TW201224206A - Steel sheet for container and method for manufacturing therefor - Google Patents

Steel sheet for container and method for manufacturing therefor Download PDF

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Publication number
TW201224206A
TW201224206A TW100133007A TW100133007A TW201224206A TW 201224206 A TW201224206 A TW 201224206A TW 100133007 A TW100133007 A TW 100133007A TW 100133007 A TW100133007 A TW 100133007A TW 201224206 A TW201224206 A TW 201224206A
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TW
Taiwan
Prior art keywords
steel sheet
film
layer
acid
amount
Prior art date
Application number
TW100133007A
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English (en)
Other versions
TWI490370B (zh
Inventor
Takeshi Suzuki
Norihiko Nakamura
Yuka Miyamoto
Yoichi Tobiyama
Original Assignee
Jfe Steel Corp
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Publication of TW201224206A publication Critical patent/TW201224206A/zh
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Publication of TWI490370B publication Critical patent/TWI490370B/zh

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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
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • 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
    • B32B1/00—Layered products having a general shape other than plane
    • B32B1/08—Tubular products
    • 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
    • B32B15/08—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 synthetic resin
    • B32B15/09—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 synthetic resin comprising polyesters
    • 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
    • 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
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • 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
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
    • C—CHEMISTRY; METALLURGY
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    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
    • C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
    • C23C22/34—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing fluorides or complex fluorides
    • 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
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    • C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
    • C23C22/34—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing fluorides or complex fluorides
    • C23C22/36—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing fluorides or complex fluorides containing also phosphates
