JPH0741957A - Method for regenerating electroless copper plating solution - Google Patents
Method for regenerating electroless copper plating solutionInfo
- Publication number
- JPH0741957A JPH0741957A JP20374893A JP20374893A JPH0741957A JP H0741957 A JPH0741957 A JP H0741957A JP 20374893 A JP20374893 A JP 20374893A JP 20374893 A JP20374893 A JP 20374893A JP H0741957 A JPH0741957 A JP H0741957A
- Authority
- JP
- Japan
- Prior art keywords
- plating solution
- copper
- electroless copper
- copper plating
- solution
- 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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Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、繰り返し使用後の無電
解銅メッキ液の再生方法に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for regenerating an electroless copper plating solution after repeated use.
【０００２】[0002]
【従来の技術】無電解銅メッキは、例えば磁器コンデン
サの如きセラミック電子部品の外部電極、プリント配線
板の導体部やプラスチックの表面を銅膜で覆う手段とし
て用いられている。このような無電解銅メッキは、銅イ
オン、還元剤及び錯化剤を主成分に含む無電解銅メッキ
液に被処理物を浸漬して処理するものであるが、銅イオ
ン供給源として硫酸銅、還元剤としてホルマリン、錯化
剤として酒石酸塩を用いた水酸化ナトリウム溶液の無電
解銅メッキ液を使用した場合には、次の反応により銅イ
オンが還元されて金属銅が被処理物表面に沈着する。2. Description of the Related Art Electroless copper plating is used as a means for covering external electrodes of ceramic electronic parts such as porcelain capacitors, conductors of printed wiring boards and surfaces of plastics with a copper film. Such electroless copper plating is performed by immersing an object to be treated in an electroless copper plating solution containing copper ions, a reducing agent and a complexing agent as main components, and copper sulfate is used as a copper ion supply source. When an electroless copper plating solution of sodium hydroxide solution using formalin as a reducing agent and tartrate as a complexing agent is used, copper ions are reduced by the following reaction and metallic copper is deposited on the surface of the object to be treated. To deposit.
【０００３】ＣｕＳＯ4 ＋２ＨＣＨＯ＋４ＮａＯＨ＝Ｃ
ｕ＋Ｈ2 ＋２Ｈ2 Ｏ＋２ＨＣＯＯＮａ＋Ｎａ2 ＳＯ4 この際、錯化剤は触媒として作用し、メッキ処理により
消費されるのはＣｕ++、ＨＣＨＯ及びＮａＯＨであるの
で、メッキ液中に硫酸銅、ホルマリン及び水酸化ナトリ
ウムを補充しながらメッキ処理を繰り返し行なうことが
行われている。CuSO 4 + 2HCHO + 4NaOH = C
u + H 2 + 2H 2 O + 2HCOONa + Na 2 SO 4 At this time, since the complexing agent acts as a catalyst and Cu ++ , HCHO and NaOH are consumed by the plating treatment, copper sulfate, formalin and hydroxide are contained in the plating solution. The plating process is repeatedly performed while supplementing sodium.
【０００４】しかしながら、繰り返し回数が多くなれ
ば、メッキ液中にギ酸ナトリウム（ＨＣＯＯＮａ）やボ
ウ硝（Ｎａ2 ＳＯ4 ）が蓄積してメッキ処理能力がなく
なり、使用できなくなる。このような繰り返し使用後の
無電解銅メッキ液は老化廃液として処理されるが、その
まま野外に投棄すると、その投棄場所によっては環境を
害する問題を起こすことと、資源の有効利用をはかる観
点から、この老化廃液の一部を再生利用することも行わ
れている。However, if the number of times of repetition increases, sodium formate (HCOONa) or glauber's salt (Na 2 SO 4 ) accumulates in the plating solution and the plating treatment capacity is lost, making it unusable. The electroless copper plating solution after such repeated use is treated as an aging waste solution, but if it is dumped outdoors as it is, it causes a problem that harms the environment depending on the dumping location, and from the viewpoint of effective use of resources, It is also practiced to recycle a part of this aging waste liquid.
