JP6684910B2 - 後処理被膜が形成された亜鉛系めっき鋼板及びその後処理方法 - Google Patents

後処理被膜が形成された亜鉛系めっき鋼板及びその後処理方法 Download PDF

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JP6684910B2
JP6684910B2 JP2018531396A JP2018531396A JP6684910B2 JP 6684910 B2 JP6684910 B2 JP 6684910B2 JP 2018531396 A JP2018531396 A JP 2018531396A JP 2018531396 A JP2018531396 A JP 2018531396A JP 6684910 B2 JP6684910 B2 JP 6684910B2
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post
coating
treatment
metal
zinc
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JP2019507238A (ja
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ヨ−ノ キム、
ヨ−ノ キム、
ヨン−グン キム、
ヨン−グン キム、
ヨン−ジュン パク、
ヨン−ジュン パク、
ヨン−ウン キム、
ヨン−ウン キム、
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Posco Holdings Inc
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Posco Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C2/00—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
    • C23C2/26—After-treatment
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/01—Layered products comprising a layer of metal all layers being exclusively metallic
    • B32B15/013—Layered products comprising a layer of metal all layers being exclusively metallic one layer being formed of an iron alloy or steel, another layer being formed of a metal other than iron or aluminium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B32B15/043—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of metal
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/18—Layered products comprising a layer of metal comprising iron or steel
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
