JPH04165079A - Method for producing and working chemical nickel plating liquid cell and chemical nickel plating method using this plating liquid cell - Google Patents
Method for producing and working chemical nickel plating liquid cell and chemical nickel plating method using this plating liquid cellInfo
- Publication number
- JPH04165079A JPH04165079A JP28589790A JP28589790A JPH04165079A JP H04165079 A JPH04165079 A JP H04165079A JP 28589790 A JP28589790 A JP 28589790A JP 28589790 A JP28589790 A JP 28589790A JP H04165079 A JPH04165079 A JP H04165079A
- Authority
- JP
- Japan
- Prior art keywords
- plating
- nitric acid
- tank
- chemical nickel
- nickel plating
- 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
Links
- 238000007747 plating Methods 0.000 title claims abstract description 52
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 239000000126 substance Substances 0.000 title claims abstract description 26
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 20
- 239000007788 liquid Substances 0.000 title claims abstract description 11
- 238000000034 method Methods 0.000 title claims description 17
- 238000004519 manufacturing process Methods 0.000 title claims description 8
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 30
- 239000010935 stainless steel Substances 0.000 claims abstract description 7
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 7
- 239000000463 material Substances 0.000 claims description 13
- 229910000831 Steel Inorganic materials 0.000 claims description 2
- 239000010959 steel Substances 0.000 claims description 2
- 229910001566 austenite Inorganic materials 0.000 abstract description 7
- 229910044991 metal oxide Inorganic materials 0.000 abstract description 5
- 150000004706 metal oxides Chemical class 0.000 abstract description 5
- 230000008021 deposition Effects 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 23
- 238000005406 washing Methods 0.000 description 21
- 238000005238 degreasing Methods 0.000 description 4
- 150000002816 nickel compounds Chemical class 0.000 description 4
- 230000004913 activation Effects 0.000 description 3
- 238000007654 immersion Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 238000002791 soaking Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000010306 acid treatment Methods 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 description 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910000881 Cu alloy Inorganic materials 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 1
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 1
- SPIFDSWFDKNERT-UHFFFAOYSA-N nickel;hydrate Chemical compound O.[Ni] SPIFDSWFDKNERT-UHFFFAOYSA-N 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 235000019260 propionic acid Nutrition 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 239000001509 sodium citrate Substances 0.000 description 1
- 229910001379 sodium hypophosphite Inorganic materials 0.000 description 1
Landscapes
- Chemically Coating (AREA)
Abstract
Description
【発明の詳細な説明】
産業上の利用分野
本発明は化学（無電解）ニッケルメッキ液槽の製作加工
方法、および該メツキ液槽を利用した化学ニッケルメッ
キ方法に関するものである。DETAILED DESCRIPTION OF THE INVENTION Field of Industrial Application The present invention relates to a method for manufacturing a chemical (electroless) nickel plating bath, and a chemical nickel plating method using the plating bath.
従来の技術
従来使用されている化学メツキ槽の殆どはその材質とし
てＳＵＳ−３０４あるいはＳ Ｕ Ｓ −３１６等のス
テンレス類のものである。BACKGROUND OF THE INVENTION Most conventionally used chemical plating tanks are made of stainless steel such as SUS-304 or SUS-316.
これらの材質のメツキ槽に化学ニッケルメッキ液（その
組成は後記参照）を建浴し、液を９０〜９５℃に加熱し
、鉄、銅、銅合金、アルミニウム等の被メツキ体にＮ１
−Ｐメツキをする場合、メッキ槽面の表面にニッケル化
合物（Ｎｉ−Ｐ）が約４０へ一８０時間位で析出してく
るため、良好なメツキ製品ができない。Prepare a chemical nickel plating solution (see below for its composition) in a plating tank for these materials, heat the solution to 90-95°C, and apply N1 to the plated materials such as iron, copper, copper alloy, aluminum, etc.
- When plating with P, a nickel compound (Ni-P) precipitates on the surface of the plating tank in about 40 to 180 hours, making it impossible to produce a good plated product.