【０００５】例えば、無電解銅メッキ液の老化廃液をイ
オン交換膜を使用した電気透析により再生することが行
われている。この方法は、陽極と陰極を備えた電気透析
槽に一対の対向させたアニオン交換膜のそれぞれを各電
極側に配置して設け、このアニオン交換膜間に無電解銅
メッキ液の老化廃液を入れて両電極に電圧を印加する。
これにより、アニオン成分を陽極側に移動させ高濃度化
させて外部に取り出し、アニオン交換膜間にはカチオン
成分を残してその溶液を再度メッキ槽に戻して循環使用
するものである。このようにすると、ギ酸と硫酸イオン
は循環系から除かれるので、ホルマリンと硫酸銅をメッ
キ槽に補充することにより無電解銅メッキ処理を繰り返
し行なうことができる。For example, an aging waste solution of an electroless copper plating solution is regenerated by electrodialysis using an ion exchange membrane. In this method, an electrodialysis tank equipped with an anode and a cathode is provided with a pair of opposed anion exchange membranes arranged on each electrode side, and an aging waste liquid of an electroless copper plating solution is placed between the anion exchange membranes. Voltage is applied to both electrodes.
As a result, the anion component is moved to the anode side so as to have a high concentration and taken out to the outside, and the cation component is left between the anion exchange membranes, and the solution is returned to the plating tank for reuse. In this way, formic acid and sulfate ions are removed from the circulation system, so that the electroless copper plating treatment can be repeated by supplementing the plating bath with formalin and copper sulfate.
【０００６】[0006]
【発明が解決しようとする課題】しかしながら、上記の
ような再生処理によって必要成分を循環使用する点は良
いが、ギ酸やボウ硝のような濃縮物は不要物であるの
で、産業廃棄物として処理しなければならず、環境問題
の本質的な解決にはならない。However, it is good that the necessary components are recycled by the above-mentioned regeneration treatment, but since concentrates such as formic acid and Glauber's salt are unnecessary substances, they are treated as industrial wastes. Must be done and does not become an essential solution to environmental problems.
【０００７】本発明の目的は、老化廃液の生じ難い、使
用済無電解銅メッキ液の再生方法を提供することにあ
る。An object of the present invention is to provide a method for regenerating a used electroless copper plating solution in which aging waste liquid is unlikely to occur.
【０００８】[0008]
【課題を解決するための手段】本発明は、上記課題を解
決するために、銅イオン、ホルムアルデヒド、及び酒石
酸塩を含有する無電解銅メッキ液の使用にともなって消
費したホルムアルデヒド及び銅イオンを補給することに
より繰り返し使用した該無電解銅メッキ液の再生方法で
あって、該繰り返し使用後の無電解銅メッキ液中のギ酸
イオンを選択的に電気分解処理する工程を有し、上記銅
イオンの補給は酸化銅、金属銅の少なくとも１種の添加
により行なう無電解銅メッキ液の再生方法を提供するも
のである。In order to solve the above problems, the present invention replenishes the formaldehyde and copper ions consumed with the use of an electroless copper plating solution containing copper ions, formaldehyde, and tartrate. A method of regenerating the electroless copper plating solution repeatedly used by, comprising the step of selectively electrolyzing the formate ion in the electroless copper plating solution after the repeated use, Replenishment provides a method for regenerating an electroless copper plating solution by adding at least one of copper oxide and metallic copper.
【０００９】[0009]
【作用】繰り返し使用後のホルムアルデヒドの消費に伴
って生じたギ酸を含有する無電解銅メッキ液を電気分解
処理すると、ギ酸根は下記式のように分解され、水と炭
酸ガスになり、炭酸ガスは揮散し、水は無害物として残
る。 ＨＣＯＯ- →ＣＯ2 ＋Ｈ+ ＋２ｅ Ｈ+ ＋ＯＨ- →Ｈ2 Ｏ これにより、メッキ液の機能を低下させるギ酸を選択的
にメッキ液から減少させることができる。一方、硫酸イ
オンはそのまま残るが、酸化銅、金属銅の少なくとも１
種を加えることによりこれらの対イオンとなるので、ボ
ウ硝として蓄積することを避けることができる。[Function] When the electroless copper plating solution containing formic acid generated by the consumption of formaldehyde after repeated use is electrolyzed, the formic acid radicals are decomposed into water and carbon dioxide as shown in the following formula. Volatilizes and the water remains as a harmless substance. HCOO − → CO 2 + H + + 2e H + + OH − → H 2 O As a result, formic acid that deteriorates the function of the plating solution can be selectively reduced from the plating solution. On the other hand, sulfate ions remain, but at least 1 of copper oxide and metallic copper
By adding seeds, these counterions are formed, so that accumulation as Glauber's salt can be avoided.