    • 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
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/82—After-treatment
    • C23C22/83—Chemical after-treatment
    • 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
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
    • C23C28/32—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer
    • 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
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
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    • C23C28/321—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer with at least one metal alloy layer
    • 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
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Description

201224206 六、發明說明： 【發明所屬之技術領域】 本發明主要是關於罐等容器加工所使用的金屬板，尤 其是與塑膠薄膜等有機樹脂的密接性優異的容器用鋼板及 其製造方法。 【先前技術】 飲料罐、食品罐、提桶或18公升提桶等的各種金屬 罐是使用鍍錫鋼板或稱無鍍錫薄鋼板的電解鉻酸處理鋼板 等的金屬板。其中，無鍍錫薄鋼板是在含6價鉻的浴中電 解處理鋼板所製造，具有塗料等優異的樹脂密接性等特長 〇 近年來，從對於環境意識的高漲，世界性地朝著限制 6價鉻使用的方向，在製造上針對所使用6價鉻浴的無鍍 錫薄鋼板尋求一種代替材。作爲不使用鉻的無鍍錫薄鋼板 的代替材有例如專利文獻1所掲示的鎢酸溶液中施以電解 處理的容器用鋼板。並在專利文獻2中，提出表面以Zr 、〇、F爲主成份，形成有幾乎不含磷酸離子之無機表面 處理層的表面處理金屬材料。 另一方面，各種金屬罐，自以往即對於無鍍錫薄鋼板 等的金屬板施以塗層之後，加工製造成罐體，但是近年來 ’爲了抑制伴隨製造所產生的廢棄物，多使用將層疊塑膠 薄膜等樹脂的層疊金屬板（樹脂包覆金屬板）來取代塗層加 工成罐體的方法。該層疊金屬板必須將樹脂與金屬板牢固 -5- 201224206 地密接，尤其是作爲飲料罐或食品罐所使用的層疊金屬板 ，在頸部份施以拉深旋轉加工，在內容物塡充後有經蒸餾 殺菌處理步驟的場合，所以要求即使在高溫的濕潤環境下 仍不致使加工率高的鋼板-樹脂的密接部剝離之強的樹脂 密接性。以加工率高的罐用鋼板，尋求優異的熔接性、抗 蝕性、塗料密接性，並進一步尋求薄膜密接性，尤其是高 加工部的薄膜密接性（以下，稱高薄膜密接性）優異的容器 用鋼板。 〔先前技術文獻〕 〔專利文獻〕 〔專利文獻1〕日本特開2004-285380號公報 〔專利文獻1〕日本特開2005-97712號公報 【發明內容】 〔發明所欲解決之課題〕 本發明進一步以提供高薄膜密接性優異的容器用鋼板 爲目的。 〔解決課題用的手段〕 本發明人，爲達成上述目的加以努力硏究的結果，發 現在含Zr離子、F離子的溶液中，藉著浸漬或電解處理 的進行在鋼板上所形成的Zr化合物薄膜上具有羥基酸處 理層的鋼板即有著高薄膜密接性優異以致創出本發明。
S -6- 201224206 亦即，本發明提供如下述。 (1) 容器用鋼板，具有：在含Zr離子、F離子的溶 液中，浸漬或電解處理鋼板所形成的附著量爲金屬Zr量 0.1〜100mg/m2、F量0.1 mg/m2以下的化學轉化處理膜， 及在該化學轉化處理膜上，附著量爲C量0.05~50mg/m2 的羥基酸處理層。 (2) 如（1)記載的容器用鋼板，上述溶液中，進一步 含磷酸離子，上述化學轉化處理膜的附著量，進一步爲P 量 0.1~50mg/m2。 (3) 如（1)或（2)記載的容器用鋼板，上述羥基酸是從 檸檬酸、酒石酸、乙醇酸、乳酸、甘油酸及扁桃酸中所選 擇至少一種。 (4) 如（1)至（3)其中之一記載的容器用鋼板，上述鋼 板在至少單面具有含 Ni量 5〜1 000mg/m2或 Sn量 100〜1 5000mg/m2之表面處理層的表面處理鋼板。 (5) 如（1)至（4)其中之一記載的容器用鋼板，上述鋼 板爲具有含Ni量5〜150mg/m2，Ni電鍍或Fe-Ni合金電鍍 相的基底 Ni層，及在上述基底 Ni層上施以 3 00〜3000mg/m2的Sri電鍍，藉熔融熔錫處理使得上述基 底Ni層的一部份或全部與上述Sn電鍍層的一部份合金化 ’而由上述Sn電鍍層未加以合金化的剩餘部所形成的島 狀Sn電鍍層的表面處理鋼板。 (6) 如（1)至（5)其中之一記載的容器用鋼板之製造方 201224206 在含Zr離子、F離子的溶液中，浸漬或電解處理鋼 板， 在上述鋼板上形成附著量爲金屬Zr量〇.l~l〇〇mg/m2 ，F量0· lmg/m2以下的化學轉化處理膜，並將具有該化 學轉化處理膜的鋼板浸漬在含羥基酸的水溶液中，或在該 化學轉化處理膜上塗佈含羥基酸的水溶液，使其乾燥。 (7) 如（6)記載的容器用鋼板之製造方法，上述乾燥 步驟的溫度爲70°C以上。 (8) 如（6)或（7)記載的容器用鋼板之製造方法，在上 述乾燥步驟之後，以80°C以上溫度的水清洗，並加以乾 燥。 〔發明效果〕 根據本發明，可提供熔接性、抗蝕性、塗料密接性優 異，並具優異薄膜密接性的容器用鋼板、其製造方法及使 用該鋼板之金屬罐、罐蓋。 【實施方式】 以下，針對本發明容器用鋼板加以詳細說明。 1.本發明所使用的原板尤其不加以限制，通常，使 用作爲容器材料所使用的鋼板。該原板的製造法、材質等 尤其不加以特別限制，可使用從通常的鋼片製造步驟經熱 軋、酸洗、冷軋、退火、冷精軋等的各步驟來製造。該原 板或對原板賦予含Ni、Sn中之1種以上的表面處理層。 -8 -