そのため、該析出物を除去するため液槽内のメツキ液を
全部抜き出し、その後に槽容積だけの冷濃硝酸（室温ま
たはそれ以下の温度の濃硝酸）を入れて約２０へ２４時
間放置し、該硝酸を抜き出し、槽内を水洗し槽の再利用
をくり返しているのが現状である０周知のごと（、硝酸
を５Ｏ３−３０４やＳＵＳ−３１６のような材質と長時
間接触させることにより、化学ニッケルメッキ液中のＮ
１−Ｐに対して非常に不活性なオーステナイトや金属酸
化物被膜が槽の表面に生成するからである。Therefore, in order to remove the precipitates, all the plating liquid in the liquid tank was extracted, and then cold concentrated nitric acid (concentrated nitric acid at room temperature or lower temperature) was added to the tank volume and left for about 24 hours. At present, the nitric acid is extracted, the inside of the tank is washed with water, and the tank is reused (as is well known). N in chemical nickel plating solution
This is because austenite and metal oxide films, which are extremely inert to 1-P, are formed on the surface of the tank.
しかしながら、従来の冷硝酸による方法だとメツキ槽の
ライフもめ４０〜８０時間と短く、さらにまた、次のよ
うな欠点があった。However, the conventional method using cold nitric acid has a short plating tank life of 40 to 80 hours, and also has the following drawbacks.
（１） メツキ槽内のクリーニングや材質再生のため
に使用する硝酸の量が多く、費用がかかる。(1) A large amount of nitric acid is used for cleaning inside the plating tank and for regenerating the material, which is expensive.
（２）使用済の硝酸は廃棄しなければならず、そのため
の費用が真人にかかる。(2) Used nitric acid must be disposed of, which incurs costs for Masato.
（３）冷硝酸で槽内を洗浄、反応させてオーステナイト
や金属酸化物被膜を生成させるには、メツキ作業を長時
間中断しなければならない。このために予６ＩＮ等の余
分の装置が必要である。(3) In order to clean the inside of the tank with cold nitric acid and cause the reaction to produce austenite or metal oxide coatings, the plating operation must be interrupted for a long time. For this purpose, extra equipment such as a pre-6IN is required.
（４） 多くの労力や時間を必要とする。(4) It requires a lot of effort and time.
発明の目的
したがって本発明の目的は、前記の欠点を解消した新規
な化学ニッケルメッキ液槽の製作加工方法を提供するこ
とである。別の目的は、前記の新規製作加工方法で得ら
れた化学ニッケルメッキ液槽を使用することを包含する
新規な化学ニンケルメソキ方法を提供することである。OBJECTS OF THE INVENTION Accordingly, it is an object of the present invention to provide a novel method for manufacturing a chemical nickel plating bath that eliminates the above-mentioned drawbacks. Another object is to provide a new chemical nickel plating method that includes using the chemical nickel plating bath obtained with the above novel fabrication and processing method.
発明の構成
本発明は、メツキ液槽を構成するＳＵＳ−３０４または
ＳＵＳ−３ｉ ６等のステンレス鋼のごとき鋼鉄系の槽
材質の内面を熱硝酸（好ましくは約４０〜５０℃の温度
の硝＃）で処理することを特徴とする化学ニッケルメッ
キ液槽の製作加工方法に関するものである０本発明はま
た、前記の製作加工方法で得られた化学ニッケルメッキ
液槽を使用することを特徴とする化学ニッケルメッキ方
法にも関する。Structure of the Invention The present invention provides a method of cleaning the inner surface of a steel-based tank material such as stainless steel such as SUS-304 or SUS-3i 6 constituting a plating liquid tank with hot nitric acid (preferably nitric acid at a temperature of about 40 to 50°C). ) The present invention is also characterized in that a chemical nickel plating solution bath obtained by the above manufacturing method is used. It also relates to chemical nickel plating methods.