【００１０】[0010]
【実施例】次に本発明の実施例を図面に基づいて説明す
る。 実施例１ 図１中、１はメッキ槽であり、次の組成の無電解銅メッ
キ液が１００ｍｌ収容されている。 ＣｕＳＯ4 ・５Ｈ2 Ｏ １５ｇ／ｌ ＨＣＨＯ水溶液（３５％濃度） １０ｍｌ／ｌ ＮａＯＨ １２ｇ／ｌ ロッシェル塩 ４０ｇ／ｌ （酒石酸カリウムナトリウム） 水 ｌEmbodiments of the present invention will now be described with reference to the drawings. Example 1 In FIG. 1, 1 is a plating tank, which contains 100 ml of an electroless copper plating solution having the following composition. CuSO 4 .5H 2 O 15 g / l HCHO aqueous solution (35% concentration) 10 ml / l NaOH 12 g / l Rochelle salt 40 g / l (potassium sodium tartrate) water l
【００１１】一方磁器素体（ＢａＴｉＯ3 の焼成体から
なる直径８ｍｍ、厚さ０．２ｍｍのコンデンサ素体）の
両端に外部電極を形成するために、その両端面をＳｎＣ
ｌ2液（４ｇのＳｎＣｌ2 を１ｌの０．５Ｎ ＨＣｌに
溶かした溶液）に室温、１０分浸漬した後、さらに同様
にＰｄＣｌ2 液（０．４ｇのＰｄＣｌ2 を１ｌの０．５
Ｎ ＨＣｌに溶かした液）に室温、１０分浸漬し、活性
化処理を行なう。On the other hand, in order to form external electrodes at both ends of a porcelain body (capacitor body made of a fired body of BaTiO 3 and having a diameter of 8 mm and a thickness of 0.2 mm), both end surfaces of the porcelain body are made of SnC.
After being immersed in a solution of l 2 (a solution of 4 g of SnCl 2 dissolved in 1 l of 0.5N HCl) at room temperature for 10 minutes, a PdCl 2 solution (0.4 g of PdCl 2 of 0.5 g of 1 l of 0.5 was also added).
The solution is immersed in a solution (dissolved in N HCl) at room temperature for 10 minutes for activation treatment.
【００１２】このような活性化処理を行ったものを５０
個用意し、上記メッキ浴に浸漬し、常温で２０分撹拌す
ることにより無電解銅メッキ処理を行った。次にその処
理物を取り出した後、銅イオン濃度検出装置（発光分光
分析装置）によりＣｕ++濃度を測定してその測定値に基
づいて予めＮａＯＨ溶液に溶解させたＣｕ2 Ｏ溶液を当
初のメッキ液のＣｕ++濃度からの不足分としてＣｕ2 Ｏ
に換算して８．４ｇ補給するとともに、試薬Ｎａ2 ＳＯ
3 とＨ2 Ｏを用いる滴定法によりホルムアルデヒドの濃
度を測定してその測定値に基づき当初のメッキ液のホル
ムアルデヒド濃度からの不足分として３５％ＨＣＨＯ液
８．６ｃｃを上記使用済メッキ液に加え、さらにＮａＯ
Ｈを加えながら撹拌し、メッキ液のｐＨを１３に調整し
た。この後、上記と同様に活性化処理を行った磁器素体
５０個をこのメッキ液に浸漬し、上記と同様にして無電
解銅メッキ処理を行った。このようなメッキ処理をさら
に８回繰り返し行なって、全部で１０回の無電解銅メッ
キ処理を行なった。その繰り返し使用後のメッキ液を用
いて上記と同様にメッキ処理を行なったが、一部メッキ
の付着しないものが発生した。A product which has been subjected to such activation treatment is 50
Individually prepared, immersed in the above plating bath, and stirred at room temperature for 20 minutes to perform electroless copper plating. Next, after taking out the treated product, the Cu ++ concentration was measured by a copper ion concentration detection device (emission spectroscopic analysis device), and based on the measured value, the Cu 2 O solution previously dissolved in the NaOH solution was used as the initial solution. Cu 2 O as a deficit from the Cu ++ concentration of the plating solution
8.4g in addition to the reagent Na 2 SO
The concentration of formaldehyde was measured by a titration method using 3 and H 2 O, and 8.6 cc of 35% HCHO solution was added to the above used plating solution as a deficiency from the original formaldehyde concentration of the plating solution based on the measured value. Further NaO
The mixture was stirred while adding H to adjust the pH of the plating solution to 13. After that, 50 porcelain bodies that had been activated in the same manner as above were immersed in this plating solution and subjected to electroless copper plating in the same manner as above. Such plating treatment was further repeated 8 times to perform a total of 10 electroless copper plating treatments. The plating treatment was repeated in the same manner as above using the plating solution after repeated use, but some plating did not adhere.
