JP2717041B2 - Surface treatment method for copper and copper alloy - Google Patents
Surface treatment method for copper and copper alloyInfo
- Publication number
- JP2717041B2 JP2717041B2 JP9946092A JP9946092A JP2717041B2 JP 2717041 B2 JP2717041 B2 JP 2717041B2 JP 9946092 A JP9946092 A JP 9946092A JP 9946092 A JP9946092 A JP 9946092A JP 2717041 B2 JP2717041 B2 JP 2717041B2
- Authority
- JP
- Japan
- Prior art keywords
- copper
- discoloration
- liquid
- inhibitor
- strip
- 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.)
- Expired - Fee Related
Links
Landscapes
- Preventing Corrosion Or Incrustation Of Metals (AREA)
- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
Description
【0001】[0001]
【産業上の利用分野】銅および銅合金条のインヒビター
水溶液を用いた変色防止処理方法において、インヒビタ
ーによる変色防止処理効果を損なうことなく、かつ液切
り不良による変色が発生しにくい変色防止処理方法に関
する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for preventing discoloration of copper and copper alloy strips using an aqueous inhibitor solution, without impairing the effect of the inhibitor for preventing discoloration and preventing discoloration due to poor drainage. .
【0002】[0002]
【従来の技術】銅、黄銅、りん青銅等の銅合金は、比較
的耐食性の高い金属材料であるが、その表面を大気中に
さらすと酸化膜が成長して変色に至り、商品価値が低下
することがある。この変色を防ぐために、通常インヒビ
ターとしてベンゾトリアゾール系の化合物を含む水溶液
に浸漬して変色防止処理を施す。2. Description of the Related Art Copper alloys such as copper, brass, and phosphor bronze are relatively high corrosion-resistant metal materials. However, when the surface is exposed to the air, an oxide film grows, resulting in discoloration and a reduction in commercial value. May be. In order to prevent this discoloration, the substrate is usually immersed in an aqueous solution containing a benzotriazole-based compound as an inhibitor to perform a discoloration prevention treatment.
【0003】条製品の製造工程では各種の熱処理と圧延
加工が行われるが、加工途中でも適宜一時防錆として変
色防止処理が行われる。例えば大気焼鈍ラインで最終の
湯洗槽にベンゾトリアゾール等のインヒビターを適宜添
加することにより、変色防止処理したり、圧延後、圧延
油を脱脂する工程で変色防止処理することもある。[0003] Various heat treatments and rolling processes are performed in the production process of a strip product, and a discoloration prevention process is appropriately performed as temporary rust prevention even during the processing. For example, a discoloration preventing treatment may be performed by appropriately adding an inhibitor such as benzotriazole to a final hot water washing tank in an air annealing line, or a discoloring preventing treatment may be performed in a step of degreasing rolling oil after rolling.
【0004】ところがインヒビター水溶液により変色防
止処理する場合、処理液から条を引き上げた後、ロール
やエアーナイフ等により、できる限り条表面の液膜を切
った後乾燥するのが通例である。ところがこの液切りお
よび乾燥が不均一であると、これによる変色が外観の斑
として認められることがある。この変色は処理直後には
目視で認められなくても、数日経過すると明確になり不
良品になることがある。[0004] However, in the case of discoloration prevention treatment using an aqueous inhibitor solution, it is customary to pull up the strip from the processing solution, cut the liquid film on the strip surface as much as possible with a roll or an air knife, and then dry. However, if the drainage and drying are not uniform, discoloration due to the drainage and drying may be recognized as uneven appearance. Even if this discoloration is not visually observed immediately after the treatment, the discoloration becomes clear after several days and may result in a defective product.
【0005】[0005]
【発明が解決しようとする課題】本発明は銅および銅合
金条の変色防止処理工程における処理の不均一に起因す
る変色を抑制する方法を提供しようとするものである。SUMMARY OF THE INVENTION It is an object of the present invention to provide a method for suppressing discoloration caused by uneven treatment in a treatment for preventing discoloration of copper and copper alloy strips.
