JPH05306471A - Method and device for forming copper electroless plating solution - Google Patents

Method and device for forming copper electroless plating solution

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Publication number
JPH05306471A
JPH05306471A JP3112893A JP11289391A JPH05306471A JP H05306471 A JPH05306471 A JP H05306471A JP 3112893 A JP3112893 A JP 3112893A JP 11289391 A JP11289391 A JP 11289391A JP H05306471 A JPH05306471 A JP H05306471A
Authority
JP
Japan
Prior art keywords
copper
solution
hydroxide
tank
copper hydroxide
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.)
Pending
Application number
JP3112893A
Other languages
Japanese (ja)
Inventor
Tatsuya Uchida
達也 内田
Juichi Kikuchi
寿一 菊池
Tokuhito Kikuhara
得仁 菊原
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Hitachi Chemical Techno Plant Ltd
Resonac Corp
Original Assignee
Hitachi Chemical Co Ltd
Hitachi Chemical Techno Plant Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Hitachi Chemical Co Ltd, Hitachi Chemical Techno Plant Ltd filed Critical Hitachi Chemical Co Ltd
Priority to JP3112893A priority Critical patent/JPH05306471A/en
Publication of JPH05306471A publication Critical patent/JPH05306471A/en
Pending legal-status Critical Current

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Abstract

PURPOSE:To form a copper electroless plating soln. not contg. an inhibiting ion and capable of supplying inexpensive and easily soluble copper hydroxide by using this device. CONSTITUTION:A copper hydroxide soln. is formed in a reaction settling tank 4 from an inexpensive copper source 1 and an alkaline soln. 2. The copper hydroxide soln. is separated by an ultrafilter 12 into a copper hydroxide soln. and a permeated liq. contg. an inhibiting ion. The copper hydroxide soln. is kept at a specified concn., mixed with an ethylenediamineacetic acid soln. or a preconditioned copper electroless plating soln. in a redissolution tank 15 and dissolved to form a copper electroless plating soln.

Description

【発明の詳細な説明】Detailed Description of the Invention

【0001】[0001]

【産業上の利用分野】本発明は、プリント配線基板やプ
ラスチック材料へ無電解銅めっきを行なう際の母液とな
る無電解銅めっき液の生成方法および生成装置に関す
る。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method and an apparatus for producing an electroless copper plating solution which is a mother liquor when electroless copper plating is performed on a printed wiring board or a plastic material.

【0002】[0002]

【従来の技術】従来、プリント配線基板やプラスチック
材料に無電解銅めっき処理を行なう無電解銅めっき液の
生成方法としては、無電解銅めっき浴に銅源としての硫
酸銅や塩化銅溶液を直接、もしくは予備溶解槽を設けて
間接的に添加する方法があり、最近では、特許第125
6876号に示されるように、酸化銅や水酸化銅の粉末
を予備溶解槽を設けて溶解させ、添加する方法も提案さ
れている。
2. Description of the Related Art Conventionally, as a method for producing an electroless copper plating solution for electroless copper plating on a printed wiring board or a plastic material, a copper sulfate or copper chloride solution as a copper source is directly added to an electroless copper plating bath. Alternatively, there is a method in which a preliminary dissolution tank is provided to add indirectly.
As disclosed in No. 6876, there is also proposed a method in which a powder of copper oxide or copper hydroxide is provided in a pre-melting tank to be melted and then added.

【0003】[0003]

【発明が解決しようとする課題】一般に、無電解銅めっ
き技術は、プリント配線基板に化学的に銅回路を形成し
たり、電子機器のプラスチックケースの内側にシールド
のために銅めっきを施す方法として、重要な技術である
が、一般的な銅源として用いられる硫酸銅や塩化銅に付
随して持ち込まれる硫酸イオンや塩素イオンの蓄積が、
めっき品質に悪影響を与え、また製造管理面から見て
も、安定した運転ができず、銅単独で添加する方式の開
発が望まれていた。
Generally, the electroless copper plating technique is used as a method of chemically forming a copper circuit on a printed wiring board or applying copper plating for shielding inside a plastic case of an electronic device. Although it is an important technology, the accumulation of sulfate ion and chloride ion brought in with copper sulfate and copper chloride used as a general copper source,
The plating quality is adversely affected, and stable operation cannot be performed from the viewpoint of manufacturing control, and development of a method of adding copper alone has been desired.

