JP3221083B2 - Electroplating method for aluminum and aluminum alloy plate - Google Patents
Electroplating method for aluminum and aluminum alloy plateInfo
- Publication number
- JP3221083B2 JP3221083B2 JP23938892A JP23938892A JP3221083B2 JP 3221083 B2 JP3221083 B2 JP 3221083B2 JP 23938892 A JP23938892 A JP 23938892A JP 23938892 A JP23938892 A JP 23938892A JP 3221083 B2 JP3221083 B2 JP 3221083B2
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- JP
- Japan
- Prior art keywords
- aluminum
- plating
- alloy plate
- aluminum alloy
- electroplating
- 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.)
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- Electroplating Methods And Accessories (AREA)
- ing And Chemical Polishing (AREA)
Description
【０００１】[0001]
【産業上の利用分野】この発明は、アルミニウムおよび
アルミニウム合金板上への電気めっき方法、特に密着性
に優れためっき皮膜を得ることができる、アルミニウム
およびアルミニウム合金板の電気めっき方法に関するも
のである。BACKGROUND OF THE INVENTION This invention can be obtained electroplating method, plating film particularly excellent in adhesion to aluminum contact and the aluminum alloy plate, relates electroplating method of an aluminum and aluminum alloy plate It is.
【０００２】[0002]
【従来の技術】自動車および家電用として、冷延鋼板お
よび表面処理鋼板が広く使用されているが、近年、比重
が鉄と比べて1/3 と大幅に小さいアルミニウムおよびア
ルミニウム合金板の使用が、軽量化および耐食性の向上
を図る目的で検討されている。しかし、アルミニウムお
よびアルミニウム合金板（以下、単にアルミニウム板と
称す）に使用目的に適った機能を付与するためには、こ
れに表面処理を施す場合が多い。表面処理法としては、
陽極酸化処理や化成処理等の他にめっき処理がある。め
っき処理の場合、酸化され易いアルミニウム板表面に直
接電気めっきを施すと、アルミニウム板素地との間に充
分な密着が得られずめっき皮膜の剥離が避けられない。2. Description of the Related Art As for automobiles and home appliances, but cold rolled steel and coated steel sheets are widely used in recent years, specific gravity is the use of one-third and much smaller aluminum and aluminum alloy plate as compared with iron It is being studied for the purpose of reducing weight and improving corrosion resistance. However, aluminum and aluminum alloy plate (hereinafter, simply aluminum plate and <br/> referred) for imparting functions expedient for the intended use is often subjected to this surface treatment. As the surface treatment method,
There is plating treatment other than anodic oxidation treatment and chemical conversion treatment. If the plating process, when subjected to direct electroplating to easily aluminum plate surface is oxidized, is unavoidable peeling of the plating film is not sufficient adhesion is obtained between the aluminum plate containing areas.
【０００３】このため、従来、アルミニウム板表面を活
性化する予備処理の後一度Ｚｎの置換めっきを行い、そ
の上に目的金属のめっきを施していた。例えば、特開平
3-130375号公報では、脱脂洗浄後化学酸による活性化の
予備処理を行い、1 分間のＺｎ置換を施し、その上に銅
めっきを施すが、添加剤の工夫により平滑性・密着性の
良いめっ皮膜が得られることを開示している。[0003] Therefore, conventionally, is performed once displacement plating of Zn after the pretreatment to activate the aluminum plate table surface, it was plated with target metal thereon. For example,
In 3-130375, pre-treatment of activation with a chemical acid is performed after degreasing and washing, Zn substitution is performed for 1 minute, and copper plating is performed thereon, but smoothness and adhesion are improved by devising additives. It discloses that an overcoat is obtained.
【０００４】一方、アルミニウム板に直接めっきする方
法も提案されている。例えば。特開昭63-166964 号公報
には、蒸着法によって亜鉛めっきをアルミニウム板の表
面に形成する方法が開示されおり、又、特開平 3-10489
5 号公報には、電気めっき法によりパルス通電を行い表
面酸化物層を溶解した後、めっき通電を行い密着性に優
れためっき皮膜を得る方法が開示されている。On the other hand, a method of directly plating an aluminum plate has also been proposed. For example. JP-A-63-166964 discloses a method of forming zinc plating on the surface of an aluminum plate by a vapor deposition method.
