JP3426489B2 - Electrolytic treatment bath mainly composed of chromic anhydride - Google Patents
Electrolytic treatment bath mainly composed of chromic anhydrideInfo
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- JP3426489B2 JP3426489B2 JP00128898A JP128898A JP3426489B2 JP 3426489 B2 JP3426489 B2 JP 3426489B2 JP 00128898 A JP00128898 A JP 00128898A JP 128898 A JP128898 A JP 128898A JP 3426489 B2 JP3426489 B2 JP 3426489B2
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- mol
- concentration
- chromic anhydride
- treatment bath
- electrolytic
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Description
【０００１】[0001]
【発明の属する技術分野】本発明は、無水クロム酸を主
成分とする電解処理浴に関するものである。TECHNICAL FIELD The present invention relates to an electrolytic treatment bath containing chromic anhydride as a main component.
【０００２】[0002]
【従来の技術】無水クロム酸を主成分とする電解クロム
めっき浴中及び電解クロム酸処理浴中に助剤として、ハ
ロゲン化物の一種または二種以上、硫化物の一種または
二種以上を添加し、組成がハロゲン化物／Ｃｒのモル比
で１／１００〜１／１０、硫化物／Ｃｒのモル比で１／
２０００〜１／５００、硫化物／ハロゲン化物の比が１
／５０以下及び不可避的不純物からなる浴で、鋼帯表面
に陰極電解によって金属クロムを主体とするめっきを施
し、次いで電解クロム酸処理を施してティンフリー鋼板
（クロムめっき鋼板）の製造方法が特開平９−２８７０
９０号公報に開示されている。2. Description of the Related Art One or more halides and one or more sulfides are added as an auxiliary agent in an electrolytic chrome plating bath containing chromic anhydride as a main component and in an electrolytic chromic acid treatment bath. , The composition is a halide / Cr molar ratio of 1/100 to 1/10, and a sulfide / Cr molar ratio of 1 /.
2000-1 / 500, sulfide / halide ratio is 1
/ 50 or less and unavoidable impurities in the bath, the surface of the steel strip is subjected to cathodic electroplating with metallic chromium as the main component, followed by electrolytic chromic acid treatment to produce a tin-free steel plate (chromium plated steel plate). Kaihei 9-2870
No. 90 publication.
【０００３】[0003]
【発明が解決しようとする課題】上記のごとき、クロム
めっき鋼板（ティンフリー鋼板）の製造方法において
は、めっき鋼板の表面明度及び耐レトルト処理性に優れ
たクロムめっき鋼板を製造することができる。しかし
て、このようなクロムめっき鋼板を安定して製造するた
めには、電解クロムめっき浴及び電解クロム酸処理浴と
して、電解による金属クロム、電解クロム酸が高効率で
析出でき、しかも浴が長期に亘って低汚染度で安定した
浴組成であることが要求されることになる。本発明は、
このような要求を有利に満足させるためになされたもの
であり、表面明度等に優れたクロムめっき鋼板を安定し
て製造することのできる無水クロム酸を主成分とする電
解クロム処理浴を提供することを目的とするものであ
る。As described above, in the method for producing a chrome-plated steel sheet (tin-free steel sheet), it is possible to produce a chrome-plated steel sheet having excellent surface brightness and resistance to retort treatment. Therefore, in order to stably produce such a chromium-plated steel sheet, electrolytic chromium plating baths and electrolytic chromic acid treatment baths can deposit metal chromium and electrolytic chromic acid by electrolysis with high efficiency, and the bath can be used for a long time. Therefore, it is required that the bath composition has a low pollution degree and a stable bath composition. The present invention is
The present invention has been made in order to advantageously satisfy such requirements, and provides an electrolytic chromium treatment bath containing chromic anhydride as a main component, which can stably produce a chromium-plated steel sheet excellent in surface brightness and the like. That is the purpose.