【0004】この対応策として、近年、阻害イオンを持
ち込まない方法として、微粉末の酸化銅や水酸化銅を用
いる方法が提案され、一部実行され始めた。しかし、こ
れらの方法は、銅源としての純度と容易にめっき液へ溶
解することが必要であることから、極めて高純度で、か
つ溶解しやすい微粉末のものを使用することが必須とな
り、製造費用的にも従来の薬品に比較し、高価でかつ取
り扱いが困難であるという問題点が指摘されている。本
発明は、このような事情に鑑みてなされたもので、本発
明の目的とするところは、硫酸イオン,塩素イオン等阻
害イオンを含まず、かつ廉価で溶解しやすい水酸化銅の
供給ができる無電解銅めっき液の生成方法および生成装
置を提供することにある。
As a countermeasure for this, in recent years, a method using finely powdered copper oxide or copper hydroxide has been proposed as a method for preventing the introduction of inhibitory ions, and a part thereof has begun to be implemented. However, since these methods require the purity as a copper source and the fact that they are easily dissolved in the plating solution, it is essential to use fine powders of extremely high purity and easy to dissolve. It has been pointed out that, in terms of cost, it is expensive and difficult to handle as compared with conventional chemicals. The present invention has been made in view of such circumstances, and an object of the present invention is to supply copper hydroxide that does not contain inhibitory ions such as sulfate ions and chloride ions and that is inexpensive and easily dissolved. An object of the present invention is to provide a method and an apparatus for producing an electroless copper plating solution.

【0005】[0005]

【課題を解決するための手段】上記目的を達成するため
に、本発明による無電解銅めっき液の生成方法は、反応
沈澱槽内で硫酸銅あるいは塩化銅等の銅源と、水酸化ナ
トリウムあるいは水酸化カリウム等のアルカリ性溶液と
を混合し、水酸化銅の懸濁性溶液を生成する水酸化銅の
生成工程と、循環槽内で、上記水酸化銅の懸濁溶液に純
水を添加しながら、限外瀘過装置に循環させ、阻外イオ
ンを含んだ瀘過液と水酸化銅溶液とに分離する水酸化銅
溶液の瀘過工程と、循環槽内の水酸化銅溶液を所定の濃
度に維持した後、再溶解槽に移送し、水酸化銅溶液とア
ルカリ性エチレンジアミン四酢酸溶液、もしくは予備調
整された無電解銅めっき液とを混合溶解する水酸化銅溶
液の再溶解工程とからなることを特徴とする。
In order to achieve the above object, the method for producing an electroless copper plating solution according to the present invention is a method of producing a copper source such as copper sulfate or copper chloride in a reaction precipitation tank and sodium hydroxide or Mixing with an alkaline solution such as potassium hydroxide to produce a copper hydroxide suspension solution, and adding pure water to the copper hydroxide suspension solution in a circulation tank. Meanwhile, the copper hydroxide solution is circulated in the ultrafiltration device, and the copper hydroxide solution is filtered through a filtration step in which the copper hydroxide solution is filtered into a filtration solution containing the exclusion ions and a copper hydroxide solution. After maintaining the concentration, it is transferred to a re-dissolving tank and consists of a re-dissolving step of a copper hydroxide solution in which a copper hydroxide solution and an alkaline ethylenediaminetetraacetic acid solution or a preconditioned electroless copper plating solution are mixed and dissolved. It is characterized by

【0006】更に、本発明による無電解銅めっき液の生
成装置は、硫酸銅あるいは塩化銅等の銅源と、アルカリ
性溶液とを混合し、水酸化銅を生成する反応沈澱槽と、
上記反応沈澱槽で生成した水酸化銅スラリーに純水を添
加しつつ、循環、瀘過する循環槽を並設した限外瀘過装
置と、循環槽内の水酸化銅スラリーに純水を供給する純
水槽と、限外瀘過装置で瀘過された水酸化銅溶液とアル
カリ性エレンジアミン四酢酸もしくは予備調整された無
電解銅めっき液とを混合して、水酸化銅溶液を再溶解さ
せる再溶解槽とからなることを特徴とする。
Further, the apparatus for producing an electroless copper plating solution according to the present invention comprises a reaction precipitation tank for producing a copper hydroxide by mixing a copper source such as copper sulfate or copper chloride with an alkaline solution.
While adding pure water to the copper hydroxide slurry produced in the reaction settling tank, supply ultrapure water to the copper hydroxide slurry in the circulation tank and an ultrafiltration device with a circulation tank installed side by side. Mix the deionized water tank with the copper hydroxide solution that has been filtered by the ultrafiltration device and the alkaline elenediamine tetraacetic acid or the preliminarily prepared electroless copper plating solution to re-dissolve the copper hydroxide solution. It is characterized by comprising a melting tank.