【0006】[0006]
【課題を解決するための手段】上記課題を解決するため
の本発明の方法は銅および銅合金の条を、インヒビター
を含む変色防止処理液に浸漬し、引き上げた後、液切り
ロール、エアーナイフ等により液を切る工程を含む表面
処理方法において、変色防止処理液から引き上げた後、
液を切る工程の前に電気伝導率が5μS/cm以下の純
水により2秒以内の時間の洗浄を行う銅および銅合金の
表面処理方法である。According to a method of the present invention, a strip of copper and a copper alloy is immersed in a discoloration-preventing treatment solution containing an inhibitor. In the surface treatment method including the step of cutting off the liquid, etc., after withdrawing from the discoloration prevention treatment liquid,
This is a surface treatment method for copper and a copper alloy in which cleaning is performed for 2 hours or less with pure water having an electric conductivity of 5 μS / cm or less before a step of draining the liquid.
【0007】条の連続的な変色防止処理は脱脂処理、酸
洗等の後水洗されてから、即ち条の表面はできるだけ清
浄な状態にされた後、変色防止処理液に浸漬処理される
のが通例である。ところが水洗液中には前工程から持ち
込まれた各種不純物が存在し、変色防止処理液に持ち込
まれる。また、条表面は完全に活性化することが困難で
あり、表面酸化物や微量の有機物により被覆されてい
る。これらの条の表面皮膜は変色防止処理液を汚染する
ことになる。こうした変色防止処理液の汚染物は変色防
止処理後液切りが不均一であると、条表面に不均一に残
留し変色の原因となる。液切りロールの場合、条により
ロール表面の損耗が不均一で、甚だしい場合は傷がつく
ことがある。液切りロール表面の凹凸は液切り不良の原
因となるが、これを完全に管理することは困難である。
またエアーナイフを用いた場合も条の全幅にわたり常時
均一に液を切ることは困難である。そのため公知のいか
なる液切り方法を用いても、長時間操業を続けると液切
りの均一性は低下する。そこで変色防止処理後純水で再
度、条表面を洗浄すると、液切り不良に起因する変色は
ほとんどなくすことができる。純水とはイオン交換水ま
たはイオン交換と蒸留を行うことにより、少なくとも上
水または井戸水などから電解質を除去したもので、電気
伝導率5μS/cm以下であることが必要である。電気
伝導率がこれ以上になると、液切りの不均一が変色にな
り易くなる。水の電気伝導率は下がるほど変色防止上は
有利であり下限は特に定めない。[0007] In the continuous discoloration prevention treatment, the strip is preferably immersed in a discoloration prevention treatment liquid after being washed with water after degreasing, pickling, etc., that is, after the surface of the strip is as clean as possible. It is customary. However, various impurities brought in from the previous process exist in the washing liquid, and are brought into the discoloration prevention treatment liquid. Further, it is difficult to completely activate the strip surface, and the strip surface is covered with a surface oxide or a trace amount of an organic substance. The surface coating of these strips contaminates the anti-tarnish treatment solution. If the contaminants of the discoloration prevention treatment liquid are not uniformly drained after the discoloration prevention treatment, the contaminants remain unevenly on the strip surface and cause discoloration. In the case of the draining roll, the surface of the roll may be unevenly worn due to the strips, and may be damaged in severe cases. Irregularities on the surface of the draining roll cause poor draining, but it is difficult to completely control this.
Also, even when an air knife is used, it is difficult to constantly and uniformly cut the liquid over the entire width of the strip. Therefore, even if any known draining method is used, if the operation is continued for a long time, the uniformity of the drainage is reduced. Therefore, when the strip surface is washed again with pure water after the discoloration prevention treatment, discoloration due to poor drainage can be almost eliminated. Pure water is ion-exchanged water or ion-exchanged and distilled water to remove the electrolyte from at least tap water or well water, and it is necessary that the electric conductivity be 5 μS / cm or less. If the electrical conductivity is higher than this, the unevenness of the liquid drainage tends to change the color. The lower the electric conductivity of water, the more advantageous in preventing discoloration, and the lower limit is not particularly defined.
