JP2007239004A - Plated steel sheet for can - Google Patents

Plated steel sheet for can Download PDF

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JP2007239004A
JP2007239004A JP2006061509A JP2006061509A JP2007239004A JP 2007239004 A JP2007239004 A JP 2007239004A JP 2006061509 A JP2006061509 A JP 2006061509A JP 2006061509 A JP2006061509 A JP 2006061509A JP 2007239004 A JP2007239004 A JP 2007239004A
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layer
steel sheet
tin
chemical conversion
plated steel
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JP4864493B2 (en
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Hiromitsu Date
博充 伊達
Masato Nakazawa
眞人 仲澤
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Nippon Steel Corp
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Nippon Steel Corp
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    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C2222/00Aspects relating to chemical surface treatment of metallic material by reaction of the surface with a reactive medium
    • C23C2222/20Use of solutions containing silanes

Abstract

<P>PROBLEM TO BE SOLVED: To provide a surface treated steel sheet having excellent organic film adhesion and corrosion resistance, and used for beverage cans, food cans or the like. <P>SOLUTION: The plated steel sheet for a can is at least provided with a metal tin layer, a tin oxide layer having a quantity of electricity satisfying 0.3 to 2.5 mC/cm<SP>2</SP>required for reduction, and a chemical conversion treatment layer comprising the phosphate or polymetaphosphate of one or more kinds selected from Sn, Fe, Al, Mg, Ca, Ti, Ni, Co and Zn by 0.1 to 5 mg/m<SP>2</SP>in terms of a P content in order from the steel sheet side. The surface of the chemical conversion treatment layer is preferably provided with a film comprising a silanol group-containing organic compound of 0.05 to 5 mg/m<SP>2</SP>in terms of an Si content. <P>COPYRIGHT: (C)2007,JPO&INPIT

Description

本発明は、飲料缶、食缶等に使用される、有機皮膜密着性、耐食性に優れた缶用めっき鋼板に関する。   The present invention relates to a plated steel sheet for cans, which is used for beverage cans, food cans and the like, and has excellent organic film adhesion and corrosion resistance.

従来、缶用材料として使用されてきた表面処理鋼板は、ブリキやLTS、TNS等の錫めっき鋼板、ニッケルめっき鋼板(TFS-NT)、電解クロムめっき鋼板(TFS-CT)が主なものである。通常、これらのめっき表面には化成処理が施され、それによって塗料や樹脂フィルムとの密着性を確保している。商品化されている缶用表面処理鋼板の化成処理の殆どは、重クロム酸塩又はクロム酸を主成分とする水溶液を用いた浸漬処理又は陰極電解処理である。例外として、特許文献1及び2に開示されているブリキのリン酸塩水溶液中での陰陽極電解処理が知られているが、用途は内面無塗装で使用する粉乳用に限定されている。リン酸電解処理が他の飲料缶、食缶に使用されないのは、塗料や樹脂フィルムのような有機皮膜の密着性が不十分であるためである。重クロム酸塩又はクロム酸を主成分とする水溶液を用いた浸漬処理又は陰極電解処理によって得られたクロム酸化膜は、有機皮膜の密着性を向上させる効果が大きく、これに代わる化成処理は、前記リン酸塩電解処理の他にも種々検討されているものの、実用化には至っていないのが現状である。   Conventionally, surface-treated steel sheets that have been used as can materials are tin-plated steel sheets such as tinplate, LTS, and TNS, nickel-plated steel sheets (TFS-NT), and electrolytic chrome-plated steel sheets (TFS-CT). . Usually, these plating surfaces are subjected to chemical conversion treatment, thereby ensuring adhesion with paints and resin films. Most of the chemical conversion treatment of commercially available surface-treated steel sheets for cans is immersion treatment or cathodic electrolysis treatment using an aqueous solution mainly composed of dichromate or chromic acid. As an exception, negative anodizing treatment in tin phosphate aqueous solution disclosed in Patent Documents 1 and 2 is known, but its application is limited to milk powder used without coating on the inner surface. The reason why the phosphoric acid electrolytic treatment is not used in other beverage cans and food cans is because the adhesion of organic coatings such as paints and resin films is insufficient. The chromium oxide film obtained by immersion treatment or cathodic electrolysis treatment using an aqueous solution containing dichromate or chromic acid as a main component has a large effect of improving the adhesion of the organic film. Although various studies have been made in addition to the above-described phosphate electrolysis, the present situation is that it has not yet been put into practical use.

例えば、特許文献3には、浸漬処理によりリン酸系皮膜を形成させたDI缶用電気めっきブリキが開示されている。また、特許文献4には、フィチン酸又はフィチン酸塩溶液中での陽極処理する方法が開示されている。   For example, Patent Document 3 discloses an electroplating tin for DI can in which a phosphoric acid-based film is formed by dipping treatment. Patent Document 4 discloses a method for anodizing in a phytic acid or phytate solution.

近年は、錫めっき層上にシランカップリング剤を使用した皮膜を施す技術が多く開示されている。例えば、特許文献5には、錫めっき鋼板のSn層又はFe-Sn合金層上にシランカップリング剤塗布層を設けた鋼板及び缶が開示されており、特許文献6には、錫めっき層上に下層としてP、Snを含有する化成皮膜、上層としてシランカップリング層を有する錫めっき鋼板が開示されている。また、特許文献6に類似した技術として、特許文献7乃至16が開示されている。   In recent years, many techniques for applying a film using a silane coupling agent on a tin plating layer have been disclosed. For example, Patent Document 5 discloses a steel plate and a can in which a silane coupling agent coating layer is provided on a Sn layer or Fe-Sn alloy layer of a tin-plated steel sheet, and Patent Document 6 discloses a tin plate on the tin-plated layer. Discloses a tin-plated steel sheet having a chemical conversion film containing P and Sn as a lower layer and a silane coupling layer as an upper layer. Further, Patent Documents 7 to 16 are disclosed as techniques similar to Patent Document 6.