【0007】[0007]

【作用】本発明方法における作用を以下の化学反応式で
示す。 (1)無電解銅めっき浴における銅析出反応 CuEDTA(Na2)+2HCHO+4NaOH→C
u+H2+2H2O+2HCOONa+EDTA・Na 4 (2)水酸化銅生成反応(銅源はCuSO4とする) CuSO4+2NaOH→Cu(OH)2+Na2SO4 (3)水酸化銅再溶解反応 Cu(OH)2+EDTA・Na4→CuEDTA(2N
a)+2NaOH すなわち、(2)式の水酸化銅が(1)式の銅を析出で
失ったEDTA・Na 4で(3)式に従い、再び無電解
銅めっき浴の銅源となる。また、(2)式で生じる硫酸
ナトリウム(Na2SO4)は、限外濾過装置で透過水中
に他の不純物とともに排出され、高純度化される。
The action in the method of the present invention is represented by the following chemical reaction
Show. (1) Copper deposition reaction in electroless copper plating bath CuEDTA (Na2) + 2HCHO + 4NaOH → C
u + H2+ 2H2O + 2HCOONa + EDTA ・ NaFour (2) Copper hydroxide formation reaction (copper source is CuSOFourCuSOFour+ 2NaOH → Cu (OH)2+ Na2SOFour (3) Copper hydroxide re-dissolution reaction Cu (OH)2+ EDTA / NaFour→ CuEDTA (2N
a) + 2NaOH That is, the copper hydroxide of the formula (2) precipitates the copper of the formula (1).
Lost EDTA / Na FourIn accordance with equation (3), electroless again
It is the source of copper in the copper plating bath. In addition, sulfuric acid generated by the formula (2)
Sodium (Na2SOFour) Is permeated water with an ultrafiltration device
It is discharged together with other impurities and is highly purified.

【0008】[0008]

【実施例】以下、本発明の実施例について、図面に基づ
いて詳細に説明する。図1は本発明による無電解銅めっ
き液の生成方法を示すフローシートである。
Embodiments of the present invention will now be described in detail with reference to the drawings. FIG. 1 is a flow sheet showing a method for producing an electroless copper plating solution according to the present invention.

【0009】図面において、1は銅源であり、硫酸銅、
塩化銅、銅アンモニア化合物等を用いる。なお、プリン
ト配線基板産業においては、一般に塩化銅、硫酸による
エッチング廃水が多量に排出される関係でこれらが利用
でき、高純度の銅源は必要としない。次いで、符号2
は、銅源を水酸化銅とするための水酸化ナトリウムや水
酸化カリウム等のアルカリ性溶液である。これらをpH
調整装置3による制御下において、反応沈澱槽4内で攪
拌反応させ、固体の水酸化銅を生成する。このとき、水
酸化銅は攪拌をやめれば沈澱し、高濃度の水酸化銅スラ
リーとなる。反応は、連続式でも回分式でもどちらでも
選択できる。そして、この工程では、後段の限外濾過装
置への負荷を低減するためと、銅源に付随して持ち込ま
れる不純物を極力排除するため、上澄液は水酸化銅スラ
リーの流動に支障のない範囲で分離水6として、排水処
理装置(図示せず)により排出することが望ましい。ま
た、銅源としての銅の反応率は、アルカリ側pH制御下
ほぼ100%である。
In the drawing, 1 is a copper source, and copper sulfate,
Copper chloride, copper ammonia compound, etc. are used. In the printed wiring board industry, copper chloride and sulfuric acid are generally discharged in large amounts because they can be used, and a high-purity copper source is not required. Then, the code 2
Is an alkaline solution such as sodium hydroxide or potassium hydroxide for changing the copper source to copper hydroxide. PH these
Under the control of the adjusting device 3, the reaction is carried out with stirring in the reaction precipitation tank 4 to produce solid copper hydroxide. At this time, the copper hydroxide precipitates when the stirring is stopped and becomes a high-concentration copper hydroxide slurry. The reaction can be selected from either a continuous system or a batch system. In this step, the supernatant liquid does not hinder the flow of the copper hydroxide slurry in order to reduce the load on the subsequent ultrafiltration device and to eliminate impurities brought along with the copper source as much as possible. It is desirable to discharge the separated water 6 within a range by a waste water treatment device (not shown). Further, the reaction rate of copper as a copper source is almost 100% under alkali side pH control.