No. 5 discloses a method in which a pulse current is applied by an electroplating method to dissolve the surface oxide layer, and then the plating is applied to obtain a plating film having excellent adhesion.
【０００５】[0005]
【発明が解決しようとする課題】しかしながら、蒸着法
は大きく且つ複雑な設備を要し、又、パルスめっき法は
一部の金属へのめっき或いは溶融塩電解などではその効
果がみられるが、アルミニウム板に水溶液めっきを施す
場合は充分なめっき密着性が得られない。そして、Ｚｎ
置換処理法は実用的であるが、作業工程が多く、且つ処
理に時間を要し特に連続処理では生産性に劣るという問
題があった。However, the vapor deposition method requires large and complicated facilities, and the pulse plating method is effective in plating some metals or electrolyzing molten salt. When an aqueous solution plating is applied to a plate , sufficient plating adhesion cannot be obtained. And Zn
Although the substitution treatment method is practical, there are problems that the number of work steps is large and that the treatment requires a long time, and that the productivity is poor particularly in continuous treatment.
【０００６】この発明の目的は、上記の問題を解決する
ため、即ち作業工程や設備の複雑さを回避し且つ密着性
に優れためっき皮膜を得ることができる電気めっき方法
を提供することにある。An object of the present invention is to solve the above-mentioned problems, that is, to provide an electroplating method capable of avoiding the complexity of working steps and equipment and obtaining a plating film having excellent adhesion. .
【０００７】[0007]
【課題を解決するための手段】この目的は、次の手段に
よって達成される。即ち、アルミニウムおよびアルミニ
ウム合金板の表面を脱脂洗浄後、弗素化合物を溶解させ
ためっき液を用いて電気めっきを行うアルミニウム及び
アルミニウム合金板の電気めっき方法であって、より好
ましくは前記弗素化合物を、弗素量換算で１０ppm 以上
溶解させためっき液を用いることであり、又、前記電気
めっきを行うに際して通電開始直前に無通電浸漬を行
い、引き続いて通電を開始すること、更に、この無通電
浸漬時間が０．１秒以上であることが一層望ましい。This object is achieved by the following means. That is, aluminum and aluminum
After degreasing the surface of um alloy plate, using a plating solution prepared by dissolving a fluorine compound be an aluminum and electroplating method of an aluminum alloy plate for performing electroplating, more preferably the fluorine compound, a fluorine amount conversion It is to use a plating solution in which 10 ppm or more is dissolved.In addition, when performing the electroplating, the non-energized immersion is performed immediately before the energization is started, and the energization is subsequently started. It is more desirable that the time be equal to or longer than seconds.
【０００８】[0008]
【作用】水溶液を用いる電気めっきや化学めっきは大仰
な設備を必要とせず、その基本技術は広く工業上の経験
も豊富な技術である。しかし、アルミニウム板にこれら
の処理を施そうとすると、その表層に生成された酸化物
が種々の問題を引き起こす。アルミニウムは、よく知ら
れているように酸素親和力の大きな金属で、大気中の酸
素や水中に溶存する酸素と常温においても容易に酸化物
を生成する。ジンケート処理と称される化学めっき処理
や電気めっき処理において、従来は、アルミニウム板を
脱脂洗浄した後、めっきを施す前に弗酸を含む酸水溶液
で酸洗し表面に生成した酸化膜を除去することがよく行
われていた。しかしながら、この酸洗工程で酸化膜は一
旦除去されるが、水溶液からなるめっき液に浸されると
再び酸化されてしまう。[Effect] Electroplating and chemical plating using an aqueous solution do not require large facilities, and their basic technology is a technology with a wide range of industrial experience. However, when you Hodokoso these processes the aluminum plate, oxides generated on the surface layer causes various problems. Aluminum is a metal having a high oxygen affinity, as is well known, and easily forms an oxide at room temperature with oxygen in the atmosphere or oxygen dissolved in water. Conventionally, in a chemical plating process or an electroplating process called a zincate process, an aluminum plate is degreased and washed, and then, before plating, is pickled with an aqueous acid solution containing hydrofluoric acid to remove an oxide film formed on the surface. Things were done well. However, the oxide film is once removed in this pickling step, but is oxidized again when immersed in a plating solution composed of an aqueous solution.
