JPS59215474A - Electroless plating bath - Google Patents

Electroless plating bath

Info

Publication number
JPS59215474A
JPS59215474A JP9019083A JP9019083A JPS59215474A JP S59215474 A JPS59215474 A JP S59215474A JP 9019083 A JP9019083 A JP 9019083A JP 9019083 A JP9019083 A JP 9019083A JP S59215474 A JPS59215474 A JP S59215474A
Authority
JP
Japan
Prior art keywords
plating
nickel
plating bath
heat treatment
film
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.)
Granted
Application number
JP9019083A
Other languages
Japanese (ja)
Other versions
JPH0515790B2 (en
Inventor
Fumio Goto
文男 後藤
Takehiko Yamamoto
山本　武彦
Toshio Ishihara
石原　敏夫
Kazuo Tateishi
立石　和男
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.)
NEC Corp
Original Assignee
NEC Corp
Nippon Electric Co 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 NEC Corp, Nippon Electric Co Ltd filed Critical NEC Corp
Priority to JP9019083A priority Critical patent/JPS59215474A/en
Publication of JPS59215474A publication Critical patent/JPS59215474A/en
Publication of JPH0515790B2 publication Critical patent/JPH0515790B2/ja
Granted legal-status Critical Current

Links

Classifications

    • 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
    • C23C18/48—Coating with alloys
    • C23C18/50—Coating with alloys with alloys based on iron, cobalt or nickel

Landscapes

  • Chemical & Material Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemically Coating (AREA)

Abstract

PURPOSE:To form an Ni alloy film which is hardly magnetized after heat treatment without reducing the plating speed by adding a tartrate to an electroless Ni plating bath having a prescribed composition. CONSTITUTION:About 0.005-0.5mol/l tartrate such as sodium tartrate is added to an aqueous soln. contg. Ni ions, a small amount of other metallic ions such as Cu ions, a hypophosphite as a reducing agent, a pH buffer and a pH adjusting agent to obtain an electroless Ni plating bath. When this plating bath is used, an Ni alloy film which is hardly magnetized after heat treatment can be formed while almost maintaining the plating speed. The plating bath is used in the formation of a nonmagnetic Ni alloy film used as an intermediate layer between the substrate and magnetic recording medium of a magnetic recorlding body by electroless plating.

Description

【発明の詳細な説明】 本発明は、磁気ディスク等の磁気記録体において基体と
磁気記憶媒体（磁性膜）の間の中間層として用いられる
非磁性ニッケル合金めっき膜を作製するための無電解め
っき浴に関するものである。Detailed Description of the Invention The present invention relates to electroless plating for producing a non-magnetic nickel alloy plating film used as an intermediate layer between a substrate and a magnetic storage medium (magnetic film) in a magnetic recording medium such as a magnetic disk. It is related to bathing.

近年、コンビーータ・システムにおける外部記憶装置と
しての重要性が増大し、磁気ディスクの記録密度は年々
著しい向上がはかられつつある。従来、磁気記録媒体と
しては、酸化鉄微粒子とバインダーの混合物を基板上に
塗布したいわゆるコーティングディスクが広く用いられ
てきたが、今後さらに高密度化を達成するためには媒体
の薄膜化が必要となる。しかし、コーティングディスク
において媒体厚を０５μｍ程度以下とし、しかも均一な
記録再生特性を実現することは困難である。In recent years, the importance of external storage devices in converter systems has increased, and the recording density of magnetic disks has been significantly improved year by year. Conventionally, so-called coated disks, in which a mixture of iron oxide fine particles and a binder is coated on a substrate, have been widely used as magnetic recording media, but in order to achieve even higher densities in the future, it will be necessary to make the media thinner. Become. However, in a coated disk, it is difficult to reduce the medium thickness to about 0.5 μm or less and to achieve uniform recording and reproducing characteristics.

そこでコーティングディスクに代る高密度磁気ディスク
として、薄膜化が容易な連続薄膜媒体を用いた磁気ディ
スクが注目されている。連続薄膜媒体きして金属めっき
膜を用いためっき磁気ディスク、酸化物磁性薄膜を用い
たスパックティヌク等が開発され、記録密度を大幅に増
加しつるものと期待されている。Therefore, as a high-density magnetic disk to replace the coated disk, a magnetic disk using a continuous thin film medium that can be easily made thin is attracting attention. Continuous thin film media, such as plated magnetic disks using metal plating films and Spacktinook using oxide magnetic thin films, have been developed and are expected to significantly increase recording density.