特開昭52-68832号公報JP 52-68832 A 特開昭52-75626号公報JP 52-75626 A 特開昭59-47396号公報JP 59-47396 A 特開昭52-92837号公報JP 52-92837 A 特開2002-285354号公報JP 2002-285354 A 特開2001-316851号公報JP 2001-316851 特開2002-275643号公報JP 2002-275643 A 特開2002-206191号公報JP 2002-206191 A 特開2002-275657号公報JP 2002-275657 A 特開2002-339081号公報Japanese Patent Laid-Open No. 2002-339081 特開2003-3281号公報JP2003-3281 特開2003-175564号公報JP2003-175564A 特開2003-183853号公報Japanese Patent Laid-Open No. 2003-183853 特開2003-239084号公報JP2003-239084 特開2003-253466号公報JP 2003-253466 A 特開2004-68063号公報JP 2004-68063 A

しかしながら、前記特許文献に記載された化成皮膜はいずれも、缶用めっき鋼板として用いるに十分な有機皮膜密着性、耐食性等の性能を備えているとは言い難い。   However, it is difficult to say that any of the chemical conversion films described in the above-mentioned patent documents has sufficient organic film adhesion, corrosion resistance, and the like for use as a plated steel sheet for cans.

そこで、本発明は、上記従来技術の問題点を解決し、有機皮膜密着性、耐食性に優れた缶用めっき鋼板を提供することを目的とする。   Then, this invention solves the problem of the said prior art, and aims at providing the plated steel plate for cans excellent in organic membrane adhesiveness and corrosion resistance.

本発明者らは、上記の課題に対して鋭意検討し、有機皮膜密着性を阻害する酸化錫の量を少なくし、かつ、その生成を抑制することのできる皮膜を形成することで、有機皮膜密着性、耐食性等の諸特性が飛躍的に向上することを見出し、本発明に至ったものである。   The inventors of the present invention diligently studied the above problems, and reduced the amount of tin oxide that inhibits organic film adhesion and formed a film capable of suppressing the formation of the organic film. The present inventors have found that various properties such as adhesion and corrosion resistance are drastically improved and have reached the present invention.

即ち、本発明の主旨とするところは、
(1) 鋼板側から順に金属錫層、還元に要する電気量として0.3〜2.5mC/cm2の酸化錫層、Sn、Fe、Al、Mg、Ca、Ti、Ni、Co、Znの1種又は2種以上のリン酸塩又はポリメタリン酸塩をP量として0.1〜5mg/m2有する化成処理層を少なくとも有することを特徴とする缶用めっき鋼板、
(2) 前記化成処理層上に、Si量として0.05〜5mg/m2のシラノール基含有有機化合物を含む皮膜を有する前記(1)記載の缶用めっき鋼板、
(3) 前記金属錫層の下地層として、Ni量として2〜100mg/m2のFe-Ni合金層又はFe-Ni-Sn合金層を有する前記(1)又は(2)に記載の缶用めっき鋼板、
である。
That is, the main point of the present invention is that
(1) In order from the steel plate side, the metal tin layer, the amount of electricity required for reduction is 0.3 to 2.5 mC / cm 2 tin oxide layer, Sn, Fe, Al, Mg, Ca, Ti, Ni, Co, Zn or one type A plated steel sheet for cans having at least a chemical conversion treatment layer having 0.1 to 5 mg / m 2 of P or more of two or more phosphates or polymetaphosphates;
(2) The plated steel sheet for cans according to (1), which has a film containing 0.05 to 5 mg / m 2 of a silanol group-containing organic compound as the amount of Si on the chemical conversion treatment layer,
(3) For cans according to (1) or (2), wherein the metal tin layer has an Fe-Ni alloy layer or Fe-Ni-Sn alloy layer having a Ni content of 2 to 100 mg / m 2 as an underlayer of the metal tin layer. Plated steel sheet,
It is.

本発明により、極めて良好な有機皮膜密着性、耐食性を具備した缶用めっき鋼板を提供することができる。   According to the present invention, it is possible to provide a plated steel sheet for cans having extremely good organic film adhesion and corrosion resistance.

以下に、本発明を詳細に説明する。   The present invention is described in detail below.

本発明で使用する鋼板には、特に制限を設ける必要はない。従来から缶用鋼板に使用されているアルミキルド鋼や低炭素鋼等の成分系の鋼板が問題なく使用できる。また、鋼板の厚みや調質度は、ユーザーが使用目的によって決定するものであるので、その指定に従えばよい。   There is no particular limitation on the steel sheet used in the present invention. Component steel plates such as aluminum killed steel and low carbon steel that have been used for steel plates for cans can be used without problems. Moreover, since the thickness and tempering degree of a steel plate are determined by the user according to the purpose of use, the designation may be followed.

本発明の主たる構成は、金属錫層と化成処理層とを有するめっき鋼板であって、該金属錫層と該化成処理層の中間層として、還元に要する電気量として0.3〜2.5mC/cm2の酸化錫層を有するめっき鋼板である。 The main structure of the present invention is a plated steel sheet having a metal tin layer and a chemical conversion treatment layer, and as an intermediate layer between the metal tin layer and the chemical conversion treatment layer, the amount of electricity required for reduction is 0.3 to 2.5 mC / cm 2. This is a plated steel sheet having a tin oxide layer.