【０００９】一方、弗酸を始め弗素化合物には金属酸化
物を溶解する作用のあることが知られ、チタンやジルコ
ン、アルミニウム等の酸素親和力の大きな金属の酸化膜
除去に用いられている。On the other hand, fluorine compounds such as hydrofluoric acid are known to have a function of dissolving metal oxides, and are used for removing oxide films of metals having a high oxygen affinity such as titanium, zircon and aluminum.
【００１０】このような成分を、めっき液に含ませるこ
とによって酸化物の再生成を防ぐことができよう。発明
者らはこの考えに基づき、弗素化合物の他の作用即ちめ
っきへの悪影響にも注意を払いながら、酸化物との関係
を究明した。その結果、弗素化合物には、めっき液中に
あっても酸化物の再生成を防ぐ作用だけではなく、酸化
物を溶解除去する作用もあることを突き止めた。[0010] By including such a component in the plating solution, regeneration of the oxide could be prevented. Based on this idea, the inventors have investigated the relationship with oxides while paying attention to the other effect of the fluorine compound, that is, the adverse effect on plating. As a result, it was found that the fluorine compound not only functions to prevent the oxide from being regenerated even in the plating solution but also functions to dissolve and remove the oxide.
【００１１】この知見をアルミニウム板のめっきに適用
すると次のようになる。アルミニウム板の場合、めっき
前の表面状況は一般に酸化物が薄く膜状に生成されてい
ると共に、多かれ少なかれ油脂類等の汚れが付着してい
る。この汚れは一般に、めっき前処理として脱脂洗浄処
理によって除かれる。この発明においても、この汚れに
よりめっき液が汚染されることを防ぐために、脱脂洗浄
を前以て行う。次に、めっき皮膜の密着性を確保するた
めに、酸化物を除去しなければならないが、この酸化物
はめっき液に弗素化合物を添加しておけば、めっき液中
で溶解し除去するこができる。言い換えれば、酸化物を
除去するために、めっき前処理として弗化物を含む酸洗
処理を独立して設ける必要はない。又、このようにし
て、めっき液中で酸化物を除去しても、そのためにめっ
きに悪影響を及ぼす現象は見当たらなかった。When this finding is applied to the plating of an aluminum plate, the following is obtained. In the case of an aluminum plate, the surface condition before plating is generally such that oxides are thinly formed in a film form and more or less stains such as oils and fats are attached. This stain is generally removed by a degreasing cleaning treatment as a plating pretreatment. Also in the present invention, in order to prevent the plating solution from being contaminated by the dirt, degreasing cleaning is performed in advance. Next, in order to ensure the adhesion of the plating film, the oxide must be removed, but this oxide can be dissolved and removed in the plating solution if a fluorine compound is added to the plating solution. it can. In other words, it is not necessary to independently provide a pickling treatment containing fluoride as a pretreatment for plating in order to remove the oxide. In addition, even if the oxide was removed in the plating solution in this manner, no adverse effect on plating was found.
【００１２】めっき液中での酸化物の除去については、
弗素化合物の量があまりに少ないと除去に時間を要す
る。電気めっきにおいて、酸化物やその他のアルミニウ
ム化合物等アルミニウム金属以外の物質が表面に残留し
たままめっき金属が電析すると、アルミニウムとめっき
金属との間に直接の結合が得られず、良好なめっき密着
性は得られない。したがって、電析が始まる前に酸化物
が除去されていることが好ましく、この観点からめっき
液に添加する弗素化合物もある程度多い方がよい。添加
量を変えてめっきを施し、めっき皮膜の密着性を尺度に
してその必要量を調べた結果、弗素イオン或いは弗素錯
イオンとして１０ppm 以上の濃度で存在すると、短時間
で酸化物が除去されて密着性が確保されることが判っ
た。Regarding the removal of oxides in the plating solution,
If the amount of the fluorine compound is too small, it takes time to remove. In electroplating, if the plating metal is electrodeposited while substances other than aluminum metal such as oxides and other aluminum compounds remain on the surface, a direct bond cannot be obtained between aluminum and the plating metal, resulting in good plating adhesion Sex is not obtained. Therefore, it is preferable that the oxide is removed before the start of the electrodeposition, and from this viewpoint, it is better that the fluorine compound added to the plating solution is somewhat large. The required amount was examined by measuring the adhesion of the plating film by changing the amount of addition, and as a result, the oxide was removed in a short time when it was present at a concentration of 10 ppm or more as fluoride ions or fluoride complex ions. It was found that the adhesion was secured.