この様な連続薄膜媒体を用いた磁気ディスクの製造は基
板形成工程と媒体形成工程Ｃζ大別され、基板形成工程
には以下に述べる問題があったり連続薄膜媒体の基板と
しては、媒体の薄膜化を可能とし低浮上量における安定
したヘッド浮揚状態を確保するための平坦性および平滑
性が要求され、基板欠陥の著しい低減が必要とされる。The manufacturing of magnetic disks using such continuous thin film media is broadly divided into a substrate forming process and a medium forming process Cζ, and the substrate forming process has the following problems. Flatness and smoothness are required to enable stable head flying at low flying heights, and a significant reduction in substrate defects is required.

また基板には機械的な強度、加工性、研磨性、軽量性、
低価格性、大量生産性なとの緒特性が必要とされ、更に
媒体形成工程におけるあるいはその後の熱処理によって
生じる基板の帯磁量が小さいほうが望ましいとされてい
る。The substrate also has mechanical strength, workability, polishability, lightness,
Low cost and mass productivity are required, and it is also desirable that the amount of magnetization of the substrate generated during the medium forming process or during subsequent heat treatment be small.

この様な基板としては、アルミニウム合金基体上にニッ
ケル・リン合金皮膜をめっきし、このニッケル・リン合
金皮膜表面を研磨した基板（以下ニッケル合金めっき基
板という）が検討されている。ニッケル・リン合金皮膜
を形成するには電、気メッキ法と無電解メッキ法の２つ
の方法があるが、電気メツキ法では欠陥の低減が十分で
なく、均一膜厚で平滑なニッケル・リン合金皮膜を得る
のが困難で生、産性に問題があるため殆ど用いられてい
ない。−力無電解〆）・ｙ千法によってニッケル・リン
合金皮膜を形成する場合には、機械的強度、加工性、研
磨性および軽量性の点で良好な特性のニッケル・合金め
っき基板が得られることに加え、基板欠陥の微小化およ
び極少数比が可能で、膜Ｊ！ＩＯ均一性と生産性に優れ
ていることなどの長所を有しているが、熱処理によって
磁性を帯びやすいという欠点をもっている。As such a substrate, a substrate in which a nickel-phosphorus alloy film is plated on an aluminum alloy base and the surface of the nickel-phosphorus alloy film is polished (hereinafter referred to as a nickel-alloy plated substrate) is being considered. There are two methods for forming a nickel-phosphorus alloy film: electroplating and electroless plating, but the electroplating method does not sufficiently reduce defects and produces a smooth nickel-phosphorus alloy film with a uniform thickness. It is hardly used because it is difficult to obtain a film and there are problems with production and productivity. - When forming a nickel-phosphorus alloy film by the electroless method, a nickel-alloy plated substrate with good properties in terms of mechanical strength, workability, polishability, and light weight can be obtained. In addition, it is possible to miniaturize substrate defects and minimize the number of defects, making it possible to improve film J! Although it has advantages such as excellent IO uniformity and productivity, it has the disadvantage of being easily magnetized by heat treatment.

酸化膜磁性薄膜を用いたスパッタディスクの媒体形成工
程においては、スパッタによりＦ　ｅ　ｓ　Ｏａ膜を形
成後、２７０℃から３００℃　の温度で１時間程度熱処
理を行ってγ−１ｉ’ｅｓＯ＊からなる磁性落動５形成
されるが、熱処理によって生じるニッケル合金めっき基
板の帯磁量が大きい程帯磁しない基板を用いた場合と比
較した再生出力の低下が大きい。In the process of forming a sputter disk medium using an oxide magnetic thin film, after forming a FesOa film by sputtering, heat treatment is performed at a temperature of 270°C to 300°C for about 1 hour to form a film made of γ-1i'esO*. Magnetic drop 5 is formed, but the greater the amount of magnetization of the nickel alloy plated substrate caused by heat treatment, the greater the reduction in reproduction output compared to the case where a non-magnetized substrate is used.

めっき磁気ディスクでは磁性薄膜媒体の上に珪酸モノマ
ーを回転塗布後熱処理を行って保商膜が形成される。こ
の保護膜は熱処理温度が高い程硬度が増加するが、この
場合も再生出力の低下を避けるため二−ツケル合金めっ
き基板の帯磁量が小さいこさが望ましい。In plated magnetic disks, a coating film is formed by spin-coating a silicic acid monomer onto a magnetic thin film medium and then subjecting it to heat treatment. The hardness of this protective film increases as the heat treatment temperature increases, but in this case as well, it is desirable that the amount of magnetization of the Nikkei alloy plated substrate be small in order to avoid a decrease in reproduction output.