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    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C—CHEMISTRY; METALLURGY
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    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C2/00—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
    • C23C2/04—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor characterised by the coating material
    • C23C2/06—Zinc or cadmium or alloys based thereon
    • C—CHEMISTRY; METALLURGY
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    • C23C20/02—Coating with metallic material
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    • C23C20/02—Coating with metallic material
    • C23C20/04—Coating with metallic material with metals
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    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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Description

本発明は、後処理被膜が形成された亜鉛系めっき鋼板及びその後処理方法に関する。
自動車板材として使用される亜鉛系めっき鋼板は、安価で耐食性に優れる上、表面外観に優れており、自動車の内・外板用としてその使用量が次第に増加している。上記めっき鋼板は、自動車製造工程でプレス成形工程、溶接や接着などの組立工程、脱脂工程、リン酸塩処理工程及び塗装工程を順次経るが、ここで、亜鉛めっき鋼板には潤滑性、溶接性、接着性、脱膜性、塗装性などの物性が要求される。
亜鉛系めっき鋼板は、鋼板上に形成されためっき層の組成及び製造方法によって物性が異なり、劣位にある物性については補完が必要である。例えば、溶融亜鉛めっき鋼板（ＧＩ）及び電気亜鉛めっき鋼板（ＥＧ）の場合、軟質のめっき層により、高圧かつ高速の摩擦を伴うプレス成形時にめっき層が脱離して金型のビード部などに融着されてしまうという問題がある。それにより、鋼板の表面にスクラッチやデントなどの欠陥が生じる。特に、溶融亜鉛めっき鋼板（ＧＩ）のように純粋な亜鉛で構成されるめっき層は、融点が低く、微量含まれるアルミニウム（Ａｌ）により溶接工程でめっき層成分が電極の表面に融着及び酸化して不導体汚染物を形成し、それにより連続打点数が低下するという問題がある。