本発明に従って熱硝酸（好ましくは４０〜５０℃位）で
ＳＵＳ−３０４や５ＬＩＳ−３１６等のステンレス鋼系
の材質の槽内面を処理することにより、化学ニッケルメ
ッキ液中のＮｉ −Ｐの析出を効果的に防止できる。こ
の熱硝酸処理によってオーステナイトや金属酸化物被膜
が全面に多量生成し、そのため、化学メツキに約２００
０時間以上使用してもメツキ槽内面の何らの析出物もな
く、すなわち確実に長時間使用できることを発見した。According to the present invention, by treating the inner surface of a tank made of a stainless steel material such as SUS-304 or 5LIS-316 with hot nitric acid (preferably at about 40 to 50°C), Ni-P is precipitated in a chemical nickel plating solution. can be effectively prevented. This hot nitric acid treatment produces a large amount of austenite and metal oxide coatings on the entire surface, resulting in approximately 200% of chemical plating.
It was discovered that there was no precipitate on the inner surface of the plating tank even after using it for 0 hours or more, that is, it could be used reliably for a long time.
また、この方法で加工して製造した化学メンキ槽を装置
内に設置することにより、予備槽等の設置が不要となり
、かつ、連続自動運転ができる。Moreover, by installing the chemical bran tank manufactured by this method in the device, there is no need to install a reserve tank or the like, and continuous automatic operation is possible.
本発明の化学メレキ方法について説明する。従来の一般
的な化学メツキ方法は次の工程からなる。The chemical melting method of the present invention will be explained. The conventional general chemical plating method consists of the following steps.
脱脂−水洗−デスマット−水洗−水洗−酸浸漬一水洗一
浸漬脱脂一水洗一活性化一水洗一水洗−（硝酸）
（硝酸）
一水洗−クロメート処理−水洗−水洗一湯浸一乾燥
本発明に従った新規化学メツキ方法は一般に次の工程か
らなる。Degreasing - Water washing - Desmutting - Water washing - Water washing - Acid soaking - Water washing - Soaking Degreasing - Water washing - Activation - Water washing - Water washing - (Nitric acid)
(Nitric acid) - Water washing - Chromate treatment - Water washing - Water washing - Hot water immersion - Drying The novel chemical plating method according to the present invention generally consists of the following steps.
脱脂−水洗−デスマット−水洗−水洗一酸浸漬−水洗−
浸漬脱脂一水洗一活性化一水洗一水洗一無電解ニッケル
ー水洗−水洗−クロメート処理−水洗一水洗一湯浸一乾
燥
すなわち本発明によれば、バシペーション工程（冷硝酸
による槽材質の活性化）がなくなる。Degreasing - Water washing - Desmutting - Water washing - Water washing Mono-acid immersion - Water washing -
Immersion degreasing - Water washing - Activation - Water washing - Water washing - Electroless nickel - Water washing - Water washing - Chromate treatment - Water washing - Water washing - Hot water soaking - Drying, that is, according to the present invention, the vacipation step (activation of the bath material with cold nitric acid) disappears.
ＳＵＳ−３０４やＳＵＳ−３１６等のステンレス鋼系の
材質の槽表面に、Ｎｉ −Ｐと反応しないオーステナイ
トを勤率よく短時間で早く生成させるためには、熱硝酸
を前記材質表面に、あたかも液をたたきつけるかのごと
く噴射することが最良であるを見出した。これは、材質
表面だけでなく、肉厚の内部まで及ぶ液のエツチング作
用により、材質内部にもオーステナイトや金属酸化物被
膜が全面的番こ多量生成するためである。In order to quickly generate austenite that does not react with Ni-P on the surface of a tank made of stainless steel materials such as SUS-304 and SUS-316, hot nitric acid is applied to the surface of the material as if it were a liquid. I have found that it is best to inject it as if hitting it. This is because a large amount of austenite or metal oxide film is formed all over the interior of the material due to the etching action of the liquid that extends not only to the surface of the material but also to the inside of the wall thickness.
この方法だと短時間（たとえば３〜５分間）の熱硝酸の
処理でよく、また、この熱硝酸は循環再使用が何回でも
できる特長がある。This method requires hot nitric acid treatment for a short time (for example, 3 to 5 minutes), and this hot nitric acid has the advantage that it can be recycled and reused any number of times.