従来、無電解ニッケルめっき液においては、めっき浴の
ＰＨを下げることにより析出皮膜中（、）リン含有量を
増加させ熱処理による帯磁量の低減がはかられていたが
、同時にめっき速度の著しい低下を伴なうため実用上問
題があった。Conventionally, in electroless nickel plating solutions, the phosphorus content in the deposited film was increased by lowering the pH of the plating bath, and the amount of magnetization due to heat treatment was reduced, but at the same time, the plating speed was significantly reduced. This posed a practical problem.

本発明の目的は上述した従来技術の欠点を改善して、め
っき速度の著しい低下を伴なうことなく熱処理による帯
磁量の少ないニッケル・合金皮膜を作製しうる無１ｉ１
１ｆめっき浴を提供することにある。The purpose of the present invention is to improve the above-mentioned drawbacks of the prior art, and to make it possible to produce a nickel alloy film with a small amount of magnetization by heat treatment without significantly reducing the plating speed.
The objective is to provide a 1f plating bath.

本発明によれば、ニッケル・イオンを主成分とする金属
イオン、前記金属イオンの還元剤きしての次亜リン酸塩
、削記金ハイオンの錯化剤、Ｐｌ−■緩衝剤およびＰＨ
’？ＪＪｊＮ剤を含む水溶液に酒石酸塩を添加したこと
を％徴とする無電解めっき浴が提供される。According to the present invention, metal ions mainly composed of nickel ions, hypophosphite as a reducing agent for the metal ions, a complexing agent for the metal ions, a Pl-■ buffer, and a PH
'? An electroless plating bath is provided in which a tartrate salt is added to an aqueous solution containing a JJjN agent.

本兄明において用いられる金属イオンとしてはニッケル
イオンを主成分とするが１少景の銅イオン、スズイオン
、マンカンイオン、亜鉛イオン、タンクステン酸イオン
、七すフデン酸イオンなどが”金談れることがあり、こ
れらはニッケル、銅）スズ、マンカン、亜鉛の硫酸塩、
塩化塩１．酢酸塩などの可溶性塩またはタングステン散
、モリブデン酸などの可溶性塩を無電解めっき浴中に溶
解することによって供給される。ニッケル・ｒオンの濃
度は０．００４〜１　ｍｏｌ／　１１　（Ｄ範囲が用い
られるが、好才しくは０．０５〜０．１５　ｒｎｏｌｌ
／ｌ　のイ・１囲である。The main metal ions used in this study are nickel ions, but there are also a few copper ions, tin ions, mankan ions, zinc ions, tankstate ions, hexafudate ions, etc. These are nickel, copper) tin, mankan, zinc sulfates,
Chloride salt 1. It is supplied by dissolving a soluble salt such as acetate or tungsten powder or molybdic acid in an electroless plating bath. The concentration of nickel r-on is 0.004 to 1 mol/11 (D range is used, but preferably 0.05 to 0.15 mol/11
/l is A.1 circle.

銅イオン、スズイオン、マンカンイオン、亜鉛イＡン、
タングスデン酸イオン、モリブテン峻イオンなどの濃度
はｏ、ｕ　ｕ　ｏ　ｉ〜０．２ｍｏｌ／ｌの範囲が用い
られるが好ましくは０．０００３〜０．０１　ｍｏ　ｌ
／　ｌの範囲である。還元剤としては次亜リン酸塩が用
いられ。Copper ion, tin ion, mankan ion, zinc ion,
The concentration of tungstate ion, molybdenum ion, etc. is in the range of o, uo i to 0.2 mol/l, but preferably 0.0003 to 0.01 mol/l.
/l range. Hypophosphite is used as a reducing agent.

００２〜０．８＋ｎｏｌ／ｌの範囲が適するが好丈しく
はｏ、１〜０．３　ｍｏｌ／１１の範囲である。A range of 0.002 to 0.8+nol/l is suitable, but a preferred range is 1 to 0.3 mol/11.