【０００４】[0004]
【課題を解決するための手段】本発明の特徴とするとこ
ろは、無水クロム酸濃度０．３〜２．５モル／ｌ、硫化
物／Ｃｒモル比１／２０００〜１／５００からなる電解
クロムめっき浴中のフッ素イオン濃度０．０３〜０．３
モル／ｌ、フッ素イオン／Ｆｅ3+イオンモル比４．０以
上にしたことを特徴とする無水クロム酸を主成分とする
電解処理浴。及び無水クロム酸濃度０．３〜２．５モル
／ｌ、硫化物／Ｃｒモル比１／２０００〜１／５００か
らなる電解クロム酸処理浴中のフッ素イオン濃度０．３
０モル／ｌ以下、フッ素イオン／Ｆｅ3+イオンモル比
４．０以上にしたことを特徴とする無水クロム酸を主成
分とする電解処理浴である。The feature of the present invention resides in that electrolytic chromium having a chromic anhydride concentration of 0.3 to 2.5 mol / l and a sulfide / Cr molar ratio of 1/2000 to 1/500. Fluorine ion concentration in plating bath 0.03 to 0.3
Mol / l, fluorine ion / Fe 3+ ion molar ratio of 4.0 or more, an electrolytic treatment bath containing chromic anhydride as a main component. And a fluorine ion concentration of 0.3 in the electrolytic chromic acid treatment bath having a chromic anhydride concentration of 0.3 to 2.5 mol / l and a sulfide / Cr molar ratio of 1/2000 to 1/500.
It is an electrolytic treatment bath containing chromic anhydride as a main component, which has a molar ratio of fluorine ion / Fe 3+ ion of 4.0 or more and 0 mol / l or less.
【０００５】[0005]
【発明の実施の形態】上記のごとく、無水クロム酸濃度
０．３〜２．５モル／ｌで、通常製造されている片面５
０〜２００ｍｇ／ｍ2 の金属クロムを効率的に析出して
めっきすることができる好ましい範囲である。また、め
っき時に金属クロム表面に水和酸化クロム層を５〜３０
ｍｇ／ｍ2 （金属クロム換算）析出生成することができ
るものである。BEST MODE FOR CARRYING OUT THE INVENTION As described above, one side 5 which is normally manufactured with a chromic anhydride concentration of 0.3 to 2.5 mol / l.
This is a preferable range in which 0 to 200 mg / m 2 of metallic chromium can be efficiently deposited and plated. In addition, a hydrated chromium oxide layer is formed on the surface of metallic chromium at the time of plating by 5 to 30.
mg / m 2 (as metal chromium) can be generated by precipitation.
【０００６】浴中の硫化物濃度としては、硫化物／Ｃｒ
モル比で１／２０００未満と硫化物が低濃度になると、
金属クロム等の析出効果が低下して触媒機能が不十分に
なる。また、１／５００超と高濃度になると水和酸化ク
ロム層中への共析量が増加して、耐レトルト性等を劣化
させることになり好ましくない。更に、硫酸イオン濃度
としては１．３０×１０-3モル／ｌ以下にすることによ
って、後述のごとき弗化物との相互作用により好ましい
触媒機能を発揮して、金属クロム及び水和酸化クロム層
の析出効率を向上することができる。The sulfide concentration in the bath is sulfide / Cr
When the concentration of sulfide is low and the molar ratio is less than 1/2000,
The effect of precipitating metal chromium and the like is reduced and the catalytic function becomes insufficient. On the other hand, if the concentration is higher than 1/500, the amount of eutectoid in the hydrated chromium oxide layer increases, which deteriorates the retort resistance and the like, which is not preferable. Further, when the sulfate ion concentration is set to 1.30 × 10 −3 mol / l or less, a preferable catalytic function is exhibited by the interaction with fluoride as described later, and the metal chromium and hydrated chromium oxide layers are formed. The deposition efficiency can be improved.