また、合金化溶融亜鉛めっき鋼板（ＧＡ）の場合、高い表面摩擦係数により潤滑特性が不十分であるため、プレス成形時に素材自体が破断されたり硬いめっき層が剥離したりするパウダリング現象が生じるという問題がある。さらに、アルミニウム（Ａｌ）やマグネシウム（Ｍｇ）をめっき層に微量含む亜鉛合金めっき鋼板は、プレス成形性には優れているものの、極表層に存在する安定した金属酸化物により接着性に劣ったり、低融点の合金相により溶接時の連続打点数が少なくなったりするという問題がある。
このような問題を解決するため、自動車板材として使用される亜鉛系めっき鋼板の表面には後処理が必要であり、それにより劣位にある物性を向上させる必要がある。
後処理に関する技術としては、亜鉛めっき層の表面にリン酸塩層を形成する技術（特許文献１）及び金属酸化物層を形成する技術（特許文献２）がある。しかし、リン酸塩層を形成する技術は、表面調整、リン酸塩処理、水洗、乾燥などの過程が必要であり、実際の操業時にはかなりの設備空間と溶液管理が必要であり、めっき層との反応性に依存する処理方法であるため、亜鉛系めっき鋼板の種類に応じて溶液の組成を変更しなければならないという煩わしさがある。また、金属酸化物層を形成する技術は、めっき層の金属成分に制限があるため、全ての亜鉛系めっき鋼板に適用することができないという問題がある。
韓国公開特許第２００１−００７４５２７号公報 特開２０１４−１８５３８１号公報
本発明は、自動車用板材に要求される物性である潤滑性、溶接性、接着性、脱膜性及び塗装性に優れた亜鉛系めっき鋼板を提供する。
また、本発明は、簡単で安価な工程により亜鉛系めっき鋼板を後処理する方法を提供する。
本発明の一実施形態によると、鋼板、上記鋼板上に形成された亜鉛系めっき層、及び上記めっき層上に形成された後処理被膜を含み、上記後処理被膜は、金属酸化物塩及び有機化合物を含み、上記後処理被膜に含まれる酸素（Ｏ）と金属（Ｍ）の原子比（Ｏ／Ｍ）は、２超２０未満である、後処理被膜が形成された亜鉛系めっき鋼板を提供する。
上記後処理被膜は、被膜上部及び被膜下部に区分され、上記被膜上部は、酸素（Ｏ）と金属（Ｍ）の原子比（Ｏ／Ｍ）が５以上であり、上記被膜下部は、酸素（Ｏ）と金属（Ｍ）の原子比（Ｏ／Ｍ）が５未満であってもよい。
上記被膜上部は、酸素（Ｏ）と金属（Ｍ）の原子比（Ｏ／Ｍ）が３．２以上であり、上記被膜下部は、酸素（Ｏ）と金属（Ｍ）の原子比（Ｏ／Ｍ）が３．２未満であってもよい。
上記被膜下部は、厚さが上記後処理被膜全体の厚さの１／４〜３／４であってもよい。
上記金属酸化物塩は、モリブデン（Ｍｏ）、ホウ素（Ｂ）、ケイ素（Ｓｉ）、チタン（Ｔｉ）及びジルコニウム（Ｚｒ）からなる群から選択される１つ以上をさらに含んでもよい。
本発明の他の実施形態によると、亜鉛系めっき鋼板上に後処理コーティング溶液を塗布して乾燥させて後処理被膜を形成する段階を含み、上記後処理被膜に含まれる酸素（Ｏ）と金属（Ｍ）の原子比（Ｏ／Ｍ）が２超２０未満である、亜鉛系めっき鋼板の後処理方法を提供する。
上記後処理被膜は、被膜上部及び被膜下部に区分され、上記被膜上部は、酸素（Ｏ）と金属（Ｍ）の原子比（Ｏ／Ｍ）が５以上であり、上記被膜下部は、酸素（Ｏ）と金属（Ｍ）の原子比（Ｏ／Ｍ）が５未満であってもよい。
上記被膜下部は、厚さが上記後処理被膜全体の厚さの１／４〜３／４であってもよい。
上記後処理コーティング溶液は、ｐＨが３．０〜７．０であってもよい。
上記後処理被膜は、被膜付着量が１００〜１０００ｍｇ／ｍ２であってもよい。
本発明の後処理被膜が形成された亜鉛系めっき鋼板は、潤滑性、溶接性、接着性、脱膜性及び塗装性に優れているという効果がある。
また、本発明の亜鉛系めっき鋼板の後処理方法は、めっき層の種類に関係なく簡単なコーティング方式を採用することにより、工程が簡単かつ工程運用コストが安価で、経済的な効果がある。