ＰＨ緩衝剤としてはアンモニウム塩、炭醒塩、有機酸塩
などが使用され、０．０ｔＪ　５〜１．５　ｍｏ１３／
　１３の範囲の濃度が用いられる。ＰＨｍ節剤としては
、ＰＨの上昇にはアンモニア、水酸化ナトリウムなどの
アルカリが月ｈ１られ、ＰＨの計重には硫酸、塩酸など
の酸が用いられる。錯化剤としては、リンゴ酸塩才た（
オリンゴ酸の可溶性塩、コハク酸またはコハク酸の可溶
性塩、酢酸または酢酸のり溶性塩、クエン酸またはクエ
ン１ｐの可溶性塩、乳酸または乳酸の可溶性塩などが、
０．０１〜１．５１１ＯＡ／ｌの濃度範囲で用いられる
。酒石酸塩としては闇石酸および酒石酸の可溶性址が便
用晦れ、０．０（１５〜ｕ、５ｍｏ／／ｌの濃度範囲が
ｙ（］いられる。更に無電解ニッケルめっき液において
は、ビンポール防止、平滑−光沢化の目的′Ｃ？１コン
陳メナル、アグリル酸メチル、プロピＡ７酸、乳酸、チ
オ原票、鉛、タリウムなどが少瀘添勾口されるこ七があ
る。Ammonium salts, carbonate salts, organic acid salts, etc. are used as pH buffering agents, and 0.0tJ 5 to 1.5 mo13/
A range of 13 concentrations is used. As a PHm moderator, an alkali such as ammonia or sodium hydroxide is used to increase the pH, and an acid such as sulfuric acid or hydrochloric acid is used to measure the pH. As a complexing agent, malate (
Soluble salts of oleic acid, succinic acid or soluble salts of succinic acid, acetic acid or acetic acid paste-soluble salts, citric acid or soluble salts of citric acid, lactic acid or soluble salts of lactic acid, etc.
It is used in a concentration range of 0.01 to 1.511 OA/l. As the tartrate, tartaric acid and soluble tartaric acid are used, and the concentration range of 0.0 (15 to 5 mo//l) is used.Furthermore, in the electroless nickel plating solution, Vinpol For the purpose of preventing, smoothing and brightening, a small amount of C-1 compound, methyl agrilate, propylene A7 acid, lactic acid, thio-base, lead, thallium, etc. is added.

以１、ホーＴ３Ａｌこよる無電解めっき浴の特長を比較
例および実施例Ｉこより説明する。In the following, the features of the electroless plating bath based on T3Al will be explained with reference to Comparative Examples and Example I.

比較例 アルミ合金基板上に酸洗浄、亜鉛Ｗ換などからなる一様
な無電解ニッケル合金めっきを行うに適した前処理を施
した後、下記のめっき浴を用いて膜厚２０μｍのニッケ
ル゛リンめっき膜を形成した。Comparative Example After performing pretreatment suitable for uniform electroless nickel alloy plating, such as acid cleaning and zinc W exchange, on an aluminum alloy substrate, a nickel phosphor layer with a thickness of 20 μm was applied using the following plating bath. A plating film was formed.

無電解ニッケル・リンめっき浴 めっき液組成 硫ｔＲニッケル０．１　　　ｍｏ１７１次亜リン酸ナト
リウム　　　　０．２３　　　ｍｏｌ／　１硫酸アンモ
−１−ラム　　　　　　０．０１ｍｏｌ／１リンゴ酸ナ
トリウム　　　　　　０．　ｌ　６　　　ｍ０１／１コ
ハク酸ナトリウム　　　　　　ｏ、　ｏ　５５　ｍｏｌ
／１めっき条件 めっき液のＰＨ，３，９〜５１ 液温　　　　９０℃ 各ＰＨ条件におけるめっき速度と得られた＃　醒解ニッ
ケル・リンめっき膜の３００℃１時間の熱処理後の飽和
磁束密度（Ｂｓ）を表１に示す。Electroless nickel-phosphorus plating bath Plating solution composition Sulfur tR Nickel 0.1 mo171 Sodium hypophosphite 0.23 mol/1 Ammonium sulfate 0.01 mol/1 Sodium malate 0. l 6 m01/1 Sodium succinate o, o 55 mol
/1 plating condition PH of plating solution, 3,9-51 Solution temperature 90℃ Plating speed under each PH condition and obtained # Saturation magnetic flux density (Bs ) are shown in Table 1.

表１．めっき液のＰＨとめっき速度、熱処理後のＢｓの
関係 表に示される様にめっき液のＰＨを低下することによっ
て熱処理後の帯磁量の低減をはかることができるが、同
時にめっき速度の著しい減少も伴うため実用上問題があ
る。Table 1. As shown in the relationship table between plating solution PH, plating speed, and Bs after heat treatment, the amount of magnetization after heat treatment can be reduced by lowering the pH of the plating solution, but at the same time, the plating speed may also be significantly reduced. This poses a practical problem.