【０００７】弗化物としては、例えばＮａＦ、ＫＦ、Ｎ
Ｈ4 Ｆ、ＨＦ一種または二種以上を添加することがで
き、電解クロムめっき浴においては、浴中のフッ素イオ
ン濃度は、フッ素イオン濃度０．０３〜０．３モル／ｌ
の添加量で金属クロムめっきと同時に水和酸化クロム層
を生成することができる。即ち、０．０３モル／ｌ未満
であると、水和酸化クロム層の生成が不均一になり表面
明度にむらが発生することがあり好ましくない。また、
０．３モル／ｌ超になると水和酸化クロム層の析出効率
が低下することがあり好ましくない。また、電解クロム
酸処理浴においては、浴中のフッ素イオン濃度０．３モ
ル／ｌ以下の添加量で水和酸化クロム層を生成すること
ができる。即ち、０．３モル／ｌ超になると電解クロム
めっき浴と同様に水和酸化クロム層の析出効率が低下す
ることがあり好ましくない。ただし、電解クロムめっき
浴に比べて電解処理時の電流密度が低いため、浴中のフ
ッ素イオン濃度が少なくても、均一な水和酸化クロム層
を安定して生成することができる。Examples of fluorides include NaF, KF and N
H 4 F, HF may be added alone or in combination of two or more. In the electrolytic chromium plating bath, the concentration of fluorine ions in the bath is 0.03 to 0.3 mol / l.
It is possible to form a hydrated chromium oxide layer at the same time as metal chromium plating with the addition amount of. That is, if it is less than 0.03 mol / l, the formation of the hydrated chromium oxide layer becomes non-uniform and unevenness in the surface brightness may occur, which is not preferable. Also,
If it exceeds 0.3 mol / l, the precipitation efficiency of the hydrated chromium oxide layer may decrease, which is not preferable. Further, in the electrolytic chromic acid treatment bath, a hydrated chromium oxide layer can be formed with an addition amount of the fluorine ion concentration in the bath of 0.3 mol / l or less. That is, if it exceeds 0.3 mol / l, the deposition efficiency of the hydrated chromium oxide layer may be reduced as in the electrolytic chromium plating bath, which is not preferable. However, since the current density during electrolytic treatment is lower than that in the electrolytic chromium plating bath, a uniform hydrated chromium oxide layer can be stably formed even if the concentration of fluorine ions in the bath is low.
【０００８】フッ素イオン／Ｆｅ3+イオンモル比は、
４．０以上とＦｅ3+イオンを低濃度にすることが必要で
ある。即ち、４．０未満の高濃度になると、水和酸化ク
ロム層の生成が不均一になりむらが発生し易くなるとと
もに、金属クロムの析出効率が極端に低下して、所定の
金属クロムめっき量を確保するためにめっき時間を長く
することになる。従って、通板速度を低下させて対処す
ることとなり生産性を低下させることになる。The fluorine ion / Fe 3+ ion molar ratio is
It is necessary to set the Fe 3+ ion concentration to 4.0 or more to a low concentration. That is, when the concentration is less than 4.0, the formation of the hydrated chromium oxide layer becomes non-uniform and unevenness is likely to occur, and the deposition efficiency of metal chromium is extremely reduced, resulting in a predetermined metal chromium plating amount. Therefore, the plating time will be lengthened in order to ensure Therefore, the stripping speed is reduced to deal with the problem, and the productivity is reduced.
【０００９】このような浴組成の好ましい範囲を数式で
示すと、ＣｒＯ3 濃度モル／ｌ÷〔硫酸濃度モル／ｌ＋
弗化物濃度モル／ｌ−（１．７〜２．３）×Ｆｅ3+濃度
モル／ｌ〕＝７．５×１８．０の数式を満足する浴組成
で操業することによって、表面明度、耐レトルト性等に
優れたクロムめっき鋼板を得ることができる。A preferable range of such a bath composition is shown by a mathematical expression. CrO 3 concentration mol / l ÷ [sulfuric acid concentration mol / l +
Fluoride concentration mol / l− (1.7 to 2.3) × Fe 3+ concentration mol / l] = 7.5 × 18.0 It is possible to obtain a chrome-plated steel sheet having excellent retort properties and the like.