従来の方法だと冷硝酸で一昼夜材質を処理しなければな
らず、さらにまた、これも約４０八８０時間位のメツキ
操作ごとに冷硝酸処理をしなければならないという大き
な欠点があったが、本発明に係る新方法だと一回だけの
短時間処理で半永久的に使用でき、メツキ装置の連続運
転が可能になったのである。With the conventional method, the material had to be treated with cold nitric acid all day and night, and this method also had the major drawback of having to treat with cold nitric acid every 4088 hours of plating operation. With the new method according to the present invention, it can be used semi-permanently with just one short treatment, making it possible to operate the plating equipment continuously.
好ましい実施態様の記述
本発明の好ましい実施例について添付図面参照下に詳細
に説明する。DESCRIPTION OF THE PREFERRED EMBODIMENTS Preferred embodiments of the invention will now be described in detail with reference to the accompanying drawings.
第１図は本発明あ一実施例に使用される化学ニッケルメ
ッキ槽（１）の平面図であって、その中にＮ１−Ｐメツ
キ液が入れられ、メツキ操作が行われる。メツキ液は槽
内面（９）と接触する。メツキ液の組成やメツキ操作は
従来の場合と同じであるのでその詳細な説明は省略する
が、参考のために、公知のメツキ液の組成例および作業
条件を次表に示す。FIG. 1 is a plan view of a chemical nickel plating bath (1) used in Example 1 of the present invention, in which an N1-P plating solution is poured and a plating operation is performed. The plating liquid comes into contact with the inner surface of the tank (9). Since the composition of the plating solution and the plating operation are the same as in the conventional case, a detailed explanation thereof will be omitted, but for reference, examples of compositions and working conditions of known plating solutions are shown in the following table.
メツキ゛の ・
（Ｉ） （Ｉ Ｉ）
硫酸ニッケル ２０ｇ／ ７！２５ｇ／ １次
亜りん酸ナトリウム ２４ｇ／ １２ ２０ｇ／ Ｉ
ｔ酢酸ナトリウム １０ｇ／ｆ乳
酸 ２７ｇ／７！ −
プロピオン酸 ２ｇ／ｚ −クエ
ン酸ナトリウム １０ｇ／／ｐＨ４，５
５，０
作業部度 ９０℃ ９０℃
第２図は、前記のメツキ槽（１）に本発明に従って硝酸
槽（２）を接続した状態を示す管系図である。メツキ槽
（ｉ）の上部に首振りノズル（８）を設置し、メツキ槽
（１）の槽内面（９）の処理の際に熱硝酸（温度は好ま
しくは４０〜５０℃程度）を硝酸槽（２）から循環ポン
プ（５）によって配管（６）を通じてメツキ槽（１）に
送給し、は硝酸加熱用の電熱ヒータ（３）および温度計
（温調計）（４）を設置する。メツキ槽（１）に供給さ
れた硝酸はその後に、戻り配管（１０）を通じて硝酸槽
（２）に戻る。番号（７）は槽の上部を覆うカバーであ
る。Nickel sulfate 20g/ 7!25g/ Sodium hypophosphite 24g/ 12 20g/ I
tSodium acetate 10g/f milk
Acid 27g/7! −
Propionic acid 2g/z -Sodium citrate 10g//pH 4,5
5.0 Working part temperature 90°C 90°C FIG. 2 is a pipe system diagram showing a state in which the nitric acid tank (2) is connected to the plating tank (1) according to the present invention. An oscillating nozzle (8) is installed at the top of the plating tank (i), and when treating the inner surface (9) of the plating tank (1), hot nitric acid (preferably at a temperature of about 40 to 50°C) is applied to the plating tank (1). A circulating pump (5) supplies water from the tank (2) to the plating tank (1) through piping (6), and an electric heater (3) for heating nitric acid and a thermometer (temperature controller) (4) are installed. . The nitric acid supplied to the plating tank (1) then returns to the nitric acid tank (2) through the return pipe (10). Number (7) is a cover that covers the top of the tank.