【００１３】更に、慎重を期すならば、充分に酸化物を
除去した後に電析を開始するとよい。この場合、アルミ
ニウム板をめっき液に浸漬した後０．１秒以上を経てめ
っき電流の通電を開始する手法が効果的である。Further, if care is taken, it is advisable to start the electrodeposition after sufficiently removing the oxide. In this case, a method of starting energization of the plating current 0.1 seconds or more after immersing the aluminum plate in the plating solution is effective.
【００１４】添加する弗素化合物は、めっき液中で溶解
し、イオン化するものならなんでも良い。例えば、弗素
イオンを生成する化合物としては、弗化水素酸、弗化ア
ンモン、弗化ソーダ等が挙げられ、弗化化合物イオンを
放出するものとしては、硼弗化アンモン、硼弗化水素
酸、チタン弗化アンモン、チタン弗化水素酸等が挙げら
れる。The fluorine compound to be added is not particularly limited as long as it dissolves and ionizes in the plating solution. Examples of the compound generating a fluorine ion, hydrofluoric acid, ammonium fluoride, sodium fluoride and the like, and those which release fluoride compound ion, borofluoride ammonium, the boron hydrofluoric acid, Titanium ammonium fluoride, titanium hydrofluoric acid and the like can be mentioned.
【００１５】[0015]
【実施例】次に、この発明を実施例によって、さらに詳
細に説明する。マグネシウムを4.5 wt% 含有したアルミ
ニウム合金板と純アルミニウム板とを、80℃、40g/l の
オルソケイ酸ソーダ中で10秒間、10A/dm2 の条件で電解
脱脂を行った。次いで、水洗し、酸洗を行わずにめっき
液に浸漬し通電時間を変えて電気めっきを行った。施し
ためっきは亜鉛めっき、亜鉛−鉄合金めっき（鉄含有量
80wt% ) およびニッケルめっきで、付着量は２０g/m2を
目標とした。めっき後試験片を折り曲げ、曲げ部のめっ
き皮膜の密着性を調べた。Next, the present invention will be described in more detail by way of examples. An aluminum alloy plate containing 4.5 wt% of magnesium and a pure aluminum plate were subjected to electrolytic degreasing in a 40 g / l sodium orthosilicate at 80 ° C. for 10 seconds at 10 A / dm 2 . Next, the plate was washed with water, immersed in a plating solution without performing acid washing, and electroplating was performed while changing the energizing time. The applied plating is zinc plating, zinc-iron alloy plating (iron content
80 wt%) and nickel plating, and the adhesion amount was targeted at 20 g / m 2 . After plating, the test piece was bent, and the adhesion of the plating film at the bent portion was examined.
