984-08-08 WO PCT/US1984/001253 patent/WO1985001070A1/en active IP Right Grant
- 1984-08-08 JP JP59503212A patent/JPS60502057A/en active Granted
- 1984-08-08 BR BR8407027A patent/BR8407027A/en not_active IP Right Cessation
- 1984-08-08 EP EP84903142A patent/EP0153369B1/en not_active Expired - Lifetime
- 1984-08-17 CA CA000461286A patent/CA1220101A/en not_active Expired
- 1984-08-21 MX MX202448A patent/MX167978B/en unknown
-
1998
- 1998-06-18 HK HK98105637A patent/HK1006860A1/en not_active IP Right Cessation
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5345787A (en) * | 1976-10-08 | 1978-04-24 | Shiguma Ruutein Narodoni Podon | Method of working nonncircular functional hole of drawing die |
| US4346128A (en) * | 1980-03-31 | 1982-08-24 | The Boeing Company | Tank process for plating aluminum substrates including porous aluminum castings |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20160132775A (en) * | 2015-05-11 | 2016-11-21 | 도쿄엘렉트론가부시키가이샤 | Plating method and recording medium |
| JP2016211044A (en) * | 2015-05-11 | 2016-12-15 | 東京エレクトロン株式会社 | Plating treatment method, and memory medium |
| US10224208B2 (en) | 2015-05-11 | 2019-03-05 | Tokyo Electron Limited | Plating method and recording medium |
Also Published As
| Publication number | Publication date |
|---|---|
| DE3486228D1 (en) | 1993-11-18 |
| BR8407027A (en) | 1985-07-30 |
| DE3486228T2 (en) | 1994-04-14 |
| EP0153369B1 (en) | 1993-10-13 |
| MX167978B (en) | 1993-04-26 |
| EP0153369A1 (en) | 1985-09-04 |
| HK1006860A1 (en) | 1999-03-19 |
| EP0153369A4 (en) | 1986-02-13 |
| WO1985001070A1 (en) | 1985-03-14 |
| CA1220101A (en) | 1987-04-07 |
| AU3217884A (en) | 1985-03-29 |
| AU558946B2 (en) | 1987-02-12 |
| JPH0319302B2 (en) | 1991-03-14 |
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