【0008】しかし、インヒビターによる保護皮膜は、
特に変色防止処理直後に水洗を過度に行うと、保護性が
低下するため水洗時間は2秒以内で行わなければならな
い。ここで水洗時間とは洗浄液を条にかけた後、液切り
するまでの時間を示す。However, the protective film formed by the inhibitor is
In particular, if the washing is performed excessively immediately after the discoloration prevention treatment, the protective property is reduced, so that the washing time must be performed within 2 seconds. Here, the term “water washing time” refers to the time from the application of the cleaning solution to the drainage until the drainage.
【0009】図1は本発明の方法を具体的に示す説明図
である。すなわち、変色防止処理液1が入っている変色
防止処理槽2の中へ条5を浸漬しながら送り、この変色
防止処理槽2から引き上げた後、スプレー洗浄ノズル3
から噴出する洗浄液で洗浄した直後、液切りロール4を
通して条5の洗浄液を液切りする方法である。FIG. 1 is an explanatory diagram specifically showing the method of the present invention. That is, the strip 5 is fed while being immersed into the discoloration prevention treatment tank 2 containing the discoloration prevention treatment liquid 1, pulled up from the discoloration prevention treatment tank 2,
This is a method in which the cleaning liquid of the strip 5 is drained through the draining roll 4 immediately after washing with the cleaning liquid ejected from the nozzle.
【0010】本発明では洗浄溶液は常に新しい水を直接
条にかけることにより、洗浄液の純度を保つことができ
る。In the present invention, the purity of the cleaning solution can be maintained by always applying fresh water directly to the cleaning solution.
【0011】また、同洗浄液中にインヒビターを添加す
ると変色防止皮膜の保護性を低下することなく、条表面
を洗浄化することができる。When an inhibitor is added to the cleaning solution, the surface of the strip can be cleaned without lowering the protection of the anti-discoloration film.
【0012】洗浄液にはインヒビターの他、界面活性
剤、アルキルアミン等の変色防止助剤、グリコール類等
の潤滑剤などを適宜添加するのは特に差し支えない。In addition to the inhibitor, a surfactant, a discoloration preventing auxiliary such as an alkylamine, a lubricant such as a glycol, or the like may be appropriately added to the cleaning liquid.
【0013】そして、変色防止処理後の洗浄は洗浄槽を
設けると、水質の管理が必要となるが、変色防止処理後
液切りまでの間に、スプレー等で条表面に常に新鮮な純
水、または純水で調整されたインヒビターを含む洗浄液
をかけると、洗浄液の不純物もなく、しかも少量の洗浄
液で液切り不良による変色問題を効果的に解決できる。If a washing tank is provided for washing after the discoloration prevention treatment, it is necessary to control the water quality. Alternatively, when a cleaning solution containing an inhibitor adjusted with pure water is applied, there is no impurity in the cleaning solution, and a small amount of the cleaning solution can effectively solve the problem of discoloration due to poor drainage.
【0014】変色防止処理液または洗浄液に用いるイン
ヒビターとしては、銅および銅合金の変色防止剤として
公知のものであれば、特に差し支えない。最も汎用的に
用いられているのは、ベンゾトリアゾール(1,2,3
−benzotriazole,BTA)であり、その
誘導体も有効である。銅および銅合金のインヒビターと
し知られるBTA誘導体の代表例として、4−meth
yl−1.H−benzotoriazole(tol
yltriazole,TTA)、4−carboxy
−1.H−benzotriazole、sodium
um−tolyltriazole、5−methyl
−1.H−benzotriazole(tolylt
riazole,TTA)、benzotriazol
e buthyl ester,silver ben
zotriazoleなどがあげられる。そのほかin
dazole,benzimidazole,indo
le,toriazine等およびそれらの誘導体等が
インヒビターとして利用できる。The inhibitor used in the discoloration preventing treatment solution or the cleaning solution is not particularly limited as long as it is known as a discoloration inhibitor for copper and copper alloys. The most commonly used is benzotriazole (1,2,3
-Benzotriazole, BTA), and derivatives thereof are also effective. A representative example of a BTA derivative known as an inhibitor of copper and copper alloys is 4-meth.
yl-1. H-benzotriazole (tol
yltriazole, TTA), 4-carboxy
-1. H-benzotriazole, sodium
um-tolyltriazole, 5-methyl
-1. H-benzotriazole (tolylt
riazole, TTA), benzotriazol
e butyl ester, silver ben
zotriazole and the like. In addition
dazole, benzimidizole, indo
le, triazine and the like and derivatives thereof can be used as inhibitors.