【００１０】操業に際しては、浴温２５〜６０℃、電流
密度１５〜１５０Ａ／ｄｍ2 で鋼帯を陰極として通電す
ることによって、鋼帯片面に５０〜２００ｍｇ／ｍ2 の
金属クロムとその上層に５〜３０ｍｇ／ｍ2(金属クロム
換算）の水和酸化クロム層からなる表面明度、耐レトル
ト性等に優れたクロムめっき鋼板を安定して製造するこ
とができるものである。During operation, the steel strip is supplied with electricity as a cathode at a bath temperature of 25 to 60 ° C. and a current density of 15 to 150 A / dm 2 to form 50 to 200 mg / m 2 of metallic chromium on one side of the steel strip and its upper layer. It is possible to stably produce a chrome-plated steel sheet having a surface brightness, a retort resistance and the like, which is composed of a hydrated chromium oxide layer of 5 to 30 mg / m 2 (as metal chromium).
【００１１】このように金属クロムめっきと同時にその
上層に水和酸化クロム層を生成させて製品にすることが
できるが、より一層表面明度、耐レトルト性等を向上す
るためには、上記のごとくめっき時に生成した水和酸化
クロム層をめっき後もめっき液に浸漬することによって
除去した後、前記のごとき浴組成で硫化物を添加するこ
となく、不純物として混入する程度とした浴組成の電解
処理浴へ導き、電流密度の制御によって金属クロムめっ
き層の上層に５〜３０ｍｇ／ｍ2 （金属クロム換算）の
水和酸化クロム層を新たに生成することにより、表面明
度、耐レトルト性等を向上することができる。As described above, a hydrated chromium oxide layer can be formed as an upper layer simultaneously with metal chromium plating to obtain a product, but in order to further improve the surface brightness, retort resistance, etc., as described above. After removing the hydrated chromium oxide layer formed during plating by immersing it in a plating solution after plating, electrolytic treatment of a bath composition such that the above bath composition is mixed as an impurity without adding sulfides The surface brightness and retort resistance are improved by introducing a hydrated chromium oxide layer of 5 to 30 mg / m 2 (calculated as metallic chromium) on top of the metallic chromium plating layer by guiding it to the bath and controlling the current density. can do.
【００１２】[0012]
【実施例】次に、本発明の実施例を比較例とともに挙げ
る。実施例は、表１〜４。比較例は、表５〜８で、比較
例の１〜６は、フッ素イオン濃度が本発明外。７〜１３
は、フッ素イオン／Ｆｅ3+イオンのモル比が本発明外。
１４〜１８は、フッ素イオン濃度とフッ素イオン／Ｆｅ
3+イオンのモル比が本発明外である。実施例及び比較例
共に１〜９は、金属クロムめっきと同時にその表面に水
和酸化クロム層を生成した。１０〜１８は、金属クロム
めっき後、同組成浴に５秒以上浸漬して表面の水和酸化
クロム層を除去し、次いで酸化物生成浴へ導き、新たに
水和酸化クロム層を生成した。EXAMPLES Next, examples of the present invention will be given together with comparative examples. Examples are Tables 1-4. Comparative examples are shown in Tables 5 to 8. In Comparative examples 1 to 6, the fluorine ion concentration is outside the present invention. 7-13
The fluorine ion / Fe 3+ ion molar ratio is outside the scope of the present invention.
14 to 18 are fluorine ion concentration and fluorine ion / Fe
The molar ratio of 3+ ions is outside the scope of the present invention. In both Examples and Comparative Examples 1 to 9, the hydrated chromium oxide layer was formed on the surface of the metal chromium plating at the same time. Samples Nos. 10 to 18 were plated with metal chromium and then immersed in a bath having the same composition for 5 seconds or longer to remove the hydrated chromium oxide layer on the surface, and then led to the oxide forming bath to newly form a hydrated chromium oxide layer.