【００１６】めっき条件については、めっき流速が２ｍ
／秒、温度が５０℃、そして、電流密度が４５A/dm2 、
弗素化合物を除いためっき液の基本組成は次のＡ，Ｂ，
Ｃである。 Ａ：ＺｎＳＯ4 ・７Ｈ2Ｏ ４００g/l Ｈ2 ＳＯ4 １００g/l pH ２．０ Ｂ：ＺｎＳＯ4 ・７Ｈ2Ｏ ２０g/l ＦｅＳＯ4 ・７Ｈ2Ｏ １００g/l pH ２．０ Ｃ：ＮｉＣｌ2 ・６Ｈ2Ｏ ４５g/l ＮｉＳＯ4 ・７Ｈ2Ｏ ２４０g/l Ｈ3ＢＯ4 ３０g/l pH ２．０Regarding the plating conditions, the plating flow rate is 2 m
/ Sec, temperature 50 ° C, current density 45A / dm 2 ,
The basic composition of the plating solution excluding the fluorine compound is as follows: A, B,
C. A: ZnSO 4 · 7H 2 O 400g / l H 2 SO 4 100g / l pH 2.0 B: ZnSO 4 · 7H 2 O 20g / l FeSO 4 · 7H 2 O 100g / l pH 2.0 C: NiCl 2 · 6H 2 O 45g / l NiSO 4 · 7H 2 O 240g / l H 3 BO 4 30g / l pH 2.0
【００１７】密着性の調査は、ＪＩＳ-Ｚ２２４８に規
定される曲げ試験を行い折り曲げ部のめっき面に粘着テ
ープを張りつけこれを強制的に剥離し、その剥離状況を
調べた。曲げ試験では、試験片の厚さの等倍（１ｔ）又
は４倍（４ｔ）の曲率半径に沿って試験片を１８０°折
り曲げた。４ｔの場合に剥離が生じなければ実用上問題
が無いが、密着性の評価は次の４段階で行った。◎：１
ｔで全く剥離を生ぜず、〇：４ｔで全く剥離を生ぜず、
△：４ｔで剥離、×：４ｔで１８０°折り曲げる以前に
剥離し、非常に密着性に劣る。For the examination of adhesion, a bending test specified in JIS-Z2248 was carried out, an adhesive tape was stuck on the plated surface of the bent portion, and this was forcibly peeled off, and the peeling state was examined. In the bending test, the test piece was bent at 180 ° along a radius of curvature equal to (1 t) or four times (4 t) the thickness of the test piece. In the case of 4t, if there is no peeling, there is no practical problem, but the evaluation of adhesion was performed in the following four stages. ◎: 1
No peeling occurred at t, Δ: No peeling occurred at 4t,
Δ: Peeled off at 4t, ×: Peeled off before bending at 180 ° at 4t, very poor adhesion.
【００１８】なお、比較のために、めっき前に酸洗を行
い酸化物を除去した後、弗素化合物を添加しないめっき
液で電気めっきを施したものについても密着性を調べ
た。この場合の酸洗条件は次のＷ，Ｘ，Ｙ，Ｚの４種で
ある。 Ｗ：Ｈ2 ＳＯ4 ５０g/l 液温 ５０℃ 浸漬時間 １０秒 Ｘ：Ｈ2 ＳＯ4 ５０g/l ＮａＦ ５０g/l 液温 ５０℃ 浸漬時間 １０秒 Ｙ：Ｈ2 ＳＯ4 ５０g/l ＮａＦ ５０g/l 液温 ５０℃ カソード電解電流 １０A/dm2 電解時間 １０秒 Ｚ：ＨＣｌ ５０g/l ＨＮＯ3 ５０g/l 液温 ５０℃ 浸漬時間 １０秒。 これらの製造条件と密着性調査の結果をまとめて表１に
示す。For comparison, the adhesion was also examined for an electrode that had been subjected to pickling prior to plating to remove oxides and then electroplated with a plating solution containing no fluorine compound. The pickling conditions in this case are the following four types of W, X, Y and Z. W: H 2 SO 4 50 g / l Liquid temperature 50 ° C. Immersion time 10 seconds X: H 2 SO 4 50 g / l NaF 50 g / l Liquid temperature 50 ° C. Immersion time 10 seconds Y: H 2 SO 4 50 g / l NaF 50 g / l l Solution temperature 50 ° C Cathode electrolysis current 10A / dm 2 Electrolysis time 10 seconds Z: HCl 50g / l HNO 3 50g / l Solution temperature 50 ° C Immersion time 10 seconds. Table 1 summarizes these manufacturing conditions and the results of the adhesion investigation.
【００１９】[0019]
【表１】 [Table 1]
【００２０】この発明の実施例では、めっき皮膜の密着
性は全て実用に耐えるものであったが、酸洗前処理で酸
化物を除去してもめっき液中に弗素化合物を添加しなか
った比較例では、満足なめっき密着性が得られなかっ
た。In the examples of the present invention, the adhesion of the plating film was all practically acceptable, but even if the oxide was removed by the pretreatment for pickling, no fluorine compound was added to the plating solution. In the example, satisfactory plating adhesion was not obtained.