【0015】変色防止処理液には、インヒビターだけで
はなく、水への溶解度の低いインヒビターを用いる場合
にはアミン系化合物や界面活性剤を添加すること、変色
防止助剤としてアルキルアミン類、メルカプタン類等を
添加すること、あるいはその後の加工工程を考慮してグ
リコール類等の潤滑剤を変色防止処理液に添加すること
などは本発明の効果を妨げない。In the discoloration preventing treatment solution, not only an inhibitor but also an amine compound or a surfactant is used when an inhibitor having low solubility in water is used. Alkylamines and mercaptans are used as discoloration preventing aids. The addition of a lubricant such as a glycol to the discoloration prevention treatment liquid in consideration of the subsequent processing steps does not hinder the effects of the present invention.
【0016】水洗水またはインヒビターを含む最終の洗
浄液に塩素が1ppm以上含むと液切りの不均一による
変色が発生し易くなる。すなわち、塩素は井戸水や水道
水には通常5ppm以上含まれているが、塩素は銅の腐
食媒として作用が大きく、これが1以上含まれる水溶液
では、液切り不良や乾燥の不均一による変色が発生し易
くなる。If chlorine is contained in the washing water or the final washing liquid containing the inhibitor in an amount of 1 ppm or more, discoloration due to uneven drainage is liable to occur. In other words, chlorine is generally contained in well water and tap water in an amount of 5 ppm or more, but chlorine has a large effect as a corrosive medium for copper. In an aqueous solution containing one or more chlorine, discoloration due to poor drainage or uneven drying occurs. Easier to do.
【0017】また、洗浄効果は洗浄液の温度によらない
が、液切り後乾燥する場合は、乾燥を効率的に行う上で
温度は60〜80℃がよい。Although the cleaning effect does not depend on the temperature of the cleaning liquid, when drying after draining the liquid, the temperature is preferably from 60 to 80 ° C. for efficient drying.
【0018】本発明は水溶液による条の連続変色防止処
理後の洗浄方法に関するものであり、変色防止処理の前
工程(同一ライン内か別ラインかを問わない)について
は制約されず有効である。たとえばアルカリ浸漬脱脂、
電解脱脂、酸洗、熱処理等の処理が適宜行われたものに
ついて適応できる。The present invention relates to a cleaning method after a continuous discoloration prevention treatment of a strip with an aqueous solution, and is effective without any restriction on a pre-process (whether in the same line or on another line) of the discoloration prevention treatment. For example, alkaline immersion degreasing,
It can be applied to those which have been subjected to processes such as electrolytic degreasing, pickling and heat treatment as appropriate.
【0019】以下、実施例および比較例によって、本発
明を具体的に説明する。Hereinafter, the present invention will be specifically described with reference to Examples and Comparative Examples.
【0020】[0020]
【実施例】板厚0.2mm、幅600mmのりん青銅条
(Cu−8%Sn−0.1%P)の圧延油の付着した圧
延材をアルカリ浸漬脱脂、水洗、変色防止処理、乾燥と
連続脱脂ラインにより、脱脂および変色防止処理を施し
た。各種条件で処理した後、耐変色性を試験した結果を
表1に示す。EXAMPLE Rolled material having a rolling oil of phosphor bronze strip (Cu-8% Sn-0.1% P) having a thickness of 0.2 mm and a width of 600 mm adhered thereto was subjected to alkali immersion degreasing, washing with water, discoloration prevention treatment, and drying. Degreasing and discoloration prevention treatment were performed by a continuous degreasing line. After treatment under various conditions, the results of a test of color fastness are shown in Table 1.
【0021】通板試験条件は以下に示すものである。液
切り後は乾燥させてコイル状に巻き取った後、サンプリ
ングして硫化水素ガスによる変色防止効果、および液切
り不良による変色の発生の有無を評価した。The passing test conditions are as follows. After draining the liquid, it was dried and wound into a coil, and then sampled to evaluate the effect of preventing discoloration by the hydrogen sulfide gas and the occurrence of discoloration due to poor drainage.