【００１３】[0013]
【表１】 [Table 1]
【００１４】[0014]
【表２】（表１のつづき） [Table 2] (Continued from Table 1)
【００１５】[0015]
【表３】（表２のつづき） [Table 3] (Continued from Table 2)
【００１６】[0016]
【表４】（表３のつづき） [Table 4] (Continued from Table 3)
【００１７】[0017]
【表５】 [Table 5]
【００１８】[0018]
【表６】（表５のつづき） [Table 6] (Continued from Table 5)
【００１９】[0019]
【表７】（表６のつづき） [Table 7] (Continued from Table 6)
【００２０】[0020]
【表８】（表７のつづき） [Table 8] (Continued from Table 7)
【００２１】注１：めっき浴組成及び酸化物生成浴の浴
温は、共に４０℃で実施。
注２：クロムのモル／ｌは、無水クロム酸のモル／ｌで
ある。
注３：耐レトルト性試験（Ｔピール剥離試験）は、クロ
ムめっき鋼板の表面にエポキシフェノール系塗料を５０
ｍｇ／ｍ2 塗布後、１８０℃で１０分間焼付けた後、反
対面に同じ塗料を同量塗布し、２１０℃で１０分間焼付
けた。この試料を巾５ｍｍ、長さ１２０ｍｍに切断し、
先行塗装面と反対面を重ね、その間に厚さ１００μｍの
ナイロン系接着剤をはさみ、ホットプレスを用いて２０
０℃で４５秒の予熱を施した後、３Ｋｇ／ｃｍ2 の加圧
下で２００℃で３０秒の圧着を行い試験片を作製した。
この試験片を９０℃に保持した０．６％ＮａＣｌ水溶液
中に７日間浸漬した後、引張試験機を用いて２００ｍｍ
／ｍｉｎの一定引張速度でＴ型剥離試験を行い剥離強度
を測定した。試験は、試験片を９個ずつ施し、その平均
値を試験結果として示した。
注４：表面明度の評価は、株式会社島津製作所製の分光
測色計ＵＶ−２１００を用い、Ｃ光源・視野角１０°の
条件で拡散反射光と鏡面反射光の測色を行い、Ｌａｂ表
色系のＬ値を明度の指標とし、拡散反射と鏡面反射のＬ
値の合計によって表面明度を評価した。Note 1: The plating bath composition and the bath temperature of the oxide forming bath were both 40 ° C. Note 2: The mol / l of chromium is the mol / l of chromic anhydride. Note 3: In the retort resistance test (T-peel peel test), 50% epoxy phenolic paint was applied on the surface of the chrome-plated steel sheet.
After applying mg / m 2, after baking at 180 ° C. for 10 minutes, the same amount of the same paint was applied on the opposite surface and baking at 210 ° C. for 10 minutes. This sample is cut into a width of 5 mm and a length of 120 mm,
Overlap the opposite side with the previous coated side, sandwich a 100 μm thick nylon adhesive between them and use a hot press to apply 20
After preheating at 0 ° C for 45 seconds, pressure was applied at 3 Kg / cm 2 and pressure was applied at 200 ° C for 30 seconds to prepare a test piece.
This test piece was immersed in a 0.6% NaCl aqueous solution kept at 90 ° C. for 7 days, and then 200 mm using a tensile tester.
The T-type peel test was performed at a constant pulling rate of / min to measure the peel strength. In the test, nine test pieces were applied, and the average value was shown as the test result. Note 4: For the evaluation of the surface brightness, the spectrophotometer UV-2100 manufactured by Shimadzu Corporation was used to measure the diffuse reflected light and the specular reflected light under the condition of C light source and a viewing angle of 10 °, and the Lab table was used. Using the L value of the color system as an index of lightness, the L of diffuse reflection and specular reflection
Surface brightness was evaluated by the sum of the values.
【００２２】[0022]
【発明の効果】本発明の電解処理浴によれば、安定して
表面明度、耐レトルト性に優れたクロムめっき鋼板が製
造でき、缶用鋼板としての諸性能を向上することができ
る等の優れた効果が得られる。According to the electrolytic treatment bath of the present invention, it is possible to stably produce a chrome-plated steel sheet having excellent surface brightness and resistance to retort, and to improve various properties as a steel sheet for cans. The effect is obtained.