【0010】次に、反応沈澱槽4で得られた水酸化銅ス
ラリーを移送ポンプ5で限外濾過循環槽8に移送する。
このとき、移送したスラリー液に純水槽9から純水移送
ポンプ10で純水を供給し、混合することにより水酸化
銅の洗浄水とする。次いで、純水と水酸化銅スラリーの
混合液を限外濾過循環ポンプ11で限外濾過装置12に
供給、循環させる。ここで、水酸化銅は限外濾過膜で透
過を阻まれ系内を循環する。一方、水酸化銅スラリー中
に持ち込まれた硫酸イオン、塩素イオンや若干の有機物
のめっき阻害物質は、限外濾過装置12の濾過膜の透過
水13とともに系外へ排出される。ここにおいて、限外
濾過装置12の特徴である微粒子は、透過させないが、
イオンや低分子の有機物は透過させる性質を利用して水
酸化銅と不純物を分離することができる。なお、純水の
添加量は、水酸化銅が不溶性のため多いほど洗浄も良好
である。また、排出される透過水13は排水処理装置で
処理してもよいが、活性炭やイオン交換装置で再び純水
となし、純水槽9へ返送し再利用することも可能であ
る。
Next, the copper hydroxide slurry obtained in the reaction precipitation tank 4 is transferred to the ultrafiltration circulation tank 8 by the transfer pump 5.
At this time, pure water is supplied from the pure water tank 9 to the transferred slurry liquid by the pure water transfer pump 10 and mixed to form copper hydroxide cleaning water. Then, a mixed solution of pure water and copper hydroxide slurry is supplied to the ultrafiltration device 12 by the ultrafiltration circulation pump 11 and circulated. Here, the copper hydroxide is blocked by the ultrafiltration membrane and circulates in the system. On the other hand, sulfate ions, chlorine ions, and some organic substance plating-inhibiting substances brought into the copper hydroxide slurry are discharged out of the system together with the permeated water 13 of the filtration membrane of the ultrafiltration device 12. Here, the fine particles that are a feature of the ultrafiltration device 12 are not permeated,
Copper hydroxide and impurities can be separated by utilizing the property of allowing ions and low-molecular organic substances to permeate. The amount of pure water added is such that copper hydroxide is insoluble, and the cleaning is better. Further, the discharged permeated water 13 may be treated with a waste water treatment device, but it is also possible to make it into pure water again with activated carbon or an ion exchange device and return it to the pure water tank 9 for reuse.

【0011】一方、循環槽8内の水酸化銅濃度や濃縮倍
率は純水と水酸化銅スラリーの定量的な供給と限外濾過
装置12の透過水量および最終めっき液の銅濃度、供給
速度等の収支バランスを求めることにより設定できる。
尚、図2は、水酸化銅濃度と種々のメーカの限外濾過膜
の透水量を示すものである。濃度の上昇で透水量が減少
するが、添加純水量に応じた透水能力をもつ限外濾過装
置を備えることで、所定の濃度に維持することができ
る。次いで、循環槽8の洗浄された水酸化銅スラリーを
移送ポンプ14により間欠的または連続的に定量的に再
溶解槽15に移送する。そして、この再溶解槽15にお
いて、めっき液調整槽16の予め調整されたエチレンジ
アミン四酢酸溶液もしくは無電解銅めっき液を移送ポン
プ17で添加し、水酸化銅を溶解後、移送ポンプ18で
めっき浴19に供給する。
なお、符号20は洗浄用純水の持ち込み
により増量されためっき液のオーバーフローめっき液を
示し、符号21は、オーバーフローめっき液20から回
収されたエチレンジアミン四酢酸溶液を示す。
On the other hand, the concentration of copper hydroxide and the concentration ratio in the circulation tank 8 are quantitatively supplied with pure water and copper hydroxide slurry, the amount of permeated water of the ultrafiltration device 12, the copper concentration of the final plating solution, the supply rate, etc. It can be set by finding the balance of
Note that FIG. 2 shows the copper hydroxide concentration and the water permeation amount of the ultrafiltration membranes of various manufacturers. Although the amount of water permeation decreases as the concentration increases, it is possible to maintain a predetermined concentration by providing an ultrafiltration device having a water permeation capacity according to the amount of added pure water. Next, the washed copper hydroxide slurry in the circulation tank 8 is intermittently or continuously quantitatively transferred to the remelting tank 15 by the transfer pump 14. Then, in this re-dissolution tank 15, the ethylenediaminetetraacetic acid solution or the electroless copper plating solution adjusted in advance in the plating solution adjusting tank 16 is added by the transfer pump 17 to dissolve the copper hydroxide, and then the transfer pump 18 is used for the plating bath. Supply to 19.
Reference numeral 20 indicates an overflow plating solution of the plating solution increased by bringing in pure water for cleaning, and reference numeral 21 indicates an ethylenediaminetetraacetic acid solution recovered from the overflow plating solution 20.