第１図は、本発明に従って使用される化学二・ノケルメ
ソキ槽の一例の略式平面図である。
第２図は、硝酸槽を接続した前記メツキ槽の略式側面図
である。
１・・・化学ニソケルメ、キ槽；２・・・硝酸槽；３・
・・電熱ヒータ；４・・・温度計；５・・・循環ポンプ
；６・・・配管；７・・・カバー；８・・・首振りノズ
ル；９・・・槽内面；１０・・・戻り配管；１１・・・
熱硝酸（温度５（１−６０℃）。FIG. 1 is a schematic plan view of an example of a chemical di-Nokelmethoxy tank used in accordance with the present invention. FIG. 2 is a schematic side view of the plating tank to which a nitric acid tank is connected. 1...Chemical nitride tank; 2...Nitric acid tank; 3.
... Electric heater; 4... Thermometer; 5... Circulation pump; 6... Piping; 7... Cover; 8... Oscillating nozzle; 9... Tank inner surface; 10...・Return piping; 11...
Hot nitric acid (temperature 5 (1-60°C).
Claims (3)
硝酸で処理することを特徴とする化学ニッケルメッキ液
槽の製作加工方法。(1) A method for manufacturing a chemical nickel plating tank, which comprises treating the inner surface of the steel-based tank material constituting the plating tank with hot nitric acid.
ごときステンレス鋼であり、熱硝酸が約４０〜５０℃の
硝酸である請求項１に記載の化学ニッケルメッキ液槽の
製作加工方法。(2) The method for manufacturing a chemical nickel plating liquid tank according to claim 1, wherein the tank material is stainless steel such as SUS-304 or SUS-316, and the hot nitric acid is nitric acid at about 40 to 50°C.
ッケルメッキ液槽を使用することを特徴とする該メッキ
液槽を利用した化学ニッケルメッキ方法。(3) A chemical nickel plating method using a chemical nickel plating bath obtained by the manufacturing method according to claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP28589790A JPH04165079A (en) | 1990-10-25 | 1990-10-25 | Method for producing and working chemical nickel plating liquid cell and chemical nickel plating method using this plating liquid cell |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP28589790A JPH04165079A (en) | 1990-10-25 | 1990-10-25 | Method for producing and working chemical nickel plating liquid cell and chemical nickel plating method using this plating liquid cell |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH04165079A true JPH04165079A (en) | 1992-06-10 |
Family
ID=17697438
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP28589790A Pending JPH04165079A (en) | 1990-10-25 | 1990-10-25 | Method for producing and working chemical nickel plating liquid cell and chemical nickel plating method using this plating liquid cell |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH04165079A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20020040702A (en) * | 2002-03-05 | 2002-05-30 | 김경수 | Jig Material for Hot-dip Galranized Metal Plate |
| CN105463418A (en) * | 2014-09-10 | 2016-04-06 | 启碁科技股份有限公司 | Metal pattern manufacturing method and substrate structure |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6419471A (en) * | 1987-07-15 | 1989-01-23 | Nec Corp | Image information processor |
| JPH0211775A (en) * | 1988-06-28 | 1990-01-16 | Aisin Seiki Co Ltd | Treatment to prevent sticking of plating metal to stainless steel which comes in contact with electroless plating liquid |
-
1990
- 1990-10-25 JP JP28589790A patent/JPH04165079A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6419471A (en) * | 1987-07-15 | 1989-01-23 | Nec Corp | Image information processor |
| JPH0211775A (en) * | 1988-06-28 | 1990-01-16 | Aisin Seiki Co Ltd | Treatment to prevent sticking of plating metal to stainless steel which comes in contact with electroless plating liquid |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20020040702A (en) * | 2002-03-05 | 2002-05-30 | 김경수 | Jig Material for Hot-dip Galranized Metal Plate |
| CN105463418A (en) * | 2014-09-10 | 2016-04-06 | 启碁科技股份有限公司 | Metal pattern manufacturing method and substrate structure |
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