JP2003064437A - HIGH PURITY Ni ALLOY ANODE MATERIAL FOR ELECTROLYTIC Ni PLATING EXHIBITING HIGH PLATING YIELD - Google Patents
HIGH PURITY Ni ALLOY ANODE MATERIAL FOR ELECTROLYTIC Ni PLATING EXHIBITING HIGH PLATING YIELDInfo
- Publication number
- JP2003064437A JP2003064437A JP2001251151A JP2001251151A JP2003064437A JP 2003064437 A JP2003064437 A JP 2003064437A JP 2001251151 A JP2001251151 A JP 2001251151A JP 2001251151 A JP2001251151 A JP 2001251151A JP 2003064437 A JP2003064437 A JP 2003064437A
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- Prior art keywords
- plating
- purity
- anode material
- electrolytic
- alloy
- 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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- Electrolytic Production Of Metals (AREA)
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Abstract
Description
【発明の詳細な説明】
【０００１】
【発明の属する技術分野】この発明は、電解Ｎｉめっき
処理に際して、高いめっき歩留、すなわち使用寿命の延
命化を可能とし、この結果陽極材の交換回数の減少をも
たらすことから、電解めっき装置のＦＡ化に寄与するほ
か、低コスト化を可能とする高純度Ｎｉ合金陽極材に関
するものである。
【０００２】
【従来の技術】例えば近年の半導体装置などの製造に
は、高純度Ｎｉ薄膜の形成が不可欠であり、またこの高
純度Ｎｉ薄膜の形成は、陽極材として９９．９９質量％
以上の高純度を有するＮｉを用い、電解めっき法により
行なわれている。
【０００３】
【発明が解決しようとする課題】一方、近年の電解めっ
き装置のＦＡ化および高純度Ｎｉ薄膜形成の低コスト化
の面から、高純度Ｎｉ陽極材にはめっき歩留の向上、す
なわち使用寿命の一段の延命化、さらに述べれば高純度
Ｎｉ陽極材１個当たりの高純度Ｎｉ薄膜の形成割合の向
上が常に求められているのが現状である。
【０００４】
【課題を解決するための手段】そこで、本発明者等は、
上述のような観点から、上記の電解Ｎｉめっき用高純度
Ｎｉ陽極材に着目し、これのめっき歩留の向上を図るべ
く研究を行った結果、
（ａ）一般に電解Ｎｉめっき処理においては、電解液中
での高純度Ｎｉ陽極材からのＮｉの溶出を一定にするた
めに、前記陽極材には常に一定の電流、例えば２Ａ／ｄ
ｍ2が流れるように負荷電圧を制御しており、したがっ
て前記負荷電圧は前記電極材からのＮｉ溶出によって変
化する表面性状に対応して上昇するものであり、例えば
１．３Ｖの初期負荷電圧（めっき開始５分後の電圧）が
約２．５Ｖに上昇した時点で電極材の使用寿命としてい
ること。
（ｂ）一方、上記陽極材からのＮｉの溶出は、樹枝状に
進行し、最終的に前記陽極材は海綿状になり、例えば約
２．５Ｖの負荷電圧は電極材の海綿状態様を示すもので
あり、この時点で使用寿命としているが、それは、ここ
でさらにめっきを続行すると負荷電圧が急激に上昇し、
陰極であるめっき面で加水分解が起り、この加水分解で
発生した水素と酸素のうち特に水素がＮｉめっき薄膜内
に巻き込まれ、ピンホールとして存在して薄膜特性を著
しく害うようになるという理由によるものであること。
（ｃ）９９．９９質量％以上の純度を有する高純度Ｎｉ
に、合金成分として、ＳｉおよびＡｌを、それぞれ、
Ｓｉ：４０〜３００ｐｐｍ、
Ａｌ：４０〜３００ｐｐｍ、
の割合で含有させてなる高純度Ｎｉ合金を電解Ｎｉめっ
きの陽極材として用いると、電解Ｎｉめっき処理中の前
記陽極材からのＮｉの溶出形態が微細化、すなわち電解
Ｎｉめっき初期の樹枝状溶出形態および同最終期の海綿
状溶出形態が微細化し、これによって陽極材における負
荷電圧の上昇が著しく抑制され、相対的に長時間に亘っ
てのめっき処理が可能となることから、めっき歩留が向
上し、相対的に電極材当たりのめっき処理量が増大する
ようになること。
以上（ａ）〜（ｃ）に示される研究結果を得たのであ
る。
【０００５】この発明は、上記の研究結果に基づいてな
されたものであって、９９．９９質量％以上の純度を有
する高純度Ｎｉに、合金成分として、ＳｉおよびＡｌ
を、それぞれ、
Ｓｉ：４０〜３００ｐｐｍ、
Ａｌ：４０〜３００ｐｐｍ、
の割合で共存含有させてなる高純度Ｎｉ合金で構成し
た、高いめっき歩留を示す電解Ｎｉめっき用高純度Ｎｉ
合金陽極材に特徴を有するものである。
【０００６】なお、この発明の高純度Ｎｉ合金陽極材を
構成する高純度Ｎｉ合金において、ＳｉおよびＡｌには
上記の通り共存含有した状態で電解めっき処理中の電極
材の溶出態様を著しく微細化し、もってめっき電圧の上
昇を抑制して、使用寿命の長期化に寄与する作用があ
り、したがってＳｉおよびＡｌのいずれかしか含有しな
い場合や、前記両成分を含有してもそのいずれかの含有
量が４０ｐｐｍ未満であったりする場合には前記作用に
所望の効果が得られず、一方その含有量がＳｉおよびＡ
ｌのいずれかでも３００ｐｐｍを越えると、陽極材表面