【００１３】図中、２は電気分解槽であり、中央に設け
たアニオン交換膜３（アニオン成分を通過させカチオン
成分を通過させない膜）により区画された両側に白金か
らなる陽極４、陰極５（対向面積１０ｃｍ2 、両極間の
距離５ｃｍ）がそれぞれ設けられ、これらには外部から
電圧が印加されるようになっている。この電気分解槽２
の陽極側の区画６に上記老化廃液とみなされるメッキ液
を収容し、両電極間に電圧を印加して６，５００クーロ
ンの電流を流し、電気分解を行なった。この電気分解を
行なう前後のギ酸を定量した結果は次のとおりであっ
た。 電気分解を行う前（１０回使用）のメッキ液のギ酸量 １ｍｏｌ／ｌ 電気分解を行った後のメッキ液のギ酸量 ０．１ｍｏｌ／ｌIn the figure, reference numeral 2 denotes an electrolysis tank, which is divided by an anion exchange membrane 3 (a membrane that allows anion components to pass and a cation component does not pass) provided in the center, and an anode 4 and a cathode 5 made of platinum on both sides ( A facing area of 10 cm 2 and a distance between both poles of 5 cm) are provided, and a voltage is applied to them externally. This electrolysis tank 2
The plating solution regarded as the above-mentioned aging waste solution was housed in the compartment 6 on the anode side of No. 3, and a voltage of 6,500 Coulomb was applied by applying a voltage between both electrodes to carry out electrolysis. The results of quantifying formic acid before and after this electrolysis were as follows. Formic acid amount of plating solution before electrolysis (used 10 times) 1 mol / l Formic acid amount of plating solution after electrolysis 0.1 mol / l
【００１４】また、酒石酸根の上記電気分解を行う前後
の定量分析の結果は次のとおりであった。 電気分解する前の酒石酸根の初期値 ４０ｇ／ｌ 電気分解した後の酒石酸根の測定値 ３８．８ｇ／ｌ なお、ギ酸、酒石酸根の分析法はイオンクロマトグラフ
ィーを用いた。The results of the quantitative analysis before and after the above-mentioned electrolysis of tartaric acid roots were as follows. Initial value of tartaric acid root before electrolysis 40 g / l Measured value of tartaric acid root after electrolysis 38.8 g / l In addition, ion chromatography was used for the analysis method of formic acid and tartaric acid root.
【００１５】電気分解処理をしたメッキ液はメッキ槽１
に戻し、上記と同様にしてＣｕ++及びＨＣＨＯの定量を
行ない、メッキ処理を行なう前の当初のメッキ液のそれ
ぞれの濃度からの不足分をＣｕ2 ＯのＮａＯＨ液及び３
５％ＨＣＨＯ液により補給し、上記と同様に磁器素体５
０個に無電解銅メッキ処理を行ったところ、上記と同様
に所定の銅色の銅メッキがなされたことが確認された。
同じメッキ液を用い、上記と同様にＣｕ++及びＨＣＨＯ
の補給を行いながら、上記と同様に磁器素体５０個に無
電解銅メッキ処理を行うことを７回繰り返し行ったがい
ずれも所定の銅メッキ処理がなされたことを確認した。
この７回使用後のメッキ液についても上記と同様に電気
分解処理を行ない、上記と同様に繰り返し使用すること
ができた。このようにしてメッキ液は電気分解処理を行
うことによって繰り返し循環使用することができ、この
間廃液を生じないようにすることができる。The electrolyzed plating solution is the plating tank 1
Then, quantification of Cu ++ and HCHO is carried out in the same manner as above, and the deficiency from the respective concentrations of the original plating solution before performing the plating treatment is adjusted to the Cu 2 O NaOH solution and 3
Replenish with 5% HCHO liquid, and porcelain body 5 as above
When zero electroless copper plating treatment was performed, it was confirmed that a predetermined copper color copper plating was performed in the same manner as above.
Using the same plating solution, Cu + + and HCHO as above
While the above replenishment was performed, 50 electroless copper plating treatments were repeated 7 times in the same manner as described above, and it was confirmed that the predetermined copper plating treatment was performed in each case.
The plating solution after 7 times of use was also electrolyzed in the same manner as above, and could be repeatedly used in the same manner as above. In this way, the plating solution can be repeatedly circulated and used by performing the electrolysis treatment, and the waste solution can be prevented from being generated during this period.