実施例１゜ 比較例と同様の手順でアルミ合金基板上に無電解ニッケ
ル合金めっきを行ったが、本実施例では下記のめっき浴
を用いて膜厚２０μｎ１のニッケル・リンめっき膜を形
成した。Example 1 Electroless nickel alloy plating was performed on an aluminum alloy substrate using the same procedure as in the comparative example, but in this example, the following plating bath was used to form a nickel-phosphorus plating film with a thickness of 20 μn1.

無電解ニッケル・リンめっき浴 めっき液組成 儲歳ニッケル　　　　　　　０．１　　ｍａｌｌ／１次
亜リン駿ナトすウム　　　　　　　　　０．２３ｒｎ　
ｏ　ｌ／’１硫酸アンモニウム　　　　　　　　　　　
ｏ、ｏ　１ｍ　ｏ　ｌ／　ｌリンゴ酸ナトリウム　　　
　　　　　　　０．１６ｍｏｌ／ｌコハク酸ナトリウム
　　　　　　　　　　０．０５ｓ　ｍｏ　ｌ／１歯石酸
ナトリウム　　　０　、　ＬＪ、１　、０．２　、０．
３　、０．４　、０．５　、０．６ｍａｌｌ／１ めっき条件 めっき液のＰＨ４，８ １１）ξ　溝　　　　　　　　　９０℃各酒石酸すｌ−
ＩＪウム濃度におけるめっき速度と得られた無電解ニッ
ケル°リンめっき膜の３００℃１時間の熱処理後のＩ３
ｓを表２に示す。Electroless nickel and phosphorus plating bath Plating solution composition Chusai nickel 0.1 mall/1 hypophosphorus sodium 0.23rn
o l/'1 ammonium sulfate
o, o 1m o l/l sodium malate
0.16 mol/l sodium succinate 0.05 s mol/1 sodium tartarate 0, LJ, 1, 0.2, 0.
3, 0.4, 0.5, 0.6 mall/1 Plating conditions PH of plating solution 4,8 11) ξ Groove 90℃ each tartaric acid l-
Plating speed at IJium concentration and I3 of the obtained electroless nickel phosphorus plating film after heat treatment at 300°C for 1 hour
s is shown in Table 2.

表２．酒石酸す）ＩＪウム濃度とめっき速度、熱処理後
のＢｓの関係 表に示される様に酒石酸ナトリウム濃度を増加すること
によってめっき速度の著しい減少を伴うことなく、熱処
理による帯磁量の少ないニッケル・リンめっき膜を作製
することができた。Table 2. As shown in the table showing the relationship between IJium tartrate concentration, plating speed, and Bs after heat treatment, increasing the sodium tartrate concentration does not significantly reduce the plating speed, resulting in nickel/phosphorus plating with less magnetization due to heat treatment. We were able to create a membrane.

実施例λ 比較例と同様の手順でアルミ合金基板上に膜厚２０μｍ
のニッケル・リンめっき膜を形成したが、本実施例では
下記のめっき浴を使用した。Example λ A film with a thickness of 20 μm was formed on an aluminum alloy substrate using the same procedure as in the comparative example.
In this example, the following plating bath was used.

；憔ｒｉｂ、　８’ｌニアケル°リンめっき浴めっき液
組成 （ｐに敵ニッケル　　　　　　Ｌｌ、　１　　ｍｏｌ／
１１伏亜リンＩ孜ナトリウム　　　０．２８　　ｍｏ　
ｌ／ｉＩＡ［アンモニウム　　　０．Ｕ　ｌ　　ｍｏｌ
！／１リ　ン　コ　配プ　　１・　リ　ウ　、ム　　　
　　０．１８　　　　ｍｏ　ＩＪ／７！フハク酸プトリ
ウム　　０．０４　口］ｏｌＪ／１酒石酸ナトリウム　
　０，０．２，０．３，０．４，０．５，０．６゜０．
７，０．８　　　ｍｏｌ／１ ノ”ロビオン（４１０，０１ｍｏ　１３／１酢ｆｉ　　
　　　０．００ＵＯ７ｒｎ０１１／１−７　（）　７　
ｆｆ、？メチＪｌ／　　　　　０．０　（ｌ　Ｏ９ｍｏ
ｌ／１アソリル（ＩＪメチル　　　　旧＋　００５　　
ｍａｌ／ｌめっき条件 めっき液のｐｉ（４，８ 訣温　　　　’Ｊ　Ｏ’Ｃ 各酒石酸す）　ＩＪウム濃度におけるめ・つき速度と得
られた無４１１ニツケル・リンめっき膜の３００℃１時
間の熱処理後のＪＪｓｔ表３に示す。; Rib, 8'l phosphorous plating bath Plating solution composition (p and nickel Ll, 1 mol/
11 Fuyarin I Sodium 0.28 mo
l/iIA [ammonium 0. U mol
! /1 link distribution 1. riu,mu
0.18 mo IJ/7! Putrium succinate 0.04 mouth] olJ/1 Sodium tartrate
0,0.2,0.3,0.4,0.5,0.6゜0.
7,0.8 mol/1 No” Robion (410,01 mo 13/1 vinegar fi
0.00UO7rn011/1-7 () 7
ff,? Methi Jl/ 0.0 (l O9mo
l/1 asoryl (IJ methyl old + 005
mal/l plating condition Plating solution pi (4,8 temperature 'J O'C each tartaric acid) Plating speed at IJum concentration and heat treatment of the obtained 411 nickel/phosphorous plating film at 300°C for 1 hour It is shown in JJst Table 3 below.