からのＮｉの電解液中への溶出が抑制されるようにな
り、これがめっき電圧上昇の原因となり、相対的に使用
寿命の短命化、すなわちめっき歩留の低下をもたらすよ
うになることから、その含有量を、それぞれＳｉ：４０
〜３００ｐｐｍ、Ａｌ：４０〜３００ｐｐｍと定めた。
また、高純度Ｎｉの純度は上記の通り９９．９９質量％
以上の高純度とすることは不可欠の要件であって、９
９．９９質量％未満の純度ではＮｉめっき薄膜の特性が
低下し、例えば半導体装置に適用することができなくな
るからである。
【０００７】
【発明の実施の形態】つぎに、この発明の高純度Ｎｉ合
金陽極材を実施例により具体的に説明する。電熱式溶解
るつぼで、それぞれ表１に示される純度の高純度Ｎｉを
真空溶解し、これにＮｉ―Ｓｉ合金およびＮｉ−Ａｌ合
金の形で、それぞれ４０〜３００ｐｐｍの範囲内の所定
の量のＳｉおよびＡｌを添加含有させて高純度Ｎｉ合金
を溶製し、直径：１００ｍｍ×長さ：１２０ｍｍのイン
ゴットに鋳造し、これに１１００℃の温度で熱間鍛造を
施して幅：１２５ｍｍ×厚さ：２３ｍｍの板材とした
後、さらに冷間圧延を施して幅：１２５ｍｍ×厚さ：１
０ｍｍの冷延板とし、さらにこれに４５０〜７５０℃の
範囲内の温度に１時間保持の条件で再結晶化熱処理を施
して、それぞれ表１に示される平均結晶粒径とし、つい
でこれより長さ：１００ｍｍ×幅：５０ｍｍ×厚さ：１
０ｍｍの寸法に切り出し、最終的に面削加工にて厚さ：
７．５ｍｍとすることにより、それぞれ表１に示される
ＳｉおよびＡｌ含有量の本発明高純度Ｎｉ合金陽極材
（以下、本発明陽極材という）１〜１２をそれぞれ製造
した。
【０００８】また、比較の目的で、同じく表１に示され
る通りＳｉおよびＡｌのうちの少なくともいずれかの含
有量がこの発明の範囲から外れた以外は同一の条件で比
較高純度Ｎｉ合金陽極材（以下、比較陽極材という）１
〜６をそれぞれ製造した。
【０００９】ついで、この結果得られた本発明陽極材１
〜１２および比較陽極材１〜６について、脱脂および酸
洗処理した状態で、撹拌羽根付き電解めっき槽に装入
し、
陰極材：無酸素銅、
電解液：塩化ニッケル：５ｇ／ｌ、スルファミン酸ニッ
ケル：３５０ｇ／ｌ、ほう酸：４０ｇ／ｌ、界面活性剤
０．０６ｇ／ｌ、を含有し、ｐＨ：４．０のスルファミ
ン酸溶液、
電解液の温度:５５℃、
電流密度：２Ａ／ｄｍ2、
の条件で上記陰極材の表面にＮｉめっきを施すめっき試
験を行ない、めっき中の表示電圧が２．５Ｖ（２．５Ｖ
の表示電圧は陰極材表面で加水分解が起る電圧である）
に上昇するまでのめっき時間を測定した。
【００１０】
【表１】
【００１１】
【発明の効果】表１に示される結果から、ＳｉおよびＡ
ｌ含有量がいずれも４０〜３００ｐｐｍである本発明陽
極材１〜１２は、いずれも長いめっき時間を示し、これ
は電解Ｎｉめっき処理に際して、陽極材が高いめっき歩
留を示すことを意味するのに対して、比較陽極材１〜６
に見られるようにＳｉおよびＡｌのうちの少なくともい
ずれかの含有量がこの発明の範囲から外れると、相対的
にめっき時間は短いものとなり、陽極材のめっき歩留の
向上は困難であることが明らかである。上述のように、
この発明の高純度Ｎｉ合金陽極材は、電解Ｎｉめっき処
理に際して、高いめっき歩留、すなわち使用寿命の延命
化を可能とし、この結果陽極材の交換回数の減少をもた
らすことから、電解めっき装置のＦＡ化に寄与するほ
か、低コスト化も可能とするなど工業上有用な効果をも
たらすものである。Description: BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention enables a high plating yield, that is, a prolonged service life in electrolytic Ni plating, and as a result, the number of replacements of the anode material is reduced. The present invention relates to a high-purity Ni alloy anode material that contributes to FA of an electroplating apparatus because of its reduction, and also enables cost reduction. 2. Description of the Related Art For example, in recent years, the production of semiconductor devices and the like requires the formation of a high-purity Ni thin film, and the formation of this high-purity Ni thin film requires 99.99% by mass as an anode material.
It is performed by electrolytic plating using Ni having the above high purity. [0003] On the other hand, in view of the recent trend toward the use of FA in an electrolytic plating apparatus and the reduction in cost of forming a high-purity Ni thin film, a high-purity Ni anode material has an improved plating yield, At present, it is always required to further extend the service life, and more specifically, to improve the formation ratio of a high-purity Ni thin film per high-purity Ni anode material. [0004] Accordingly, the present inventors have proposed:
From the above-mentioned viewpoints, focusing on the above-mentioned high-purity Ni anode material for electrolytic Ni plating and conducting research to improve the plating yield thereof, (a) In general, in electrolytic Ni plating, In order to keep the elution of Ni from the high-purity Ni anode material in the liquid constant, the anode material always has a constant current, for example, 2 A / d.
The load voltage is controlled so that m 2 flows. Therefore, the load voltage rises in accordance with the surface texture that changes due to the elution of Ni from the electrode material. For example, an initial load voltage of 1.3 V ( (5 minutes after the start of plating) rises to about 2.5 V, which indicates that the service life of the electrode material is reached. (B) On the other hand, the elution of Ni from the anode material proceeds in a dendritic manner, and finally the anode material becomes spongy. For example, a load voltage of about 2.5 V indicates the sponge state of the electrode material. At this point, the service life is reached, but if the plating is continued further here, the load voltage rises sharply,
Hydrolysis occurs on the plating surface, which is the cathode, and the hydrogen and oxygen generated by the hydrolysis are particularly caught in the Ni plating thin film, which is present as pinholes and significantly impairs the thin film characteristics. It is due to. (C) High-purity Ni having a purity of 99.99% by mass or more
When a high-purity Ni alloy containing Si and Al as alloy components at a ratio of Si: 40 to 300 ppm and Al: 40 to 300 ppm is used as an anode material for electrolytic Ni plating, electrolytic Ni plating The dissolution form of Ni from the anode material during the treatment is finer, that is, the dendritic dissolution form at the initial stage of electrolytic Ni plating and the spongy dissolution form at the final stage are finer, whereby the load voltage on the anode material is significantly increased. Since the plating process is suppressed for a relatively long time, the plating yield is improved, and the plating process amount per electrode material is relatively increased. The research results shown in (a) to (c) above were obtained. The present invention has been made on the basis of the above-mentioned research results, and it has been proposed that high purity Ni having a purity of 99.99 mass% or more is added to Si and Al as alloy components.