金属錫の付着量は限定しないが、缶用材料とする場合は0.2〜22.4g/m2が適当である。0.2g/m2未満では、溶接缶とする場合、溶接時に溶融金属の飛散が生じるため、十分な溶接性が得られないし、絞り-扱き缶とする場合、金属錫の固体潤滑剤としての作用が不十分である。また、22.4g/m2を超えても品質特性は向上しないので、経済的な理由や希少資源を浪費しないためにも、22.4g/m2を超える付着量の錫は使用しないほうがよい。 The amount of metallic tin deposited is not limited, but 0.2 to 22.4 g / m 2 is appropriate for a can material. If it is less than 0.2 g / m 2 , when welding cans are used, molten metal scatters during welding, so that sufficient weldability cannot be obtained, and when used as a draw-and-handle can, metallic tin acts as a solid lubricant. Is insufficient. Moreover, since quality characteristics do not improve even if it exceeds 22.4 g / m 2 , it is better not to use tin with an adhesion amount exceeding 22.4 g / m 2 in order not to waste economic reasons and scarce resources.

化成処理層は、Sn、Fe、Al、Mg、Ca、Ti、Ni、Co、Znの1種又は2種以上のリン酸塩またはポリメタリン酸塩をP量として0.1〜5mg/m2有する層からなることが必要である。P量として0.1mg/m2未満では、リン酸塩又はポリメタリン酸塩がめっき表面に点在する分布となり、金属錫層及び酸化錫層を十分に被覆することができず、有機皮膜密着性を阻害する酸化錫層の成長を抑えることができない。一方、P量が5mg/m2を超えると、リン酸塩又はポリメタリン酸塩皮膜は凝集破壊し易く、有機皮膜密着性はむしろ低下する。 The chemical conversion treatment layer is composed of Sn, Fe, Al, Mg, Ca, Ti, Ni, Co, Zn having a P content of 0.1 to 5 mg / m 2 as one or more phosphates or polymetaphosphates. It is necessary to become. When the amount of P is less than 0.1 mg / m 2 , the distribution of phosphate or polymetaphosphate is scattered on the plating surface, the metal tin layer and the tin oxide layer cannot be sufficiently covered, and the organic film adhesion is poor. The growth of the inhibited tin oxide layer cannot be suppressed. On the other hand, when the amount of P exceeds 5 mg / m 2 , the phosphate or polymetaphosphate film tends to cohesively break, and the organic film adhesion is rather lowered.

上記化学種及び量のリン酸塩又はポリメタリン酸塩皮膜が金属錫層及び酸化錫層を被覆すると、有機皮膜密着性を阻害する酸化錫層の成長が著しく抑制される。   When the phosphate or polymetaphosphate coating of the chemical species and amount covers the metal tin layer and the tin oxide layer, the growth of the tin oxide layer that inhibits the adhesion of the organic coating is remarkably suppressed.

金属錫層と化成処理層の中間層として、還元に要する電気量として0.3〜2.5mC/cm2の酸化錫層を有することが必要である。酸化錫層の還元に要する電気量は、化成処理層、又は、その上層にシラノール基含有有機化合物皮膜を有する錫めっき鋼板を、窒素ガスのバブリング等の手段によって溶存酸素を除去した0.001mol/Lの臭化水素酸水溶液中で0.05mA/cm2の定電流で陰極電解し、得られる電位-時間曲線から求めることができる。酸化錫層は化成処理層との密着力向上に寄与するため、0.3mC/cm2より少ないと化成処理層が剥離し易くなり、十分な有機皮膜密着性が得られない。一方、酸化錫層は非常に脆いため、2.5mC/cm2を超えると凝集破壊し易くなるので、有機皮膜密着性はむしろ低下する。 As an intermediate layer between the metal tin layer and the chemical conversion treatment layer, it is necessary to have a tin oxide layer of 0.3 to 2.5 mC / cm 2 as the amount of electricity required for reduction. The amount of electricity required for the reduction of the tin oxide layer is 0.001 mol / L obtained by removing dissolved oxygen from a chemical conversion treatment layer or a tin-plated steel sheet having a silanol group-containing organic compound film on the upper layer by means such as bubbling of nitrogen gas. Cathodic electrolysis in a hydrobromic acid aqueous solution at a constant current of 0.05 mA / cm 2 and obtained from a potential-time curve. Since the tin oxide layer contributes to improving the adhesion with the chemical conversion treatment layer, if it is less than 0.3 mC / cm 2 , the chemical conversion treatment layer tends to peel off and sufficient organic film adhesion cannot be obtained. On the other hand, since the tin oxide layer is very brittle, if it exceeds 2.5 mC / cm 2 , it tends to cohesive failure, so the organic film adhesion is rather lowered.

化成処理層上には、Si量として0.05〜5mg/ m2のシラノール基含有有機化合物を含む皮膜を有することが好ましい。シラノール基含有有機化合物の皮膜は、空気が金属錫表面に達する障壁となって酸化錫層の成長を抑制すると共に、親水基が化成処理層のリン酸塩又はポリメタリン酸塩の-OH基と脱水結合し、疎水性の部分が有機皮膜と結合することで、有機皮膜の密着性を向上させる作用をする。シラノール基含有有機化合物が0.05mg/m2未満では、化成処理層を十分に被覆することができず、空気のバリア層としての作用が不十分となることがある。一方、5mg/m2を超える量のシラノール基含有有機化合物は、自己縮合によって弱い皮膜となってしまうため、有機皮膜密着性はむしろ低下することがある。 It is preferable to have a film containing a silanol group-containing organic compound in an amount of 0.05 to 5 mg / m 2 on the chemical conversion treatment layer. The film of silanol group-containing organic compound acts as a barrier for air to reach the surface of the metal tin and suppresses the growth of the tin oxide layer, and the hydrophilic group dehydrates with the -OH group of the chemical conversion treatment layer phosphate or polymetaphosphate. By bonding, the hydrophobic part binds to the organic film, thereby improving the adhesion of the organic film. If the silanol group-containing organic compound is less than 0.05 mg / m 2 , the chemical conversion treatment layer may not be sufficiently covered, and the action as an air barrier layer may be insufficient. On the other hand, since the silanol group-containing organic compound in an amount exceeding 5 mg / m 2 becomes a weak film by self-condensation, the adhesion of the organic film may rather decrease.