表３．酒石酸ナトリウム濃度とめっき速度、熱処理後の
Ｂｓの関係 表に示される様に酒石酸ナトリウム濃度を増加すること
ｌこよってめっき速度を殆ど減少させることなく、熱処
理による帯磁量の少ないニッケル・リンめっき膜を得る
ことができた。Table 3. As shown in the table showing the relationship between sodium tartrate concentration, plating speed, and Bs after heat treatment, increasing the sodium tartrate concentration can produce a nickel-phosphorus plating film with less magnetization due to heat treatment without almost decreasing the plating speed. I was able to get it.

なお、本実施例ではめっき膜の表面状態改善の目的でめ
っき液組成に少量のグロピオン酸、酢酸、マロン酸メチ
ル、アクリル酸メチルを添加しており、これによりピン
ホールが少なく平滑なめっき膜が得られた。In this example, a small amount of gropionic acid, acetic acid, methyl malonate, and methyl acrylate were added to the plating solution composition for the purpose of improving the surface condition of the plating film, which resulted in a smooth plating film with few pinholes. Obtained.

実施例３゜ 比較例と同様の手順でアルミ合金基板上に無電解ニッケ
ル合金めっきを行ったが、本実施例では下記のめっき浴
を用いて膜厚２０μｍのニッケル・スズ・リンめっき膜
を形成した。Example 3 Electroless nickel alloy plating was performed on an aluminum alloy substrate using the same procedure as in the comparative example, but in this example, the following plating bath was used to form a nickel-tin-phosphorus plating film with a thickness of 20 μm. did.

Ｗ、、寛解ニッケル・スズ・リンめっき浴めっき液組成 硫酸ニッケル　　　　　　０．１５　　ｍｏ１７１次亜
リン酸ナトリウム　　　　０．３０　　ｍｏｌ／１硫酸
アンモニウム　　　　　　０．０２　　ｍｏｌ／１乳酸
　　　　　　　　　　　０．９　　ｍｏｌ／１塩化第二
スズ　　　　　　　　０．１　　ｍｏｌ／１酒石酸ナト
リウム　　０，０．＞、０．２，０．３，０．４，０．
５ｍｏｌ／１めっき条件 めっき液のＰＨ５，２ 液温　　　　９０℃ 各酒石酸ナトリウム濃度におけるめっき速度と得られた
無電解ニッケル・スズ・リンめっき膜の３００℃１時間
の熱処理後のＢｓを表４に示す。W,, Relaxed nickel tin phosphorus plating bath Plating solution composition Nickel sulfate 0.15 mo171 Sodium hypophosphite 0.30 mol/1 Ammonium sulfate 0.02 mol/1 Lactic acid 0.9 mol/1 Tin chloride 0 .1 mol/1 sodium tartrate 0.0. >, 0.2, 0.3, 0.4, 0.
5 mol/1 plating condition Plating solution PH5.2 Solution temperature 90°C Plating speed at each sodium tartrate concentration and Bs of the obtained electroless nickel-tin-phosphorus plating film after heat treatment at 300°C for 1 hour are shown in Table 4. .