【0012】次いで、図3は本発明による無電解銅めっ
き液の生成方法の第2実施例を示すもので、この実施例
においては、限外濾過装置として連続式フィルタープレ
ス22を用いている。尚、符号23は脱水EDTA移送
ポンプを示す。そして、第1実施例に比較し、フィルタ
ープレス脱水室での純水洗浄方式であるため、洗浄水量
の節減には寄与できるが、水酸化銅の回収率や脱水後水
酸化銅ケーキの移送ポンプの流動性、定量性に若干の問
題があるものの、本発明方法の特徴を妨げるものではな
い。ここにおいて、不純物を含む銅液から得られた水酸
化銅を純水により洗浄することにより高純度化し、無電
解銅めっき浴に銅源として供給することができる。
Next, FIG. 3 shows a second embodiment of the method for producing an electroless copper plating solution according to the present invention. In this embodiment, a continuous filter press 22 is used as an ultrafiltration device. Reference numeral 23 indicates a dehydration EDTA transfer pump. Further, compared with the first embodiment, since it is a pure water cleaning method in the filter press dehydration chamber, it can contribute to the reduction of the amount of cleaning water, but the copper hydroxide recovery rate and the transfer pump for the copper hydroxide cake after dehydration. Although there are some problems in the fluidity and quantification property of the above, it does not hinder the characteristics of the method of the present invention. Here, the copper hydroxide obtained from the copper solution containing impurities can be highly purified by washing with pure water and supplied to the electroless copper plating bath as a copper source.

【0013】次いで、本発明の具体的実施例を表1のバ
ランスシートにてその概略を示す。
Next, a concrete example of the present invention is schematically shown in the balance sheet of Table 1.

【0014】銅源として、硫酸銅溶液500l(硫酸と
過酸化水素水溶液の基板エッチング廃液)を用い、限外
濾過装置の濾過膜はB社製(米国ロミコン社製、HF6
6−43−PM−50)を用い、溶解液としてアルカリ
性EDTA液を用いた。槽容量は反応沈澱槽600l、
循環槽300l、純水槽4000l、再溶解槽2500
lに設定した。
As a copper source, a copper sulfate solution of 500 l (a substrate etching waste liquid of sulfuric acid and hydrogen peroxide solution) was used, and the filtration membrane of the ultrafiltration device was manufactured by Company B (Romicon, USA, HF6).
6-43-PM-50) and an alkaline EDTA solution was used as a solution. The tank capacity is 600 l of reaction precipitation tank,
Circulation tank 300l, pure water tank 4000l, re-dissolution tank 2500
set to 1.

【0015】[0015]

【表1】 [Table 1]

【0016】[0016]

【発明の効果】以上説明した通り、本発明による無電解
銅めっき液の生成方法および生成装置は、以下に記載す
る格別の作用効果を有する。 (1)本発明によれば、全工程中溶液で処理するため、
取り扱いが極めて容易である。 (2)本発明によれば、めっきに悪影響を与える銅源に
付随する同伴イオンや不純物の分離を限外濾過装置によ
り確実に行なえ、高純度化できる。また、これにより不
純物を含む安価な銅源が使用できる。 (3)本発明によれば、高純度化された含水水酸化銅ス
ラリーは、容易にめっき液中に溶解するため、めっき液
の管理等を簡単に行なえる等の効果を有する。
As described above, the method and apparatus for producing an electroless copper plating solution according to the present invention have the following special operational effects. (1) According to the present invention, since the treatment is performed with the solution in all steps,
It is extremely easy to handle. (2) According to the present invention, separation of entrained ions and impurities accompanying a copper source that adversely affects plating can be reliably performed by an ultrafiltration device, and high purity can be achieved. It also allows the use of cheap copper sources containing impurities. (3) According to the present invention, the highly purified water-containing copper hydroxide slurry is easily dissolved in the plating solution, so that the plating solution can be easily managed.