シラノール基含有有機化合物は、シランカップリング剤を加水分解させることでシラノール基を生じさせて得ることができる。シラノール基含有有機化合物を得るために用いるシランカップリング剤は、その分子中にアミノ基を有するものであることが好ましい。例として、3-(2-アミノエチル)アミノプロピルトリメトキシシラン、3-(2-アミノエチル)アミノプロピルメチルジメトキシシラン、3-アミノプロピルトリエトキシシラン等を挙げることができる。アミノ基を有するシランカップリング剤の加水分解によって生じたシラノール基含有有機化合物は、他のシランカップリング剤と比べて、ポリエチレンテレフタレート、ポリブチレンテレフタレート等のポリエステル系樹脂やエポキシ塗料等に対し、顕著な密着性向上効果が認められる。   The silanol group-containing organic compound can be obtained by hydrolyzing a silane coupling agent to generate a silanol group. The silane coupling agent used to obtain the silanol group-containing organic compound preferably has an amino group in the molecule. Examples include 3- (2-aminoethyl) aminopropyltrimethoxysilane, 3- (2-aminoethyl) aminopropylmethyldimethoxysilane, 3-aminopropyltriethoxysilane, and the like. Silanol group-containing organic compounds produced by hydrolysis of amino group-containing silane coupling agents are more prominent than polyester resins such as polyethylene terephthalate and polybutylene terephthalate, and epoxy paints, compared to other silane coupling agents. Adhesive improvement effect is recognized.

金属錫層の下地層として、Ni量として2〜100mg/m2のFe-Ni合金層又はFe-Ni-Sn合金層があってもよい。該合金層は、上層の錫をリフロー処理する場合、地鉄と錫とが接触するのを妨げるバリア層となり、Fe-Sn合金化を抑制すると言うメリットがある。Fe-Ni合金層がNi量として2mg/m2未満では、上記Fe-Sn合金化反応のバリアとしての効果が認められない。一方、100mg/m2を超えてもFe-Sn合金化のバリアとしての性能は向上せず、むしろNi-Sn合金化が促進される傾向があるため、好ましくない。 As the underlayer of the metal tin layer, there may be an Fe—Ni alloy layer or an Fe—Ni—Sn alloy layer having a Ni content of 2 to 100 mg / m 2 . When the upper layer tin is subjected to reflow treatment, the alloy layer becomes a barrier layer that prevents the contact between the base iron and the tin, and has an advantage of suppressing Fe-Sn alloying. When the Fe—Ni alloy layer is less than 2 mg / m 2 as the amount of Ni, the effect as a barrier of the Fe—Sn alloying reaction is not recognized. On the other hand, even if it exceeds 100 mg / m 2 , the performance as a barrier for Fe—Sn alloying is not improved, but rather Ni—Sn alloying tends to be promoted, which is not preferable.

次に、本発明のめっき鋼板を製造するための方法を以下に示す。ただし、この方法によって本発明(1)〜(3)を限定するものではない。   Next, the method for manufacturing the plated steel plate of this invention is shown below. However, the present invention (1) to (3) is not limited by this method.

鋼板のめっき前処理の方法及び用いる錫めっき浴については、本発明では特に規定しないが、前処理として電解アルカリ脱脂及び希硫酸酸洗を施した後、フェノールスルホン酸浴等の酸性錫めっき浴で電気錫めっきを施すと、良好な錫めっきが得られる。なお、錫めっきの前にFe-Ni合金めっきを施しても、また、ニッケルめっきを施した後、加熱してニッケルを鋼板表面層に拡散させてFe-Ni合金層を形成させてもよい。錫めっき後の鋼板は、水又は錫めっき液の希釈液の入ったドラクアウト槽に浸漬、乾燥され、リフロー処理が施される。リフロー処理は非酸化性雰囲気又は還元性雰囲気中で行い、直後にクエンチ処理することで、表面の錫の酸化が抑制される。非酸化性雰囲気ガスとしては、窒素、炭酸ガス、アルゴン等が、また、還元雰囲気としては水素ガスを5vol%混合した窒素ガス等が挙げられるが、経済的な理由から、窒素雰囲気が最も好適である。   The method for pretreatment of the steel plate and the tin plating bath to be used are not particularly defined in the present invention, but after pretreatment with electrolytic alkaline degreasing and dilute sulfuric acid pickling, an acidic tin plating bath such as a phenolsulfonic acid bath is used. When electrotin plating is performed, good tin plating can be obtained. Note that Fe—Ni alloy plating may be performed before tin plating, or after nickel plating, heating may be performed to diffuse nickel into the steel sheet surface layer to form an Fe—Ni alloy layer. The steel plate after tin plating is immersed and dried in a drag-out tank containing water or a diluted solution of a tin plating solution, and subjected to a reflow treatment. The reflow treatment is performed in a non-oxidizing atmosphere or a reducing atmosphere, and the quenching treatment is performed immediately thereafter, so that oxidation of tin on the surface is suppressed. Examples of the non-oxidizing atmosphere gas include nitrogen, carbon dioxide gas, and argon. Examples of the reducing atmosphere include nitrogen gas mixed with 5 vol% of hydrogen gas. For economic reasons, a nitrogen atmosphere is most preferable. is there.