以下、様々な実施形態を参照して本発明の好ましい実施形態について説明する。しかし、本発明の実施形態は、様々な他の形態に変形することができ、本発明の範囲が以下に説明する実施形態に限定されるものではない。
本発明は、後処理被膜が形成された亜鉛系めっき鋼板及びその後処理方法に関し、具体的には、鋼板、上記鋼板上に形成された亜鉛系めっき層、及び上記めっき層上に形成された後処理被膜を含み、上記後処理被膜は、金属酸化物塩及び有機化合物を含み、上記後処理被膜に含まれる酸素（Ｏ）と金属（Ｍ）の原子比（Ｏ／Ｍ）は、２超２０未満である、後処理被膜が形成された亜鉛系めっき鋼板を提供する。
本発明の後処理被膜が形成された亜鉛系めっき鋼板は、自動車用板材に要求される物性である潤滑性、溶接性、接着性、脱膜性及び塗装性に優れているという効果がある。
自動車製造工程では、自動車用板材にプレス成形工程、溶接や接着などの組立工程、脱脂工程、リン酸塩処理工程及び塗装工程が順次行われるが、ここで、上記自動車用板材には潤滑性、溶接性、接着性、脱膜性、塗装性などの物性が要求される。上記プレス成形工程で潤滑性が不十分な場合、素材自体が破断されたり硬いめっき層が剥離したりするパウダリング現象が生じることがある。上記組立工程で溶接性が不十分な場合、溶接時に溶接電極に汚染が発生して電極の寿命及び連続打点数が低下することがあり、接着性が不十分な場合、引張試験時に界面の剥離が生じることがある。また、上記脱脂工程で脱膜性が不十分な場合、後処理被膜が十分に除去されず、それにより後工程のリン酸塩処理及び塗装工程時に不良を起こすことがあり、塗装性が低下することがある。
自動車製造工程で要求される物性である潤滑性、溶接性、接着性、脱膜性及び塗装性を向上させるために、本発明の亜鉛系めっき鋼板は、めっき層上に形成された後処理被膜を含んでもよく、上記後処理被膜は、金属酸化物塩及び有機化合物を含んでもよい。また、上記後処理被膜に含まれる酸素（Ｏ）と金属（Ｍ）の原子比（Ｏ／Ｍ）を２超２０未満に制御してもよい。
上記後処理被膜中の酸素（Ｏ）と金属（Ｍ）の原子比（Ｏ／Ｍ）は、上記後処理被膜が形成された亜鉛系めっき鋼板をアセトン脱脂した後におけるＸＰＳ（Ｘ−ｒａｙ Ｐｈｏｔｏｅｌｅｃｔｒｏｎ Ｓｐｅｃｔｒｏｓｃｏｐｙ）分析法を用いたナノメートルスケールの単位深さ別の平均値である。
上記後処理被膜に含まれる酸素の含量は、亜鉛系めっき鋼板の物性を決定する重要な条件であり、特に、上記後処理被膜は、それに含まれる酸素（Ｏ）と金属（Ｍ）の原子比（Ｏ／Ｍ）が２超２０未満であることが好ましく、２超１０未満であることがより好ましい。
酸素（Ｏ）と金属（Ｍ）の原子比（Ｏ／Ｍ）が２以下であると、後処理被膜中の酸素の含量が少なすぎるため、プレス金型と鋼板間で潤滑性を付与する金属酸化物塩の分率が低くなって十分な潤滑性の確保が難しく、それにより、鋼板のプレス成形時にめっき層が脱離したり鋼板素材が破断されたりするという問題が生じることがある。また、融点が高い金属酸化物塩の分率が低くなることから、溶接工程で電極の汚染が増加して電極の寿命及び連続打点数が低下するため、溶接性の確保が難しい。さらに、オキソ（Ｏｘｏ）リガンドやヒドロキシ基などの酸素を媒体とする結合サイトが不足するため、亜鉛系めっき鋼板と接着剤間の接着強度を確保する接着性が低下することがある。
一方、酸素（Ｏ）と金属（Ｍ）の原子比（Ｏ／Ｍ）が２０以上であると、後処理被膜中の酸素の含量が過度に増え、特に、オキソ（Ｏｘｏ）リガンドや水酸基などの結合サイトの分率が高くなるため、脱膜性が低下することがある。これにより、上記後処理被膜が十分に除去されず、リン酸塩処理工程及び塗装工程時に不良を起こすことがあり、また、塗装性が低下することがある。