【0022】脱脂及び変色防止処理 1)脱脂液 組成 炭酸ナトリウム 20
g/L りん酸第三ナトリウム 35g/L トリポリリン酸ナトリウム 5g/L メタケイ酸ナトリウム 30g/L 界面活性剤 10g/L 温度 50℃ 時間 10秒 2)水洗 スプレー水洗 時間 3秒 3)変色防止処理 組成 ベンゾトリアゾール 10
0ppm 温度 70℃ 時間 3秒 4)洗浄 図1に示すように変色防止処理液1から条
5が引き上げられた後、液切りロール4により液を切ら
れるまでの間に、スプレー洗浄ノズル3を設置し純水ま
たは純水より調整されたインヒビター溶液をかけた。洗
浄時間即ちスプレーをかけてから液切りロール4で液を
切るまでの時間は、条5の通板速度またはスプレー洗浄
ノズル3とロール4の配置を変えることにより調整し
た。 Degreasing and Discoloration Prevention Treatment 1) Degreasing Solution Composition Sodium Carbonate 20
g / L tertiary sodium phosphate 35 g / L sodium tripolyphosphate 5 g / L sodium metasilicate 30 g / L surfactant 10 g / L temperature 50 ° C. time 10 seconds 2) water washing spray water washing time 3 seconds 3) discoloration preventing treatment composition benzo Triazole 10
0 ppm Temperature 70 ° C. Time 3 seconds 4) Cleaning As shown in FIG. 1, after the strip 5 is pulled up from the discoloration prevention treatment liquid 1, the spray cleaning nozzle 3 is installed between the time when the liquid is cut off by the liquid discharge roll 4. Then, pure water or an inhibitor solution adjusted from pure water was applied. The washing time, that is, the time from the application of the spray to the removal of the liquid by the liquid removing roll 4 was adjusted by changing the passing speed of the strip 5 or the arrangement of the spray cleaning nozzle 3 and the roll 4.
【0023】スプレーによる液供給量は材料の600m
m幅に対し20L/minの流量で一定とした。The amount of liquid supplied by spraying is 600 m of material.
The flow rate of 20 L / min was constant with respect to the m width.
【0024】洗浄液の温度は70℃とした。The temperature of the cleaning liquid was 70 ° C.
【0025】5)液切り ネオプレン性の200mmφ
のゴムロールで条の両面から、抑えて、液切りを行っ
た。液切り不良の影響を見る目的でゴムロール表面に
は、深さ0.5mm、長さ200mmの傷のあるものを
用いた。5) Drainer Neoprene 200 mmφ
The liquid was drained while holding down both sides of the strip with a rubber roll. For the purpose of observing the effect of poor drainage, a rubber roll surface having a depth of 0.5 mm and a length of 200 mm was used.
【0026】耐変色性評価方法 りん青銅条を短冊状試験片に切り出し、3ppmH
2S,40℃、50%RHの硫化水素雰囲気に20分間
暴露し、試験片の硫化変色の程度を目視により評価し
た。Discoloration resistance evaluation method A phosphor bronze strip was cut into strip-shaped test pieces, and 3 ppm H
The specimen was exposed to a hydrogen sulfide atmosphere at 2 S, 40 ° C. and 50% RH for 20 minutes, and the degree of discoloration of the specimen by sulfurization was visually evaluated.
【0027】液切り不良による変色の発生の評価 各通板条件毎にりん青銅条を通板幅(600mm)で1
mの長さ切り出し、1週間室内暴露して、液切り不良に
起因する変色の発生の有無を目視観察した。 Evaluation of Discoloration due to Poor Drainage Phosphor bronze strip with a passing width (600 mm) of 1 for each passing condition
The length of m was cut out and exposed indoors for one week, and the occurrence of discoloration due to poor drainage was visually observed.