リフロー処理は、錫の融点である232℃以上で行うが、300℃を超えるとFe-Sn合金化が促進されてしまうので好ましくない。錫めっき鋼板の加熱の手段としては、電気抵抗加熱や誘導加熱、又はそれらを組み合わせて用いるとよい。クエンチ処理は、錫を溶融した錫めっき鋼板を、水の中に漬ければよい。ストリップを連続的にリフロー処理及びクエンチ処理すると、クエンチ槽の水は80℃位まで上昇するが、差し支えない。クエンチ処理後、1.5秒以上、6秒以内に化成処理を施すことで、好ましい量の酸化錫層が得られる。   The reflow treatment is performed at 232 ° C. or higher, which is the melting point of tin, but if it exceeds 300 ° C., Fe—Sn alloying is promoted, which is not preferable. As a means for heating the tin-plated steel sheet, electric resistance heating, induction heating, or a combination thereof may be used. The quench process may be performed by immersing a tin-plated steel sheet in which tin is melted in water. When the strip is continuously reflowed and quenched, the water in the quench bath rises to about 80 ° C., but it does not matter. A preferable amount of the tin oxide layer can be obtained by performing the chemical conversion treatment within 1.5 seconds or more and 6 seconds after the quench treatment.

リフロー時に酸化錫層が形成されない非酸化性雰囲気又は還元雰囲気でのリフロー処理を施した場合、クエンチ処理から化成処理までの時間が1.5秒未満では酸化錫層が0.3mC/cm2未満となり易く、6秒を超えると酸化錫層が2.5mC/cm2を超えてしまう。化成処理に用いる処理液は、リン酸水溶液又はポリリン酸水溶液、又は、Sn、Fe、Al、Mg、Ca、Ti、Ni、Co、Znの1種又は2種以上のカチオン(0.2〜5g/L)又はこれに配位子が配位した錯体とリン酸イオン又はポリリン酸イオンとを含む水溶液が好ましい。 When a reflow treatment is performed in a non-oxidizing atmosphere or a reducing atmosphere where a tin oxide layer is not formed during reflow, the tin oxide layer is likely to be less than 0.3 mC / cm 2 if the time from quench treatment to chemical conversion treatment is less than 1.5 seconds, If it exceeds 6 seconds, the tin oxide layer exceeds 2.5 mC / cm 2 . The treatment liquid used for the chemical conversion treatment is phosphoric acid aqueous solution or polyphosphoric acid aqueous solution, or one or more cations (0.2 to 5 g / L) of Sn, Fe, Al, Mg, Ca, Ti, Ni, Co, Zn. ) Or an aqueous solution containing a complex coordinated with a ligand and a phosphate ion or a polyphosphate ion.

リン酸イオン又はポリリン酸イオンの濃度は、リン酸イオン換算で5〜80g/L、液温は25〜60℃の範囲が適当である。該処理液に鋼板を0.5〜3秒間浸漬するか、該処理液中で1〜10A/dm2の陰極電流密度で2〜20C/dm2の電気量の電解処理をするか、又は該処理液を塗布し、水洗して、又は水洗しないで乾燥するとよい。 The concentration of phosphate ions or polyphosphate ions is suitably 5 to 80 g / L in terms of phosphate ions, and the liquid temperature is suitably in the range of 25 to 60 ° C. The steel plate is immersed in the treatment liquid for 0.5 to 3 seconds, or is subjected to an electrolytic treatment of an electric quantity of 2 to 20 C / dm 2 at a cathode current density of 1 to 10 A / dm 2 in the treatment liquid, or the treatment liquid It is good to apply | coat, wash with water, or to dry without washing.

化成処理後、鋼板をさらにシランカップリング剤水溶液に浸漬するかこれを塗布し、ロールで余剰の処理液を絞って、又は絞らずに、直ちに乾燥することが好ましい。処理液が均一に分布せずにハジキが生じる場合は、少量のエタノールを処理液に添加するとよい。   After the chemical conversion treatment, it is preferable that the steel plate is further immersed in an aqueous solution of a silane coupling agent or coated, and dried immediately with or without squeezing excess treatment liquid with a roll. In the case where repellency occurs without the processing solution being evenly distributed, a small amount of ethanol may be added to the processing solution.

鋼板が自然乾燥する前に100℃以上200℃以下の温度で乾燥すると、鋼板への密着性が良好で、空気が錫表面に達するのを妨げるバリアとしても良好なシラノール含有有機化合物の皮膜が形成されるので好ましい。さらに、めっき鋼板表面の過剰なシラノール基含有有機化合物を水洗し、乾燥させてもよい。好適なシランカップリング剤として、例えば、3-(2-アミノエチル)アミノプロピルトリメトキシシランが挙げられる。この水溶液(0.01〜1g/L)に鋼板を浸漬した後、鋼板上の処理液の量が、1m2当たり5〜20mLとなるよう、ゴムロールの絞り圧を調整して処理液を絞ると、適当な厚みシラノール基含有有機化合物皮膜となる。 When the steel plate is dried at a temperature of 100 ° C or higher and 200 ° C or lower before it is naturally dried, a film of organic compound containing silanol is formed that has good adhesion to the steel plate and also serves as a barrier that prevents air from reaching the tin surface. This is preferable. Furthermore, the excess silanol group-containing organic compound on the surface of the plated steel sheet may be washed with water and dried. Suitable silane coupling agents include, for example, 3- (2-aminoethyl) aminopropyltrimethoxysilane. After immersing the steel sheet in the aqueous solution (0.01 to 1 g / L), the amount of treatment liquid on the steel sheet, so as to be 1 m 2 per 5-20 ml, when adjusting the throttle pressure of the rubber roller to squeeze the processing liquid, suitable A thick silanol group-containing organic compound film is obtained.