表４．酒石酸ナトリウム濃度とめっき速度、熱処理後の
Ｂｓの関係 表に示される様に酒石酸ナトリウム濃度を増加すること
によってめっき速度を殆ど減少させることなく、熱処理
後の帯磁量が少ないニッケル・スズ−リンめっき膜を得
ることができた。Table 4. As shown in the table showing the relationship between sodium tartrate concentration, plating speed, and Bs after heat treatment, by increasing the sodium tartrate concentration, the plating speed hardly decreases, and the nickel/tin-phosphorus plating film has a small amount of magnetization after heat treatment. I was able to get

実施例４、 比較例と同様の手屓でアルミ合金基板上に無電解ニッケ
ル合金めっきを行ったが、本実施例では下記のめっき浴
を用いて膜Ｊ！￥２０μｍのニッケル・銅・リンめっき
膜を形成した。Example 4 Electroless nickel alloy plating was performed on an aluminum alloy substrate in the same manner as in Comparative Example, but in this example, the following plating bath was used to form the film J! A 20 μm nickel/copper/phosphorus plating film was formed.

無電解ニッケル・銅−リンめっき浴 めっき液組成 硫酸ニッケル　　　　　　　　０．１２５　　ｍｏｌ／
／１塩化銅　　　　　　３Ｘ１０　　ｍａｉ１７１次亜
リン酸ナトリウム　　　　　　　　０．０８　　　ｍｏ
ｌ／１リンシ酸ナトリウム　　　　　　　　　０−２　
　　　ｍｏｌ／ノ酢酸　　　　　　　０．０７　　ｍｏ
ｌ／１クエン酸　　　　　　　　　　０．０２　　　ｍ
ｏｌ／１乳酸　　　　　Ｉ　ＸＩＯ’　ｍｏ　ｌ／ｌマ
ロン酸メチル　　　　　　　　　　　５×ｌＯ〜’ｍｏ
ｌ／１アクリル酸メチル　　　　　　　　　　０．０１
３　　ｍｏｌ／１酒石酸ナトリウム　　０　、０．１　
、０．２　、０．３　、０．４　、０．５ｍ　ｏ　ｌ　
／　１ めっき条件 めっき液のＰＨ５，３ 液　　温　　　　　　　　　　　９０℃各ｎ石酸ナトリ
ウム濃度におけるめっき速度と得られた無電解ニッケル
・銅・リンめっき膜の３００℃　１時間の熱処理後のＢ
ｇを表５に示す。Electroless nickel/copper-phosphorus plating bath Plating solution composition Nickel sulfate 0.125 mol/
/1 Copper chloride 3X10 mai171 Sodium hypophosphite 0.08 mo
l/1 sodium phosphate 0-2
mol/noacetic acid 0.07 mo
l/1 citric acid 0.02 m
ol/1 lactic acid I XIO' mol/l methyl malonate 5×lO~'mo
l/1 methyl acrylate 0.01
3 mol/1 sodium tartrate 0, 0.1
,0.2,0.3,0.4,0.5mol
/ 1 Plating conditions Plating solution PH5, 3 Solution temperature 90℃ Plating speed at each sodium phosphate concentration and B of the obtained electroless nickel/copper/phosphorus plating film after heat treatment at 300℃ for 1 hour
g is shown in Table 5.

衣５．　　ｒｉ’ｎ石敵ナトリウム濃度とめつき速度、
熱処理後のＢｓの関係 表に示される様に酒石酸す）　ＩＪウム濃度を増加する
ことによってめっき速度を殆ど減少させることなく、熱
処理後の帯磁量が少ないニッケル・銅・リンめっき膜を
得ることができた０ 以上、比較例および実施例で示された様に本発明によれ
ば、ニッケルイオンを主成分とする金属イオン、前記金
属イオンの還元剤としての次亜リン酸塩、前記金属イオ
ンの錯化剤、ＰＨ緩衝剤およびＰＨ調節剤を含む水浴液
に酒石酸塩を添加することにより、めっき速度の著しい
低下を伴なうことなく、熱処理による帯磁量の少ないニ
ッケル合金皮膜が得られる。Clothes 5. ri'n stone enemy sodium concentration and plating speed,
As shown in the relationship table for Bs after heat treatment, by increasing the IJ concentration, it is possible to obtain a nickel/copper/phosphorus plating film with a small amount of magnetization after heat treatment without decreasing the plating speed. As shown in the comparative examples and examples above, according to the present invention, metal ions mainly composed of nickel ions, hypophosphite as a reducing agent for the metal ions, and By adding tartrate to a water bath solution containing a complexing agent, a PH buffer, and a PH adjuster, a nickel alloy film with less magnetization due to heat treatment can be obtained without significantly reducing the plating rate.