本発明の後処理被膜は、被膜上部及び被膜下部に区分され、上記被膜上部は、酸素（Ｏ）と金属（Ｍ）の原子比（Ｏ／Ｍ）が５以上であり、上記被膜下部は、酸素（Ｏ）と金属（Ｍ）の原子比（Ｏ／Ｍ）が５未満であることが好ましい。また、上記被膜上部は、酸素（Ｏ）と金属（Ｍ）の原子比（Ｏ／Ｍ）が３．２以上であり、上記被膜下部は、酸素（Ｏ）と金属（Ｍ）の原子比（Ｏ／Ｍ）が３．２未満であることがより好ましい。
本発明においては、上記被膜上部の酸素（Ｏ）と金属（Ｍ）の原子比（Ｏ／Ｍ）が５以上の高い酸素含量を有するように制御してもよい。こうすることにより、本発明の亜鉛系めっき鋼板の表層は、金属酸化物塩の分率が高いため、潤滑性及び溶接性に優れ、オキソリガンドやヒドロキシ基などの結合サイトが表層に密集するため、組立工程で接着剤との親和性を高めて接着強度を確保することができる。
また、本発明においては、上記被膜下部の酸素（Ｏ）と金属（Ｍ）の原子比（Ｏ／Ｍ）が５以下の低い酸素含量を有するように制御してもよい。こうすることにより、上記被膜下部は、塗装工程の前に行われる脱脂工程で後処理被膜の脱膜性を円滑に誘導することができるため、後工程のリン酸塩処理工程及び塗装工程時に不良を防止して塗装性を確保することができ、そして、優れた塗装性により耐食性を確保することができる。
一方、上記被膜下部の厚さは、後処理被膜全体の厚さの１／４〜３／４であってもよく、１／３〜２／３であることがより好ましい。上記被膜下部の厚さが後処理被膜全体の厚さの１／４未満であると、脱膜性に優れた被膜下部の占有率が低いため、リン酸塩処理や電着塗装時に欠陥を生じさせることがあり、３／４を超えると、密着力の不足により接着剤の接着強度の確保が難しいことがある。
上記後処理被膜に含まれる金属酸化物塩は、モリブデン（Ｍｏ）、ホウ素（Ｂ）、ケイ素（Ｓｉ）、チタン（Ｔｉ）及びジルコニウム（Ｚｒ）からなる群から選択される１つ以上をさらに含むことが好ましい。また、リン（Ｐ）を単独で含むか、又は上記リンと共に上記金属酸化物塩を含む後処理被膜であってもよい。
一方、上記有機化合物は、水酸基（−ＯＨ）を含む有機化合物であれば特に制限されない。例えば、ヒドロキシ基、カルボニル基などの官能基を備えた有機化合物であってもよく、また、例えば、ポリ酢酸ビニル（ＰＶＡｃ）、ポリビニルアルコール（ＰＶＡ）、ポリアクリル酸（ＰＡＡ）、ポリビニルブチラール（ＰＶＢ）、ポリエチレングリコール（ＰＥＧ）などを含む化合物であってもよい。
本発明の一実施形態によると、亜鉛系めっき鋼板上に後処理コーティング溶液を塗布して乾燥させて後処理被膜を形成する段階を含み、上記後処理被膜に含まれる酸素（Ｏ）と金属（Ｍ）の原子比（Ｏ／Ｍ）が２超２０未満である、亜鉛系めっき鋼板の後処理方法を提供する。
亜鉛系めっき鋼板の後処理時のコーティング方法としては、ＰＶＤ、ＣＶＤなどの乾式コーティング法、溶射コーティングなどの粉末噴射コーティング法、ロールコーティングなどといった溶液塗布法などがあるが、本発明は、めっき層の種類に関係なく、後処理コーティング溶液をめっき層上に簡単に塗布する溶液塗布法で後処理を行うことにより、工程が簡単かつ工程運用コストが安価で、経済的な効果がある。
上記後処理コーティング溶液を上記めっき層上に塗布して乾燥させて形成された後処理被膜は、酸素（Ｏ）と金属（Ｍ）の原子比（Ｏ／Ｍ）が２超２０未満であることが好ましく、上記原子比を上記範囲に制御する理由は前述した通りである。