【図面の簡単な説明】[Brief description of drawings]

【図1】本発明における無電解銅めっき液の生成方法の
第1実施例を示すフローシート。
FIG. 1 is a flow sheet showing a first embodiment of a method for producing an electroless copper plating solution according to the present invention.

【図2】限外濾過装置に使用する各メーカの水酸化銅溶
液濃度と透過水量の測定結果を示すグラフ。
FIG. 2 is a graph showing the measurement results of copper hydroxide solution concentration and permeated water amount of each manufacturer used for the ultrafiltration device.

【図3】本発明による無電解銅めっき液の生成方法の第
2実施例を示すフローシート。
FIG. 3 is a flow sheet showing a second embodiment of the method for producing an electroless copper plating solution according to the present invention.

【符号の説明】[Explanation of symbols]

1 銅源 2 アルカリ性溶液 3 pH調整装置 4 反応沈澱槽 5 移送ポンプ 6 分離水 7 銅濃度計または懸濁物質濃度計 8 循環槽 9 純水槽 10 移送ポンプ 11 限外濾過循環ポンプ 12 限外濾過装置 13 限外濾過膜透過水 14 移送ポンプ 15 再溶解槽 16 めっき液調整槽 17,18 移送ポンプ 19 無電解銅めっき浴 20 オーバーフローめっき液 21 EDTA溶液 22 フィルタープレス 23 脱水EDTA移送ポンプ 1 Copper Source 2 Alkaline Solution 3 pH Adjuster 4 Reaction Precipitation Tank 5 Transfer Pump 6 Separation Water 7 Copper Concentration Meter or Suspended Substance Concentration Meter 8 Circulation Tank 9 Pure Water Tank 10 Transfer Pump 11 Ultrafiltration Circulation Pump 12 Ultrafiltration Equipment 13 Ultrafiltration Membrane Permeated Water 14 Transfer Pump 15 Redissolution Tank 16 Plating Solution Adjusting Tank 17, 18 Transfer Pump 19 Electroless Copper Plating Bath 20 Overflow Plating Solution 21 EDTA Solution 22 Filter Press 23 Dehydration EDTA Transfer Pump

───────────────────────────────────────────────────── フロントページの続き (72)発明者 菊原 得仁 東京都千代田区神田駿河台2丁目5番地の 4 日立化成テクノプラント株式会社内 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Tokuhito Kikuhara 2-5-5 Sugawada Kanda, Chiyoda-ku, Tokyo 4 Hitachi Chemical Techno Plant Co., Ltd.

Claims (3)