【0028】[0028]
【表1】 [Table 1]
【0029】[0029]
【発明の効果】以上説明したように本発明によれば、銅
および銅合金条の変色防止処理工程において、インヒビ
ターによる変色防止処理効果を低下させることなく、液
切り不良による変色の発生を防止することができる。As described above, according to the present invention, in the step of preventing discoloration of copper and copper alloy strips, the occurrence of discoloration due to poor drainage is prevented without reducing the effect of the inhibitor to prevent discoloration. be able to.
【図1】本発明の一具体例の説明図である。FIG. 1 is an explanatory diagram of a specific example of the present invention.
1 変色防止処理液 2 変色防止処理槽 3 スプレー洗浄ノズル 4 液切りロール 5 条 1 Discoloration prevention treatment liquid 2 Discoloration prevention treatment tank 3 Spray cleaning nozzle 4 Drip roll 5
───────────────────────────────────────────────────── フロントページの続き (56)参考文献 特開 平3−188289(JP,A) 特開 昭50−3032(JP,A) 特公 昭61−24471(JP,B2) ──────────────────────────────────────────────────続 き Continuation of the front page (56) References JP-A-3-188289 (JP, A) JP-A-50-3032 (JP, A) JP-B-61-24471 (JP, B2)
Claims (3)
含む変色防止処理液に浸漬し、引き上げた後、液切りロ
ール、エアーナイフ等により液を切る工程を含む表面処
理方法において、変色防止処理液から引き上げた後、液
を切る工程の前に電気伝導率が5μS/cm以下の純水
により2秒以内の時間の洗浄を行うことを特徴とする銅
および銅合金の表面処理方法。1. A surface treatment method comprising a step of immersing copper and copper alloy strips in a discoloration preventing treatment solution containing an inhibitor, pulling up the strip, and then cutting off the liquid with a draining roll, an air knife or the like. A surface treatment method for copper and a copper alloy, comprising washing with pure water having an electric conductivity of 5 μS / cm or less for 2 seconds or less before a step of removing the solution from the solution.
の純水に銅および銅合金の変色防止インヒビターおよび
その助剤を添加した水溶液であることを特徴とする請求
項1記載の銅および銅合金の表面処理方法。2. The copper and copper according to claim 1, wherein the cleaning liquid is an aqueous solution obtained by adding an inhibitor for preventing discoloration of copper and a copper alloy and an auxiliary thereof to pure water having an electric conductivity of 5 μS / cm or less. Alloy surface treatment method.
ることを特徴とする請求項1または請求項2記載の銅お
よび銅合金の表面処理方法。3. The surface treatment method for copper and copper alloy according to claim 1, wherein the concentration of chlorine in the cleaning solution is 1 ppm or less.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP9946092A JP2717041B2 (en) | 1992-04-20 | 1992-04-20 | Surface treatment method for copper and copper alloy |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP9946092A JP2717041B2 (en) | 1992-04-20 | 1992-04-20 | Surface treatment method for copper and copper alloy |
Publications (2)
Publication Number | Publication Date |
---|---|
JPH05295571A JPH05295571A (en) | 1993-11-09 |
JP2717041B2 true JP2717041B2 (en) | 1998-02-18 |
Family
ID=14247931
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP9946092A Expired - Fee Related JP2717041B2 (en) | 1992-04-20 | 1992-04-20 | Surface treatment method for copper and copper alloy |
Country Status (1)
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JP (1) | JP2717041B2 (en) |
Families Citing this family (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102732874B (en) * | 2012-06-28 | 2014-04-16 | 中宇建材集团有限公司 | Surface treatment production line of copper products |
JPWO2014156362A1 (en) * | 2013-03-28 | 2017-02-16 | 古河電気工業株式会社 | Surface treatment electrolytic copper foil |
WO2014156361A1 (en) * | 2013-03-28 | 2014-10-02 | 古河電気工業株式会社 | Surface-treated copper foil |
JP6115311B2 (en) * | 2013-05-24 | 2017-04-19 | 住友金属鉱山株式会社 | Surface treatment method and method for producing metallized resin film using the same |
-
1992
- 1992-04-20 JP JP9946092A patent/JP2717041B2/en not_active Expired - Fee Related
Also Published As
Publication number | Publication date |
---|---|
JPH05295571A (en) | 1993-11-09 |
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