本発明の後処理被膜は、被膜上部及び被膜下部に区分され、上記被膜上部は、酸素（Ｏ）と金属（Ｍ）の原子比（Ｏ／Ｍ）が５以上であり、上記被膜下部は、酸素（Ｏ）と金属（Ｍ）の原子比（Ｏ／Ｍ）が５未満であることが好ましい。また、上記被膜上部は、酸素（Ｏ）と金属（Ｍ）の原子比（Ｏ／Ｍ）が３．２以上であり、上記被膜下部は、酸素（Ｏ）と金属（Ｍ）の原子比（Ｏ／Ｍ）が３．２未満であることがより好ましい。一方、上記被膜下部の厚さは、後処理被膜全体の厚さの１／４〜３／４であってもよく、１／３〜２／３であることがより好ましい。上記被膜上部及び上記被膜下部の上記原子比を上記範囲に制御する理由及び上記被膜下部の厚さを上記範囲に制御する理由は前述した通りである。
上記後処理被膜に含まれる金属酸化物塩は、モリブデン（Ｍｏ）、ホウ素（Ｂ）、ケイ素（Ｓｉ）、チタン（Ｔｉ）及びジルコニウム（Ｚｒ）からなる群から選択される１つ以上をさらに含むことが好ましい。上記後処理コーティング溶液に含まれる金属酸化物塩は、コロイド状に分散した溶液を用いてもよく、酸化物の形態で溶液に溶解させて用いてもよい。
一方、上記有機化合物は、水酸基（−ＯＨ）を含む有機化合物であれば特に制限されない。例えば、ヒドロキシ基、カルボニル基などの官能基を備えた有機化合物であってもよく、また、例えば、ポリ酢酸ビニル（ＰＶＡｃ）、ポリビニルアルコール（ＰＶＡ）、ポリアクリル酸（ＰＡＡ）、ポリビニルブチラール（ＰＶＢ）、ポリエチレングリコール（ＰＥＧ）などを含む化合物であってもよい。
上記後処理コーティング溶液のｐＨは、特に限定されないが、めっき層が溶解することを防止して安定した被膜を形成するためには、ｐＨ３．０〜７．０であることが好ましい。
以下、具体的な実施例により本発明をより具体的に説明する。下記実施例は本発明の理解を助けるための例示にすぎず、本発明の範囲はこれに限定されるものではない。
＜実施例１＞
厚さ０．８ｍｍ、延伸率３６〜３７％、めっき量４０ｇ／ｍ２、めっき層がＡｌ２．５％、Ｍｇ３％、Ｚｎ９４．５％で構成される亜鉛系めっき鋼板を準備した。上記鋼板上にＭｏ１重量％、Ｂ０．２重量％を含有する金属酸化物塩、ＰＥＧ０．３重量％及び残部として水を含むコーティング溶液をバーコーティング法で塗布し、その後ＰＭＴ１００℃の条件で付着量が３００ｍｇ／ｍ２になるように後処理被膜を形成した。
＜実施例２＞
厚さ０．８ｍｍ、延伸率３６〜３７％、めっき量４０ｇ／ｍ２、めっき層がＡｌ２．５％、Ｍｇ３％、Ｚｎ９４．５％で構成される亜鉛系めっき鋼板を準備した。上記鋼板上にＭｏ１重量％、Ｂ０．５重量％を含有する金属酸化物塩、ＰＥＧ０．５重量％及び残部として水を含むコーティング溶液をバーコーティング法で塗布し、その後ＰＭＴ１００℃の条件で付着量が３００ｍｇ／ｍ２になるように後処理被膜を形成した。
＜実施例３＞
厚さ０．８ｍｍ、延伸率３６〜３７％、めっき量４０ｇ／ｍ２、めっき層がＡｌ２．５％、Ｍｇ３％、Ｚｎ９４．５％で構成される亜鉛系めっき鋼板を準備した。上記鋼板上にＭｏ１重量％、Ｂ１重量％を含有する金属酸化物塩、ＰＥＧ１重量％及び残部として水を含むコーティング溶液をバーコーティング法で塗布し、その後ＰＭＴ１００℃の条件で付着量が３００ｍｇ／ｍ２になるように後処理被膜を形成した。
＜実施例４＞
厚さ０．８ｍｍ、延伸率３６〜３７％、めっき量４０ｇ／ｍ２、めっき層がＡｌ２．５％、Ｍｇ３％、Ｚｎ９４．５％で構成される亜鉛系めっき鋼板を準備した。上記鋼板上にＭｏ０．５重量％、Ｂ１重量％を含有する金属酸化物塩、ＰＥＧ１．５重量％及び残部として水を含むコーティング溶液をバーコーティング法で塗布し、その後ＰＭＴ１００℃の条件で付着量が３００ｍｇ／ｍ２になるように後処理被膜を形成した。
＜比較例１＞
厚さ０．８ｍｍ、延伸率３６〜３７％、めっき量４０ｇ／ｍ２、めっき層がＡｌ２．５％、Ｍｇ３％、Ｚｎ９４．５％で構成される亜鉛系めっき鋼板を準備し、上部に後処理被膜を形成しなかった。
＜比較例２＞