上記の製造方法の他、以下の方法によっても本発明のめっき鋼板を得ることができる。鋼板のめっき前処理、錫めっき、リフローの方法は、上記と同様でよい。化成処理前に、リン酸水溶液、リン酸水素ナトリウム水溶液、炭酸ナトリウム水溶液等、酸性又はアルカリ性の電解質を2mass%以上含む水溶液中で陰極電解し、錫表面の酸化層を還元する。陰極電流密度2A/dm2以上10A/dm2以下、電解電気量3C/dm2以上10C/dm2以下で好ましい量の酸化錫層が得られる。化成処理以降は、上記の方法と同様でよい。 In addition to the above manufacturing method, the plated steel sheet of the present invention can also be obtained by the following method. The plating pretreatment, tin plating, and reflow methods for the steel sheet may be the same as described above. Before the chemical conversion treatment, cathodic electrolysis is performed in an aqueous solution containing 2 mass% or more of an acidic or alkaline electrolyte such as an aqueous solution of phosphoric acid, an aqueous solution of sodium hydrogenphosphate, an aqueous solution of sodium carbonate, and the oxide layer on the tin surface is reduced. A preferable amount of tin oxide layer can be obtained when the cathode current density is 2 A / dm 2 or more and 10 A / dm 2 or less and the amount of electrolysis is 3 C / dm 2 or more and 10 C / dm 2 or less. After the chemical conversion treatment, the same method as described above may be used.

以下、実施例によって、本発明をさらに詳細に説明する。   Hereinafter, the present invention will be described in more detail by way of examples.

低炭素冷延鋼帯を連続焼鈍、次いで調質圧延して得た板厚0.18mm、調質度T-5CAの鋼帯を使用した。めっき前処理として、10mass%水酸化ナトリウム溶液中で電解脱脂した後、5mass%希硫酸で酸洗した。   A steel strip having a thickness of 0.18 mm and a tempering degree of T-5CA obtained by continuous annealing and then temper rolling of a low carbon cold rolled steel strip was used. As a pretreatment for plating, electrolytic degreasing was carried out in a 10 mass% sodium hydroxide solution, followed by pickling with 5 mass% dilute sulfuric acid.

次いで、フェロスタン浴を用いて電気錫めっきを施した。錫イオンを20g/L、フェノールスルホン酸イオンを75g/L、界面活性剤を5g/L含む43℃のめっき液中で、電流密度20A/dm2で陰極電解した。錫めっき量は、電解時間で調節し、1.3g/m2とした。錫めっき後は水洗し、ロールで水切りをした後、乾燥し、通電加熱によって10秒間で250℃まで昇温させて錫をリフローし、直ちに水でクエンチした。リフロー処理の際、雰囲気を窒素、水素を5vol%混合した窒素、空気の中から選んだ。 Subsequently, electrotin plating was performed using a ferrostan bath. Cathodic electrolysis was performed at a current density of 20 A / dm 2 in a plating solution at 43 ° C. containing 20 g / L of tin ions, 75 g / L of phenolsulfonic acid ions, and 5 g / L of surfactant. The tin plating amount was adjusted to 1.3 g / m 2 by adjusting the electrolysis time. After tin plating, it was washed with water, drained with a roll, dried, heated to 250 ° C. for 10 seconds by energization heating, reflowed tin, and immediately quenched with water. During the reflow treatment, the atmosphere was selected from nitrogen, nitrogen mixed with 5 vol% hydrogen, and air.

引き続き、該錫めっき鋼板に下記のように化成処理を施した。液温40℃のリン酸水溶液、又はこれにSn、Fe、Al、Mg、Ca、Ti、Ni、Co、Znの1種又は2種以上の塩化物を含む水溶液に鋼板を1.2秒間浸漬し、水洗して冷風乾燥した。比較のため、該化成処理を施さない条件も行った。   Subsequently, the tin-plated steel sheet was subjected to chemical conversion treatment as follows. Immerse the steel sheet in a phosphoric acid aqueous solution with a liquid temperature of 40 ° C. or an aqueous solution containing one or more chlorides of Sn, Fe, Al, Mg, Ca, Ti, Ni, Co, Zn for 1.2 seconds, Washed with water and dried in cold air. For comparison, conditions for not performing the chemical conversion treatment were also performed.

化成処理後、鋼板をさらに25℃の3-(2-アミノエチル)アミノプロピルトリメトキシシラン(シランカップリング剤)水溶液に浸漬した後、鋼板上の処理液の量が、1m2当たり5〜20mLとなるよう、ゴムロールの絞り圧を調整して処理液を絞った。鋼板が自然乾燥する前に140℃の雰囲気温度で乾燥した。 After chemical conversion treatment, the steel plate is further immersed in a 3- (2-aminoethyl) aminopropyltrimethoxysilane (silane coupling agent) aqueous solution at 25 ° C., and the amount of the treatment liquid on the steel plate is 5 to 20 mL per 1 m 2 . The treatment liquid was squeezed by adjusting the squeezing pressure of the rubber roll. Before the steel sheet naturally dried, it was dried at an ambient temperature of 140 ° C.

Sn、Fe、Al、Mg、Ca、Ti、Ni、Co、Zn、P、Siの付着量は、蛍光X線強度から、予め作成した検量線を使って算出した。   The adhesion amount of Sn, Fe, Al, Mg, Ca, Ti, Ni, Co, Zn, P, and Si was calculated from the fluorescent X-ray intensity using a calibration curve prepared in advance.