【特許請求の範囲】[Claims] 【請求項1】反応沈澱槽内で硫酸銅あるいは塩化銅等の
銅源と、水酸化ナトリウムあるいは水酸化カリウム等の
アルカリ性溶液とを混合し、水酸化銅の懸濁性溶液を生
成する水酸化銅の生成工程と、 循環槽内で、上記水酸化銅の懸濁溶液に純水を添加しな
がら、限外瀘過装置に循環させ、阻外イオンを含んだ瀘
過液と水酸化銅溶液とに分離する水酸化銅溶液の瀘過工
程と、 循環槽内の水酸化銅溶液を所定の濃度に維持した後、再
溶解槽に移送し、水酸化銅溶液とアルカリ性エチレンジ
アミン四酢酸溶液、もしくは予備調整された無電解銅め
っき液とを混合溶解する水酸化銅溶液の再溶解工程と、 からなることを特徴とする無電解銅めっき液の生成方
法。
1. A hydroxide which forms a suspension of copper hydroxide by mixing a copper source such as copper sulfate or copper chloride with an alkaline solution such as sodium hydroxide or potassium hydroxide in a reaction precipitation tank. In the copper production process, while adding pure water to the above-mentioned copper hydroxide suspension solution in the circulation tank, the solution is circulated through the ultrafiltration device, and the filtration solution containing the blocking ions and the copper hydroxide solution. And a filtration step of the copper hydroxide solution to separate into, and after maintaining the copper hydroxide solution in the circulation tank at a predetermined concentration, transferred to the re-dissolution tank, the copper hydroxide solution and the alkaline ethylenediaminetetraacetic acid solution, or A method for producing an electroless copper plating solution, which comprises: a step of re-dissolving a copper hydroxide solution in which a preliminarily prepared electroless copper plating solution is mixed and dissolved.
【請求項2】硫酸銅あるいは塩化銅等の銅源と、アルカ
リ性溶液とを混合し、水酸化銅を生成する反応沈澱槽
と、上記反応沈澱槽で生成した水酸化銅スラリーに純水
を添加しつつ、循環、瀘過する循環槽を並設した限外瀘
過装置と、循環槽内の水酸化銅スラリーに純水を供給す
る純水槽と、限外瀘過装置で瀘過された水酸化銅溶液と
アルカリ性エレンジアミン四酢酸もしくは予備調整され
た無電解銅めっき液とを混合して、水酸化銅溶液を再溶
解させる再溶解槽とからなることを特徴とする無電解銅
めっき液の生成装置。
2. A pure water is added to a reaction precipitation tank in which a copper source such as copper sulfate or copper chloride is mixed with an alkaline solution to produce copper hydroxide, and to the copper hydroxide slurry produced in the reaction precipitation tank. In the meanwhile, an ultrafiltration device in which a circulation tank for circulation and filtration is installed in parallel, a pure water tank for supplying pure water to the copper hydroxide slurry in the circulation tank, and the water filtered by the ultrafiltration device. Mixing a copper oxide solution and an alkaline elenediamine tetraacetic acid or a pre-prepared electroless copper plating solution, and a re-dissolving tank for re-dissolving a copper hydroxide solution Generator.
【請求項3】限外瀘過装置は、回分式もしくは連続式の
フィルタープレスであることを特徴とする請求項2記載
の無電解銅めっき液の生成装置。
3. The apparatus for producing an electroless copper plating solution according to claim 2, wherein the ultrafiltration apparatus is a batch type or continuous type filter press.
JP3112893A 1991-05-17 1991-05-17 Method and device for forming copper electroless plating solution Pending JPH05306471A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP3112893A JPH05306471A (en) 1991-05-17 1991-05-17 Method and device for forming copper electroless plating solution

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP3112893A JPH05306471A (en) 1991-05-17 1991-05-17 Method and device for forming copper electroless plating solution

Publications (1)

Publication Number Publication Date
JPH05306471A true JPH05306471A (en) 1993-11-19

Family

ID=14598147

Family Applications (1)

Application Number Title Priority Date Filing Date
JP3112893A Pending JPH05306471A (en) 1991-05-17 1991-05-17 Method and device for forming copper electroless plating solution

Country Status (1)

Country Link
JP (1) JPH05306471A (en)

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS56133455A (en) * 1980-03-24 1981-10-19 Hitachi Ltd Method for reducing amount of chemical copper plating solution
JPS56136968A (en) * 1980-03-27 1981-10-26 Hitachi Ltd Method and apparatus for selectively deionizing chemical copper plating bath
JPS5732360A (en) * 1980-08-07 1982-02-22 Hitachi Ltd Method and device for regeneration of chemical copper plating solution
JPS5932542A (en) * 1982-08-17 1984-02-22 Aisin Seiki Co Ltd Signal transmission device on steering operation board
JPS6326377A (en) * 1986-07-17 1988-02-03 Kanto Gakuin Device for regenerating plating solution
JPS6347371A (en) * 1986-08-15 1988-02-29 Nec Corp Device for regenerating chemical copper plating solution

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS56133455A (en) * 1980-03-24 1981-10-19 Hitachi Ltd Method for reducing amount of chemical copper plating solution
JPS56136968A (en) * 1980-03-27 1981-10-26 Hitachi Ltd Method and apparatus for selectively deionizing chemical copper plating bath
JPS5732360A (en) * 1980-08-07 1982-02-22 Hitachi Ltd Method and device for regeneration of chemical copper plating solution
JPS5932542A (en) * 1982-08-17 1984-02-22 Aisin Seiki Co Ltd Signal transmission device on steering operation board
JPS6326377A (en) * 1986-07-17 1988-02-03 Kanto Gakuin Device for regenerating plating solution
JPS6347371A (en) * 1986-08-15 1988-02-29 Nec Corp Device for regenerating chemical copper plating solution

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