厚さ０．８ｍｍ、延伸率３６〜３７％、めっき量４０ｇ／ｍ２、めっき層がＡｌ２．５％、Ｍｇ３％、Ｚｎ９４．５％で構成される亜鉛系めっき鋼板を準備した。上記鋼板上にＭｏ１重量％を含有する金属酸化物塩、ＰＥＧ ０．１重量％及び残部として水を含むコーティング溶液をバーコーティング法で塗布し、その後ＰＭＴ１００℃の条件で付着量が３００ｍｇ／ｍ２になるように後処理被膜を形成した。
＜比較例３＞
厚さ０．８ｍｍ、延伸率３６〜３７％、めっき量４０ｇ／ｍ２、めっき層がＡｌ２．５％、Ｍｇ３％、Ｚｎ９４．５％で構成される亜鉛系めっき鋼板を準備した。上記鋼板上にＭｏ１重量％、Ｂ０．５重量％を含有する金属酸化物塩、ＰＥＧ３重量％及び残部として水を含むコーティング溶液をバーコーティング法で塗布し、その後ＰＭＴ１００℃の条件で付着量が３００ｍｇ／ｍ２になるように後処理被膜を形成した。
上記実施例１〜４及び上記比較例１〜３の後処理被膜の酸素（Ｏ）と金属（Ｍ）の原子比（Ｏ／Ｍ）を測定して表１に示した。上記原子比は、上記後処理被膜が形成された亜鉛系めっき鋼板をアセトン脱脂した後におけるＸＰＳ（Ｘ−ｒａｙ Ｐｈｏｔｏｅｌｅｃｔｒｏｎ Ｓｐｅｃｔｒｏｓｃｏｐｙ）分析法を用いたナノメートルスケールの単位深さ別の平均値である。上部と下部の境界は総厚さの１／２地点にした。酸素（Ｏ）と金属（Ｍ）の原子比（Ｏ／Ｍ）の条件に応じた物性を評価するために、加工性、接着性及び脱膜性を評価し、その結果は表１に示した。
＜加工性評価＞
加工性を評価するためにカップ絞り試験（ｃｕｐ ｄｒａｗｉｎｇ ｔｅｓｔ）を実施し、上記カップ絞り試験では、金型とパンチとで構成された試験機を用いて、ＢＨＦ（Ｂｌａｎｋ Ｈｏｌｄｉｎｇ Ｆｏｒｃｅ）を高めながら試験を行い、素材の破断が起こる直前のＢＨＦ値を最大ＢＨＦ値として表１に記載した。最大ＢＨＦ値が大きいほど加工性に優れていることを意味し、本実施例で施行したカップ絞り試験の詳細条件は以下の通りである。
※カップ絞り試験の詳細条件
・パンチの直径（Ｐｕｎｃｈ ｄｉａｍｅｔｅｒ）：５０ｍｍ
・パンチの端部の半径（Ｐｕｎｃｈ ｅｄｇｅ ｒａｄｉｕｓ）：６ｍｍ
・金型の直径（Ｄｉｅ ｄｉａｍｅｔｅｒ）：５２．２５ｍｍ
・パンチの移動速度：２３０ｍｍ／分
・後処理被膜は金型に接触させ、表面に洗浄油を塗布した後に試験を実施した。
＜接着性評価＞
接着性試験は、２５ｍｍ×１００ｍｍの大きさで試料２枚を製作し、洗浄油を塗布してから垂直に立てて１日放置し、その後、試料の端部から１０ｍｍ内側に２５ｍｍ（幅）×２５ｍｍ（長さ）×３ｍｍ（高さ）の大きさでマスチックシーラ（ｍａｓｔｉｃ ｓｅａｌｅｒ）接着剤を塗布し、他の試料を重ねて１７０℃で２０分間硬化させ、次いで、上下の試料の接着剪断強度を測定し、その結果を表１に示した。剪断強度は５０ｍｍ／分の速度で測定し、測定された最大剪断力を接着面積６．２５ｃｍ２で割って表記した。
＜脱膜性評価＞
脱膜性試験は、自動車製造工程に使用される脱脂溶液を用いて５０〜５５℃で２分間素材を攪拌浸漬して水洗し、その後、素材の表面に残留するコーティング被膜の量を測定し、脱脂前の被膜付着量に対する脱膜率を百分率で計算して表１に示した。コーティング被膜の残留量は、所定の面積のコーティング層を酸溶液で溶解し、その後、溶解溶液のモリブデン含量をＩＣＰ（Ｉｎｄｕｃｔｉｖｅｌｙ Ｃｏｕｐｌｅｄ Ｐｌａｓｍａ）で定量分析して面積当たりの残留量を計算した。
Figure 0006684910
上記表１に示したように、後処理コーティング被膜が形成された実施例１〜６は、後処理していない比較例１に比べて、最大ＢＨＦ値及び接着強度が著しく高いことから、実施例１〜６は自動車用板材として使用可能な物性である加工性及び接着性に著しく優れていることが確認された。