Claims (1)

【特許請求の範囲】[Claims] ニッケルイオンを主成分とする金属イオン、前記金属イ
オンの還元剤としての次亜リン酸塩、前記金属イオンの
錯化剤、ＰＨ緩衝剤およびＰＨ調節剤を含む水溶液に酒
石酸塩を添加したことを特徴とする無電解めっき浴。Addition of tartrate to an aqueous solution containing metal ions mainly composed of nickel ions, hypophosphite as a reducing agent for the metal ions, a complexing agent for the metal ions, a PH buffer, and a PH regulator. Characteristic electroless plating bath.
JP9019083A 1983-05-23 1983-05-23 Electroless plating bath Granted JPS59215474A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP9019083A JPS59215474A (en) 1983-05-23 1983-05-23 Electroless plating bath

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP9019083A JPS59215474A (en) 1983-05-23 1983-05-23 Electroless plating bath

Publications (2)

Publication Number Publication Date
JPS59215474A true JPS59215474A (en) 1984-12-05
JPH0515790B2 JPH0515790B2 (en) 1993-03-02

Family

ID=13991562

Family Applications (1)

Application Number Title Priority Date Filing Date
JP9019083A Granted JPS59215474A (en) 1983-05-23 1983-05-23 Electroless plating bath

Country Status (1)

Country Link
JP (1) JPS59215474A (en)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS62274076A (en) * 1986-05-23 1987-11-28 Toyo Kohan Co Ltd Electroless nickel-phosphorus plating bath
JP2013144835A (en) * 2012-01-16 2013-07-25 Qualtec:Kk ELECTROLESS Ni-P-Sn PLATING SOLUTION
JP2014162950A (en) * 2013-02-25 2014-09-08 Kanto Gakuin Electroless NiSnP plating film
JP2015021178A (en) * 2013-07-22 2015-02-02 株式会社クオルテック ELECTROLESS Ni-P-Sn PLATING SOLUTION

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS548450A (en) * 1977-06-21 1979-01-22 Matsushita Electric Ind Co Ltd Multistage multistable multivibrator
JPS55164067A (en) * 1979-06-08 1980-12-20 Hitachi Ltd Method for nonelectrolytic plating

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS548450A (en) * 1977-06-21 1979-01-22 Matsushita Electric Ind Co Ltd Multistage multistable multivibrator
JPS55164067A (en) * 1979-06-08 1980-12-20 Hitachi Ltd Method for nonelectrolytic plating

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS62274076A (en) * 1986-05-23 1987-11-28 Toyo Kohan Co Ltd Electroless nickel-phosphorus plating bath
JP2013144835A (en) * 2012-01-16 2013-07-25 Qualtec:Kk ELECTROLESS Ni-P-Sn PLATING SOLUTION
JP2014162950A (en) * 2013-02-25 2014-09-08 Kanto Gakuin Electroless NiSnP plating film
JP2015021178A (en) * 2013-07-22 2015-02-02 株式会社クオルテック ELECTROLESS Ni-P-Sn PLATING SOLUTION

Also Published As

Publication number Publication date
JPH0515790B2 (en) 1993-03-02

Similar Documents

Publication Publication Date Title
JPS59215474A (en) Electroless plating bath
JPS59170254A (en) Electroless plating bath
JPH0766034A (en) Soft magnetic material film and manufacture thereof
JP3533880B2 (en) Electroless nickel plating solution and electroless nickel plating method
JPS62270778A (en) Electroless plating bath
JPH0666086B2 (en) Magnetic recording medium and manufacturing method thereof
JPS62274076A (en) Electroless nickel-phosphorus plating bath
JPS6115985A (en) Electroless plating bath
JPS6256577A (en) Electroless plating bath
JPS6383281A (en) Electroless plating bath
JPS60103181A (en) Electroless plating bath
JPS5858267A (en) Electroless plating bath
JPH0229753B2 (en) MUDENKAIMETSUKIHOHO
EP0322895A2 (en) Methods and compositions for electroless plating of magnetic recording media
JPS60149785A (en) Electroless plating bath
JPS6270580A (en) Electroless plating bath
JPS6016011B2 (en) Manufacturing method for high recording density magnetic disks
JPS59232264A (en) Electroless co-ni-p plating bath
JPS63134668A (en) Magnetic plating solution
JPH0310085A (en) Surface treatment for substrate
JPS6235476B2 (en)
JPS6381622A (en) Magnetic recording body and its production
JPS5858270A (en) Electroless plating bath
JPS6283474A (en) Electroless plating bath
JPS6210279A (en) Electroless plating bath