【００１６】上記はメッキ液のＣｕ++の不足分をＣｕ2
Ｏにより補給したが、その他の酸化銅、金属銅あるいは
これらの混合物を補給しても良い。また、上記はアニオ
ン交換膜を使用したが、カチオン交換膜でも良く、これ
らの交換膜は電気分解槽の中央に離間して複数設け、そ
の間に処理対象物を収容するようにしても良い。In the above, the shortage of Cu ++ in the plating solution is replaced by Cu 2
Although supplemented with O, other copper oxide, metallic copper, or a mixture thereof may be supplemented. Further, although the anion exchange membrane is used in the above, a cation exchange membrane may be used, and a plurality of these exchange membranes may be provided separately in the center of the electrolysis tank, and the object to be treated may be accommodated therebetween.
【００１７】[0017]
【発明の効果】本発明によれば、銅イオン、ホルムアル
デヒド、酒石酸塩を含有する無電解銅メッキ液の銅イオ
ンの消費に伴う不足分を酸化銅、金属銅の少なくとも１
種により補給したので、硫酸イオンを増やすことなく銅
イオンを補給することができ、老化物としてのボウ硝を
蓄積させることがないとともに、老化メッキ液を電気分
解処理することにより、酒石酸塩を分解することなく、
ホルムアルデヒドの使用に伴って生じるギ酸根を選択的
に分解して炭酸ガスと水とにし無害化したので、銅イオ
ン及びホルムアルデヒドの不足分を追加することにより
老化メッキ液は再生され、メッキ液として繰り返し再使
用することができ、廃液を生じないようにすることがで
きる。According to the present invention, the deficiency associated with the consumption of copper ions in the electroless copper plating solution containing copper ions, formaldehyde and tartrate is at least one of copper oxide and metallic copper.
Since it was replenished by seeds, it is possible to replenish copper ions without increasing sulfate ions, do not accumulate Glauber's salt as an aging substance, and decompose the tartrate salt by electrolyzing the aging plating solution. Without doing
Formic acid radicals generated by the use of formaldehyde were selectively decomposed into carbon dioxide gas and water to make them harmless.By adding a shortage of copper ions and formaldehyde, the aging plating solution was regenerated and repeatedly used as a plating solution. It can be reused and waste liquid can be avoided.
【図１】本発明の方法の１実施例の概略工程図である。FIG. 1 is a schematic process diagram of one embodiment of the method of the present invention.
１ メッキ槽 ２ 電気分解槽 ４ 陽極 ５ 陰極 1 Plating tank 2 Electrolysis tank 4 Anode 5 Cathode
Claims (1)
酸塩を含有する無電解銅メッキ液の使用にともなって消
費したホルムアルデヒド及び銅イオンを補給することに
より繰り返し使用した該無電解銅メッキ液の再生方法で
あって、該繰り返し使用後の無電解銅メッキ液中のギ酸
イオンを選択的に電気分解処理する工程を有し、上記銅
イオンの補給は酸化銅、金属銅の少なくとも１種の添加
により行なう無電解銅メッキ液の再生方法。1. A method of regenerating an electroless copper plating solution, which is repeatedly used by replenishing formaldehyde and copper ions consumed with the use of an electroless copper plating solution containing copper ions, formaldehyde, and tartrate. Therefore, there is a step of selectively electrolyzing the formate ions in the electroless copper plating solution after the repeated use, and the copper ions are supplied by adding at least one of copper oxide and metallic copper. Regeneration method of electrolytic copper plating solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP20374893A JPH0741957A (en) | 1993-07-27 | 1993-07-27 | Method for regenerating electroless copper plating solution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP20374893A JPH0741957A (en) | 1993-07-27 | 1993-07-27 | Method for regenerating electroless copper plating solution |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0741957A true JPH0741957A (en) | 1995-02-10 |
Family
ID=16479196
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP20374893A Pending JPH0741957A (en) | 1993-07-27 | 1993-07-27 | Method for regenerating electroless copper plating solution |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0741957A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7495241B2 (en) | 2004-02-26 | 2009-02-24 | Tdk Corporation | Ion beam irradiation apparatus and insulating spacer for the same |
| JP2011514936A (en) * | 2008-03-12 | 2011-05-12 | マクダーミッド インコーポレーテッド | Method of electrolytically dissolving nickel in electroless nickel plating solution |
-
1993
- 1993-07-27 JP JP20374893A patent/JPH0741957A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7495241B2 (en) | 2004-02-26 | 2009-02-24 | Tdk Corporation | Ion beam irradiation apparatus and insulating spacer for the same |
| JP2011514936A (en) * | 2008-03-12 | 2011-05-12 | マクダーミッド インコーポレーテッド | Method of electrolytically dissolving nickel in electroless nickel plating solution |
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