───────────────────────────────────────────────────── フロントページの続き (56)参考文献 特開 平９−287090（ＪＰ，Ａ) 特開 昭47−42347（ＪＰ，Ａ) 特開 昭57−140897（ＪＰ，Ａ) (58)調査した分野(Int.Cl.7，ＤＢ名) C25D 3/04 ─────────────────────────────────────────────────── ─── Continuation of the front page (56) Reference JP-A-9-287090 (JP, A) JP-A-47-42347 (JP, A) JP-A-57-140897 (JP, A) (58) Field (Int.Cl. 7 , DB name) C25D 3/04
Claims (5)
ｌ、硫化物／Ｃｒモル比１／２０００〜１／５００から
なる電解クロムめっき浴中のフッ素イオン濃度０．０３
〜０．３モル／ｌ、フッ素イオン／Ｆｅ3+イオンモル比
４．０以上にしたことを特徴とする無水クロム酸を主成
分とする電解処理浴。1. A chromic anhydride concentration of 0.3 to 2.5 mol /
l, fluorine ion concentration in electrolytic chrome plating bath consisting of sulfide / Cr molar ratio 1/2000 to 1/500 0.03
˜0.3 mol / l, fluorine ion / Fe 3+ ion molar ratio 4.0 or more, an electrolytic treatment bath containing chromic anhydride as a main component.
ｌ、硫化物／Ｃｒモル比１／２０００〜１／５００から
なる電解クロム酸処理浴中のフッ素イオン濃度０．３０
モル／ｌ以下、フッ素イオン／Ｆｅ3+イオンモル比４．
０以上にしたことを特徴とする無水クロム酸を主成分と
する電解処理浴。2. A chromic anhydride concentration of 0.3 to 2.5 mol /
1, sulfide / Cr molar ratio of 1/2000 to 1/500 in the electrolytic chromic acid treatment bath, fluorine ion concentration 0.30
Mol / l or less, fluorine ion / Fe 3+ ion molar ratio 4.
An electrolytic treatment bath containing chromic anhydride as a main component, which is set to 0 or more.
／ｌ＋弗化物濃度モル／ｌ−（１．７〜２．３）×Ｆｅ
3+濃度モル／ｌ〕＝７．５〜１８．０の数式を満足する
ことを特徴とする請求項１に記載の無水クロム酸を主成
分とする電解処理浴。3. CrO 3 concentration mol / l ÷ [sulfuric acid concentration mol / l + fluoride concentration mol / l- (1.7 to 2.3) × Fe
3 + concentration mol / l] = 7.5-18.0. The electrolytic treatment bath containing chromic anhydride as a main component according to claim 1, characterized in that:
ＨＦの一種または二種以上を添加したことを特徴とする
請求項１または請求項２または請求項３に記載の無水ク
ロム酸を主成分とする電解処理浴。4. NaF, KF, NH 4 F as a fluoride,
The electrolytic treatment bath containing chromic anhydride as a main component according to claim 1, 2 or 3, wherein one or more kinds of HF are added.
モル／ｌ以下を含有する請求項１または請求項２または
請求項３または請求項４に記載の無水クロム酸を主成分
とする電解処理浴。5. A sulfate ion concentration of 1.30 × 10 −3
The electrolytic treatment bath containing chromic anhydride as a main component according to claim 1, 2 or 3 or 4, containing less than 1 mol / l.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP00128898A JP3426489B2 (en) | 1998-01-07 | 1998-01-07 | Electrolytic treatment bath mainly composed of chromic anhydride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP00128898A JP3426489B2 (en) | 1998-01-07 | 1998-01-07 | Electrolytic treatment bath mainly composed of chromic anhydride |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH11200086A JPH11200086A (en) | 1999-07-27 |
| JP3426489B2 true JP3426489B2 (en) | 2003-07-14 |
Family
ID=11497278
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP00128898A Expired - Fee Related JP3426489B2 (en) | 1998-01-07 | 1998-01-07 | Electrolytic treatment bath mainly composed of chromic anhydride |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3426489B2 (en) |
-
1998
- 1998-01-07 JP JP00128898A patent/JP3426489B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH11200086A (en) | 1999-07-27 |
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