また、酸素（Ｏ）と金属（Ｍ）の原子比（Ｏ／Ｍ）が２超２０未満である実施例１〜６は、９５％以上の脱膜率を有することから、脱膜性に優れていることが確認された。しかし、酸素（Ｏ）と金属（Ｍ）の原子比（Ｏ／Ｍ）が２以下である比較例２は、加工性及び接着性が劣位であり、酸素（Ｏ）と金属（Ｍ）の原子比（Ｏ／Ｍ）が２０以上である比較例３は、加工性及び接着性は良好であるが、脱膜率が８７％以下であることから、脱膜率が劣位であることが確認された。
以上、本発明の実施形態について詳細に説明したが、本発明の権利範囲は、これに限定されるものではなく、請求の範囲に記載された本発明の技術的思想から逸脱しない範囲内で様々な修正及び変形が可能であることは当該技術分野における通常の知識を有する者には自明である。

Claims (5)

  1. 鋼板と、
    前記鋼板上に形成された亜鉛系めっき層と、
    前記めっき層上に形成された後処理被膜とを含み、
    前記後処理被膜は、金属酸化物塩及び有機化合物を含み、
    前記後処理被膜に含まれる酸素（Ｏ）と金属（Ｍ）の原子比（Ｏ／Ｍ）は、２超２０未満であり、
    前記金属は、モリブデン（Ｍｏ）、ホウ素（Ｂ）、チタン（Ｔｉ）及びジルコニウム（Ｚｒ）からなる群から選択される１つ以上を含み、
    前記有機化合物は、ポリ酢酸ビニル（ＰＶＡｃ）、ポリビニルアルコール（ＰＶＡ）、ポリアクリル酸（ＰＡＡ）、ポリビニルブチラール（ＰＶＢ）及びポリエチレングリコール（ＰＥＧ）からなる群から選択される１つ以上を含み、
    前記後処理被膜は、後処理被膜全体の厚さの１／４〜３／４厚さの被膜下部及び残部厚さの被膜上部に区分され、
    前記被膜上部は、酸素（Ｏ）と金属（Ｍ）の原子比（Ｏ／Ｍ）が５以上であり、
    前記被膜下部は、酸素（Ｏ）と金属（Ｍ）の原子比（Ｏ／Ｍ）が５未満である、後処理被膜が形成された亜鉛系めっき鋼板。
  2. 前記被膜上部は、酸素（Ｏ）と金属（Ｍ）の原子比（Ｏ／Ｍ）が３．２以上であり、
    前記被膜下部は、酸素（Ｏ）と金属（Ｍ）の原子比（Ｏ／Ｍ）が３．２未満である、請求項１に記載の後処理被膜が形成された亜鉛系めっき鋼板。
  3. 亜鉛系めっき鋼板上に金属酸化物塩及び有機化合物を含む後処理コーティング溶液を塗布して乾燥させて後処理被膜を形成する段階を含み、
    前記後処理被膜に含まれる酸素（Ｏ）と金属（Ｍ）の原子比（Ｏ／Ｍ）が２超２０未満であり、
    前記金属は、モリブデン（Ｍｏ）、ホウ素（Ｂ）、チタン（Ｔｉ）及びジルコニウム（Ｚｒ）からなる群から選択される１つ以上を含み、
    前記有機化合物は、ポリ酢酸ビニル（ＰＶＡｃ）、ポリビニルアルコール（ＰＶＡ）、ポリアクリル酸（ＰＡＡ）、ポリビニルブチラール（ＰＶＢ）及びポリエチレングリコール（ＰＥＧ）からなる群から選択される１つ以上を含み、
    前記後処理被膜は、後処理被膜全体の厚さの１／４〜３／４厚さの被膜下部及び残部厚さの被膜上部に区分され、
    前記被膜上部は、酸素（Ｏ）と金属（Ｍ）の原子比（Ｏ／Ｍ）が５以上であり、
    前記被膜下部は、酸素（Ｏ）と金属（Ｍ）の原子比（Ｏ／Ｍ）が５未満である、亜鉛系めっき鋼板の後処理方法。
  4. 前記後処理コーティング溶液は、ｐＨが３．０〜７．０である、請求項３に記載の亜鉛系めっき鋼板の後処理方法。
  5. 前記後処理被膜は、被膜付着量が１００〜１０００ｍｇ／ｍ２である、請求項３又は４に記載の亜鉛系めっき鋼板の後処理方法。
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