Of high purity Ni for electrolytic Ni plating exhibiting a high plating yield, which is composed of a high purity Ni alloy coexisting at a ratio of Si: 40 to 300 ppm and Al: 40 to 300 ppm, respectively.
It has characteristics in the alloy anode material. In the high-purity Ni alloy constituting the high-purity Ni alloy anode material of the present invention, the elution mode of the electrode material during the electroplating process is remarkably reduced while Si and Al coexist as described above. Therefore, it has the effect of suppressing the increase in plating voltage and contributing to prolonging the service life. Therefore, when only one of Si and Al is contained, and even when both of the above components are contained, the content of either of them is contained. If the content is less than 40 ppm, the desired effect cannot be obtained in the above-mentioned action, while the content of Si and A
If any one exceeds 300 ppm, the elution of Ni from the anode material surface into the electrolytic solution is suppressed, which causes an increase in plating voltage and relatively shortens the service life, that is, plating. Since the yield is lowered, the content is set to Si: 40, respectively.
３００300 ppm, Al: 40-300 ppm.
The purity of high-purity Ni is 99.99% by mass as described above.
High purity is an essential requirement,
If the purity is less than 9.99% by mass, the characteristics of the Ni-plated thin film are deteriorated and, for example, it cannot be applied to a semiconductor device. Next, the high-purity Ni alloy anode material of the present invention will be specifically described with reference to examples. In an electrothermal melting crucible, high-purity Ni having the purity shown in Table 1 was vacuum-melted, and a predetermined amount of Si in the range of 40 to 300 ppm was obtained in the form of a Ni-Si alloy and a Ni-Al alloy. And Al are added and melted to produce a high-purity Ni alloy, cast into an ingot having a diameter of 100 mm and a length of 120 mm, and subjected to hot forging at a temperature of 1100 ° C. to have a width of 125 mm and a thickness of: After making a plate material of 23 mm, it is further subjected to cold rolling to obtain a width: 125 mm × thickness: 1
0 mm cold-rolled sheet, and further subjected to recrystallization heat treatment at a temperature in the range of 450 to 750 ° C. for 1 hour to obtain an average grain size shown in Table 1, and then to a longer length. Length: 100mm x width: 50mm x thickness: 1
Cut out to a size of 0mm and finally thickness by facing:
By adjusting the thickness to 7.5 mm, high purity Ni alloy anode materials of the present invention (hereinafter, referred to as the present invention anode materials) 1 to 12 having the Si and Al contents shown in Table 1 were respectively manufactured. [0008] For comparison purposes, as shown in Table 1, comparative high-purity Ni alloy anode material under the same conditions except that the content of at least one of Si and Al is out of the range of the present invention. (Hereinafter referred to as comparative anode material) 1
To 6 were each manufactured. Next, the resulting anode material 1 of the present invention was obtained.
-12 and the comparative anode materials 1-6 were degreased and pickled, placed in an electrolytic plating tank with stirring blades, cathode material: oxygen-free copper, electrolyte solution: nickel chloride: 5 g / l, sulfamic acid Nickel: 350 g / l, boric acid: 40 g / l, surfactant: 0.06 g / l, pH: 4.0, sulfamic acid solution, temperature of electrolyte: 55 ° C., current density: 2 A / dm 2 A plating test was performed in which Ni plating was performed on the surface of the cathode material under the conditions of (1) and (2), and the display voltage during plating was 2.5 V (2.5 V).