酸化錫量は、化成処理層、又は、その上層にシラノール基含有有機化合物皮膜を施した錫めっき鋼板を、窒素バブリングによって脱気した0.001mol/Lの臭化水素酸水溶液中で0.05mA/cm2の定電流陰極電解し、得られた電位-時間曲線から、還元に要する電気量として求めた。 The amount of tin oxide is 0.05 mA / cm in a 0.001 mol / L hydrobromic acid aqueous solution obtained by degassing a chemical conversion treatment layer or a tin-plated steel sheet coated with a silanol group-containing organic compound film thereon by nitrogen bubbling. The amount of electricity required for reduction was determined from the obtained constant-current cathodic electrolysis 2 and the obtained potential-time curve.

上記処理材について、以下に示す(A)〜(D)の各項目について評価試験を実施した。   About the said processing material, the evaluation test was implemented about each item of (A)-(D) shown below.

(A) フィルム密着性
評価材に、予めエポキシ接着剤を2μm塗布した厚さ15μmのPET(ポリエチレンテレフタレート)系フィルムを、230℃でラミネートした後、地鉄に達するクロスカットを入れ、速やかに240℃に加熱し、クロスカット中央部に5kg/cm2の空気ガスを垂直に吹きつけ、フィルムの剥離状況を評価した。全く剥離が認められなかったものを◎(非常に良好)、カット部から0.5mm以下の剥離が認められたものを○(良好)、カット部から0.5mmを超える剥離が認められたものを×(不良)とした。なお、○以上をフィルム密着性の合格レベルと判断した。
(A) Film adhesion A 15 μm thick PET (polyethylene terephthalate) film with 2 μm of epoxy adhesive applied in advance to the evaluation material was laminated at 230 ° C., and then a crosscut reaching the base iron was added. The film was heated to 0 ° C., and 5 kg / cm 2 of air gas was blown vertically to the center of the crosscut to evaluate the peeling state of the film. ◎ (excellent) where no separation was observed, ○ (excellent) where separation of 0.5 mm or less from the cut part was observed, and x where separation exceeding 0.5 mm was observed from the cut part (Defect). In addition, (circle) or more was judged as the pass level of film adhesiveness.

(B) 塗料密着性
評価材に、エポキシ・フェノール系塗料を60mg/dm2塗布し、210℃で10分間の焼き付けを行った。この塗装板から5mm×10cmの大きさの試料を切り出した。2枚の試料を、塗装面が向かい合わせになるようにし、間に厚さ100μmのフィルム状のナイロン接着剤を挟んだ。これを、つかみ代を残してホットプレスで200℃、120秒間予熱した後、2.9×105Paの圧力をかけ、200℃で30秒間の圧着し、引張試験片とした。つかみ部をそれぞれ90゜の角度で曲げてT字状とし、引張試験機のチャックでつかんで引っ張り、剥離強度を測定して、塗料密着性を評価した。
(B) Paint adhesion The evaluation material was coated with 60 mg / dm 2 of epoxy / phenolic paint and baked at 210 ° C. for 10 minutes. A sample having a size of 5 mm × 10 cm was cut out from the coated plate. Two samples were placed so that the painted surfaces face each other, and a film-like nylon adhesive having a thickness of 100 μm was sandwiched between them. This was preheated with a hot press at 200 ° C. for 120 seconds, leaving a grip, and then subjected to a pressure of 2.9 × 10 5 Pa and pressed at 200 ° C. for 30 seconds to obtain a tensile test piece. The gripping portions were bent at 90 ° angles to form a T shape, which were gripped and pulled with a chuck of a tensile tester, and the peel strength was measured to evaluate the paint adhesion.

試験片幅5mm当たりの測定強度が、68.6N以上を◎、49.0N以上68.6N未満を○、29.4N以上49.0N未満を△、29.4N未満を×とした。   The measured strength per 5 mm test piece width was rated as ◎ for 68.6N or more, ◯ for 49.0N or more and less than 68.6N, △ for 29.4N or more and less than 49.0N, and × for less than 29.4N.

(C) 耐食性
評価材の缶内面に相当する面の耐食性を評価するため、UCC(アンダーカッティング・コロージョン)試験を行った。缶内面側に相当する面に厚さ15μmのPET(ポリエチレンテレフタレート)系フィルムをラミネートし、地鉄に達するまでクロスカットを入れた後、1.5%クエン酸と1.5%塩化ナトリウムからなる55℃の試験液中に、大気開放下で96時間浸漬した。水洗・乾燥後、速やかにスクラッチ部及び平面部をテープで剥離して、スクラッチ部近傍の腐食状況、スクラッチ部のピッティング腐食及び平面部のフィルム剥離状況を観察して、耐食性を評価した。テープ剥離も腐食も認められないものを◎(非常に良好)、スクラッチ部から0.4mm未満のテープ剥離又は目視で認められない僅かな腐食の一方又は両方が認められたものを○(良好)、スクラッチ部から0.4mm以上、1mm以下のテープ剥離又は目視で認められる小さい腐食の一方又は両方が認められたものを△(やや不良)とした。
(C) Corrosion Resistance In order to evaluate the corrosion resistance of the surface corresponding to the inner surface of the evaluation material, a UCC (under cutting corrosion) test was conducted. Laminate a PET (polyethylene terephthalate) film with a thickness of 15μm on the surface corresponding to the inner surface of the can, make a crosscut until it reaches the ground iron, and then test at 55 ° C consisting of 1.5% citric acid and 1.5% sodium chloride It was immersed in the liquid for 96 hours under open air. After washing with water and drying, the scratched part and the flat part were quickly peeled off with a tape, and the corrosion state in the vicinity of the scratch part, the pitting corrosion of the scratch part and the film peeling state of the flat part were observed to evaluate the corrosion resistance. ◎ (very good) where no tape peeling or corrosion is observed, ○ (good), where one or both of tape peeling less than 0.4 mm from the scratch part or slight corrosion not visually recognized is observed, The case where one or both of tape peeling of 0.4 mm or more and 1 mm or less from the scratch portion or small corrosion visually observed was recognized as Δ (somewhat poor).