【００２１】[0021]
【発明の効果】以上説明したように、この発明によれ
ば、めっき液中に弗素化合物を添加しているので、前処
理として酸洗を行わずとも密着性に優れためっき皮膜を
得ることができ、処理工程が極めて簡素化された。更
に、電気めっきの前段に時間のかかる亜鉛置換処理を施
す必要もなくなり、生産性を飛躍的に高めたこの発明の
効果は大きい。As described above, according to the present invention, since the fluorine compound is added to the plating solution, a plating film having excellent adhesion can be obtained without performing pickling as a pretreatment. The process has been greatly simplified. Further, it is not necessary to perform a time-consuming zinc substitution treatment prior to the electroplating, and the effect of the present invention that dramatically improves productivity is great.
フロントページの続き (72)発明者 鷺山 勝 東京都千代田区丸の内一丁目１番２号 日本鋼管株式会社内 審査官 日比野 隆治 (56)参考文献 特開 平５−65691（ＪＰ，Ａ) (58)調査した分野(Int.Cl.7，ＤＢ名) C25D 3/44 C25D 5/44 Continuation of the front page (72) Inventor Masaru Sagiyama 1-2-1 Marunouchi, Chiyoda-ku, Tokyo Examiner, Nippon Kokan Co., Ltd. Takaharu Hibino (56) References JP-A-5-65691 (JP, A) (58) Field surveyed (Int. Cl. 7 , DB name) C25D 3/44 C25D 5/44
Claims (4)
の表面を脱脂洗浄後、弗素化合物を溶解させためっき液
を用いて電気めっきを行うことを特徴とするアルミニウ
ムおよびアルミニウム合金板の電気めっき方法。1. A aluminum and degreased cleaning the surface of the aluminum alloy plate, aluminum and electroplating method of an aluminum alloy plate and performing electroplating using a plating solution prepared by dissolving a fluorine compound.
上溶解させためっき液を用いることを特徴とする請求項
１記載のアルミニウムおよびアルミニウム合金板の電気
めっき方法。Wherein the fluorine compound, aluminum and electroplating method of an aluminum alloy plate 請 Motomeko 1 wherein Rukoto using a plating solution obtained by dissolving 10ppm or more fluorine equivalence.
に無通電浸漬を行い、引き続いて通電を開始することを
特徴とする請求項１又は請求項２記載のアルミニウムお
よびアルミニウム合金板の電気めっき方法。3. performs unpowered immersed in energized immediately before when performing electroplating, that you initiate energization subsequently
請 Motomeko 1 or claim 2 aluminum and electroplating method of an aluminum alloy plate, wherein.
徴とする請求項３記載のアルミニウムおよびアルミニウ
ム合金板の電気めっき方法。4. JP-free current dip line Ukoto 0.1 seconds
請 Motomeko 3 aluminum and electroplating method of an aluminum alloy plate according to symptoms.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP23938892A JP3221083B2 (en) | 1991-09-09 | 1992-09-08 | Electroplating method for aluminum and aluminum alloy plate |
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3-258380 | 1991-09-09 | ||
| JP25838091 | 1991-09-09 | ||
| JP23938892A JP3221083B2 (en) | 1991-09-09 | 1992-09-08 | Electroplating method for aluminum and aluminum alloy plate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH05195282A JPH05195282A (en) | 1993-08-03 |
| JP3221083B2 true JP3221083B2 (en) | 2001-10-22 |
Family
ID=26534220
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP23938892A Expired - Fee Related JP3221083B2 (en) | 1991-09-09 | 1992-09-08 | Electroplating method for aluminum and aluminum alloy plate |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3221083B2 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104328466A (en) * | 2014-07-30 | 2015-02-04 | 国家电网公司 | Aluminum alloy silver-plating pre-treatment method |
-
1992
- 1992-09-08 JP JP23938892A patent/JP3221083B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH05195282A (en) | 1993-08-03 |
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