Is the voltage at which hydrolysis occurs on the cathode material surface)
The plating time until the temperature rose was measured. [Table 1] According to the results shown in Table 1, Si and A
Each of the anode materials 1 to 12 of the present invention having a l content of 40 to 300 ppm shows a long plating time, which means that the anode material shows a high plating yield in electrolytic Ni plating treatment. In contrast, the comparison anode materials 1-6
As seen from the above, if the content of at least one of Si and Al is out of the range of the present invention, the plating time becomes relatively short, and it is difficult to improve the plating yield of the anode material. it is obvious. As mentioned above,
The high-purity Ni alloy anode material of the present invention enables a high plating yield, that is, a prolonged service life in electrolytic Ni plating treatment, and as a result, reduces the number of replacements of the anode material. Besides contributing to FA, it also has industrially useful effects such as enabling cost reduction.
Claims (1)
純度Ｎｉに、合金成分として、ＳｉおよびＡｌを、それ
ぞれ、 Ｓｉ：４０〜３００ｐｐｍ、 Ａｌ：４０〜３００ｐｐｍ、 の割合で含有させてなる高純度Ｎｉ合金で構成したこと
を特徴とする高いめっき歩留を示す電解Ｎｉめっき用高
純度Ｎｉ合金陽極材。Claims 1. A high-purity Ni having a purity of 99.99% by mass or more, in which Si and Al are added as alloy components to Si: 40 to 300 ppm and Al: 40 to 300 ppm, respectively. A high-purity Ni alloy anode material for electrolytic Ni plating exhibiting a high plating yield, characterized in that the anode material is constituted by a high-purity Ni alloy contained in a proportion.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001251151A JP3985130B2 (en) | 2001-08-22 | 2001-08-22 | High purity Ni alloy anode material for electrolytic Ni plating showing high plating yield |
| TW92103699A TWI255869B (en) | 2001-08-22 | 2003-02-21 | Ni alloy as an anode for Ni electroplating |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001251151A JP3985130B2 (en) | 2001-08-22 | 2001-08-22 | High purity Ni alloy anode material for electrolytic Ni plating showing high plating yield |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2003064437A true JP2003064437A (en) | 2003-03-05 |
| JP3985130B2 JP3985130B2 (en) | 2007-10-03 |
Family
ID=19079842
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2001251151A Expired - Fee Related JP3985130B2 (en) | 2001-08-22 | 2001-08-22 | High purity Ni alloy anode material for electrolytic Ni plating showing high plating yield |
Country Status (2)
| Country | Link |
|---|---|
| JP (1) | JP3985130B2 (en) |
| TW (1) | TWI255869B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004074555A1 (en) * | 2003-02-21 | 2004-09-02 | Mitsubishi Materials Corporation | Ni ALLOY ANODE MATERIAL FOR ELECTROLYTIC Ni PLATING |
| JP2008184637A (en) * | 2007-01-29 | 2008-08-14 | Nec Electronics Corp | ELECTROLYTIC Ni PLATING APPARATUS AND METHOD OF MANUFACTURING SEMICONDUCTOR DEVICE |
| CN105200267A (en) * | 2014-06-11 | 2015-12-30 | 丹阳市凯鑫合金材料有限公司 | Pure nickel N6 for lithium battery rivets and production method thereof |
-
2001
- 2001-08-22 JP JP2001251151A patent/JP3985130B2/en not_active Expired - Fee Related
-
2003
- 2003-02-21 TW TW92103699A patent/TWI255869B/en not_active IP Right Cessation
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004074555A1 (en) * | 2003-02-21 | 2004-09-02 | Mitsubishi Materials Corporation | Ni ALLOY ANODE MATERIAL FOR ELECTROLYTIC Ni PLATING |
| US7393499B2 (en) | 2003-02-21 | 2008-07-01 | Mitsubishi Materials Corporation | Ni alloy anode material for Ni electroplating |
| JP2008184637A (en) * | 2007-01-29 | 2008-08-14 | Nec Electronics Corp | ELECTROLYTIC Ni PLATING APPARATUS AND METHOD OF MANUFACTURING SEMICONDUCTOR DEVICE |
| CN105200267A (en) * | 2014-06-11 | 2015-12-30 | 丹阳市凯鑫合金材料有限公司 | Pure nickel N6 for lithium battery rivets and production method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| TWI255869B (en) | 2006-06-01 |
| TW200416308A (en) | 2004-09-01 |
| JP3985130B2 (en) | 2007-10-03 |
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