(D) 外観
評価材の外観を、光沢、色調、ムラの総合的なものとして目視で評価した。非常に良好な外観であるものを◎、商品として問題のない良好な外観であるものを○、商品としては外観にやや不良な点があるものを△、外観不良で商品にならないものを×とした。
(D) Appearance The appearance of the evaluation material was visually evaluated as an overall gloss, color tone, and unevenness. ◎ for a very good appearance, ◯ for a good appearance with no problem as a product, △ for a product with a slightly poor appearance, × for a product with a poor appearance that does not become a product did.

以上の性能評価結果から、総合評価を◎(非常に良好)、○(良好)、△(やや不良)、×(不良)の4段階に分類し、◎、○を合格レベルとした。   Based on the above performance evaluation results, the overall evaluation was classified into four stages: ◎ (very good), ○ (good), △ (slightly bad), and × (bad), and ◎ and ○ were regarded as acceptable levels.

上記に記載しなかった試験条件、及び、評価結果を表1に示した。   Table 1 shows the test conditions that were not described above and the evaluation results.

Figure 2007239004
Figure 2007239004

本発明の実施例1〜18は、全ての評価項目及び総合評価で◎又は○で、求められる性能を満足した。   Examples 1 to 18 of the present invention satisfied the required performance with ◎ or ○ in all evaluation items and overall evaluation.

比較例1は、化成処理層のない例である。酸化錫が成長し、フィルム密着性、塗料密着性、耐食性がいずれも劣っていた。   Comparative Example 1 is an example without a chemical conversion treatment layer. Tin oxide grew and film adhesion, paint adhesion, and corrosion resistance were all poor.

比較例2は、クエンチ処理から化成処理までの時間が長く、酸化錫量が多かった例である。フィルム密着性、塗料密着性、耐食性がいずれも不十分であった。   Comparative Example 2 is an example in which the time from the quench treatment to the chemical conversion treatment is long and the amount of tin oxide is large. Film adhesion, paint adhesion, and corrosion resistance were all insufficient.

比較例3は、空気中でリフロー処理した例である。酸化錫量が多く、フィルム密着性、塗料密着性、耐食性がいずれも不十分であった。   Comparative Example 3 is an example in which reflow treatment is performed in air. The amount of tin oxide was large, and film adhesion, paint adhesion, and corrosion resistance were all insufficient.

比較例4は、窒素-5%水素雰囲気中でリフロー処理、クエンチから1秒後に化成処理を施した例である。酸化錫量が非常に少なく、フィルム密着性、塗料密着性、耐食性がいずれも不十分であった。   Comparative Example 4 is an example in which chemical conversion treatment was performed 1 second after reflow treatment and quenching in a nitrogen-5% hydrogen atmosphere. The amount of tin oxide was very small, and film adhesion, paint adhesion, and corrosion resistance were all insufficient.

比較例5は、リン付着量の少ない例である。フィルム密着性、塗料密着性が不十分で、耐食性が劣っていた。   Comparative Example 5 is an example with a small amount of phosphorus adhesion. Film adhesion and paint adhesion were insufficient and corrosion resistance was poor.

比較例6は、リン付着量の多い例である。フィルム密着性、塗料密着性、耐食性がいずれも劣っていた。   Comparative Example 6 is an example with a large amount of phosphorus adhesion. Film adhesion, paint adhesion, and corrosion resistance were all poor.

比較例7は、化成処理層のカチオンがナトリウムの例である。フィルム密着性、塗料密着性を阻害され、耐食性が劣っていた。   Comparative Example 7 is an example in which the cation of the chemical conversion treatment layer is sodium. Film adhesion and paint adhesion were hindered and the corrosion resistance was poor.

Claims (3)

鋼板側から順に金属錫層、還元に要する電気量として0.3〜2.5mC/cm2の酸化錫層、Sn、Fe、Al、Mg、Ca、Ti、Ni、Co、Znの1種又は2種以上のリン酸塩又はポリメタリン酸塩をP量として0.1〜5mg/m2有する化成処理層を少なくとも有することを特徴とする缶用めっき鋼板。 In order from the steel sheet side, the metal tin layer, the amount of electricity required for reduction is 0.3 to 2.5 mC / cm 2 tin oxide layer, Sn, Fe, Al, Mg, Ca, Ti, Ni, Co, Zn, one or more A plated steel sheet for cans, comprising at least a chemical conversion treatment layer having 0.1 to 5 mg / m 2 of a phosphate or polymetaphosphate as a P amount. 前記化成処理層上に、Si量として0.05〜5mg/m2のシラノール基含有有機化合物を含む皮膜を有する請求項1記載の缶用めっき鋼板。 2. The plated steel sheet for cans according to claim 1, which has a film containing 0.05 to 5 mg / m 2 of a silanol group-containing organic compound on the chemical conversion treatment layer. 前記金属錫層の下地層として、Ni量として2〜100mg/m2のFe-Ni合金層又はFe-Ni-Sn合金層を有する請求項1又は2に記載の缶用めっき鋼板。 3. The plated steel sheet for cans according to claim 1, wherein the metal tin layer has an Fe—Ni alloy layer or Fe—Ni—Sn alloy layer having a Ni content of 2 to 100 mg / m 2 as an underlayer of the metal tin layer.
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