S 201224206 對於賦予的方法尤其不加以限定。 2.表面處理 表面處理鋼板具有在鋼板的至少一方的面含有Sn(錫） 或Ni (.鎳）的表面處理層。表面處理層雖不加以特別限定， 但以每單面含 Ni 量 5~1000mg/m2 或含 Sn 量 1 00〜1 5 0 0 0mg/m2 爲佳。
Sn可發揮優異的加工性、熔接性、抗蝕性，發現此 —效果是金屬Sn在100mg/m2以上爲佳。爲確保充分的溶 接性是以200mg/m2以上，爲確保充分的加工性則是賦予 1 000mg/m2以上爲佳。隨著Sn附著量的增加，雖會增加 Sn優異的加工性、熔接性的提升效果，但是超過 1 5 000mg/m2以上會使得抗蝕性的提升效果飽和而不利於 經濟性。因此，Sn的附著量是以金屬Sn在1 5000mg/m2 以下爲佳。並且，Sn電鍍後進行逆流處理形成有Sn合金 層，可進一步提升抗蝕性。
Ni對於塗料密接性、薄膜密接性、抗蝕性、熔接性 可發揮其效果，因此，金屬Ni量是以5mg/m2以上爲佳》 隨著Ni附著量的增加，雖會增加Ni優異的薄膜密接性、 抗蝕性、熔接性的提升效果，但是超過1 000mg/m2以上會 使其提升效果飽和而不利於經濟性。因此，進一步Ni的 附著量是以金屬Ni在l〇mg/m2以上、1000mg/m2以下爲 佳。 具體而言，以使用Ni或Sn的電銨層爲佳。從包含在 -9- 201224206 其上所形成的Zr薄膜的化學轉化處理膜之均勻包覆性的 點爲佳的電鏟層是形成Fe-Sn-Ni合金層，或Fe-Sn合金 層的單一層所成的中間層，或在最下層爲Fe-Ni合金層， 在其上面爲Fe-Sn-Ni合金層的複合層所成的中間層，並 具有含形成在上述中間層上面的金屬Sn層之電鍍層的鋼 板。 更具體而言，表面處理鋼板爲具有，含 Ni爲 5~150mg/m2的Ni電鍍或Fe-Ni合金電鍍相的基底Ni層 ，及在上述基底Ni層上施以1 〇〇~3 00 0mg/m2的Sn電銨， 藉熔融熔錫處理使上述基底Ni層的一部份或全部與上述
Sn電鍍層的一部份合金化，具有由上述Sn電鍍層之未合 金化的剩餘部所形成的島狀的Sn電鍍層的表面處理鋼板 〇 電鍍層的s η附著量小於1 ο 〇 m g / m 2有抗ΙΦ性劣化的傾 向。另一方面，超過3 000mg/m2則電鎪層會變得過厚，會 有減小成本效應的場合。再者，Sn附著量可藉著電解剝 離法或螢光X射線進行表面分析來測定。 對施以鋼板或鎳系電鍍的電鍍鋼板施以Sn電鍍之後 進行的熔融熔錫處理也稱爲逆流處理，在Sn電鍍之後， 將溫度上升至Sn熔點的23 2 °C以上使得表面的Sn熔融， 使其表面光澤呈現而進行。並進行熔融熔錫處理使表面的 Sn熔融，與基底鋼板或基底金屬合金化以形成Sn_Fe合 金層或Sn-Fe-Ni合金層，來提升合金層的抗蝕性。又， 適當控制該熔融熔錫處理，可形成島狀Sn。藉此，可製
S -10- 201224206 造具有使不存在有金屬Sn的塗料及薄膜密接性優異的 Fe-Ni合金電鍍層或Fe-Ni-Sn合金電鍍層露出的電鍍構造 的表面處理鋼板。 3 .化學轉化處理膜 鋼板上直接，或在含該等的Ni、Sn的1種以上之表 面處理層的上層，賦予含Zr化合物與F的化學轉化處理 膜以獲得化學轉化處理膜。賦予該等薄膜的方法有藉著將 鋼板浸漬在溶解Zr離子、F離子後的酸性水溶液的方法 及陰極電解處理進行的方法。浸漬處理係蝕刻基底形成有 各種的薄膜，因此處理時間長，不利於工業生產性。另一 方面，陰極電解處理是隨著強制性電荷移動及在鋼板界面 產生氫使表面清潔化與藉著pH上升獲得附著促進效果， 可獲得均勻的薄膜。另外，該陰極電解處理中，根據在處 理液中共存著硝酸離子與銨離子，可以數秒乃至數十秒程 度的短時間處理來促進抗蝕性及密接性的提升效果優異的 含Zr氧化物、或Zr磷氧化物的Zr化學轉化處理膜的析 出，在工業上極爲有利。因此，化學轉化處理膜的賦予是 以陰極電解處理爲佳，尤其是以硝酸離子和銨離子共存之 處理液的陰極電解處理爲佳。 又，陰極電解處理的處理液中的銨離子的濃度在 100~1 0000 質量 ppm 程度，硝酸離子的濃度在 1 000〜20000質量ppm程度範圍，可根據生產設備及生產 速度（能力）來適當調整即可。陰極電解處理可設電流密度 -11 - • »-· 201224206 爲0.05〜50A/dm2，電解時間爲0.01〜10秒。
Zr化合物的功能爲抗蝕性與密接性的確保。Zr化合 物主要是以氧化Zr、氫氧化Zr所構成的Zr水合氧化物 、Zr磷氧化物，但該等的Zr化合物具有優異的抗蝕性與 密接性。因此，Zr薄膜增加時，抗蝕性與密接性會開始 提升，金屬Zr量一旦形成lmg/m2以上時，實用上，可確 保無問題位準的抗蝕性與密接性。另外，Zr薄膜量增加 時抗蝕性、密接性的提升效果也會增加，但是Zr薄膜量 在金屬Zr量超過100mg/m2時，Zr薄膜會變得過厚使得 Zr薄膜本身的密接性劣化，而有電阻上升使熔接性劣化 。因此，Zr薄膜附著量是以金屬ΖΓ量1〜100mg/m2。 銷薄膜的附著量是以金屬銷量〇.lmg/m2~9mg/m2爲佳 。更佳的是錐薄膜的附著量是爲金屬锆量lmg/m2~8mg/m2 "設鉻薄膜的附著量在此範圍內，可確保蒸餾後的抗蝕性 ，並獲得均質性高且加工性優異的薄膜。 又，Zr磷氧化物增加時雖可發揮更優異的抗蝕性與 密接性，但可明確辨識其效果爲金屬P量在0· lmg/m2以 上。磷酸薄膜量增加時也會增加抗蝕性、密接性的提升效 果，但是磷酸薄膜量在P量超過50mg/m2時，磷酸薄膜會 變得過厚而使磷酸薄膜本身的密接性劣化並使電阻上升使 其溶接性劣化。因此，磷酸薄膜附著量是以 P量 0.1~50mg/m2爲佳。磷酸薄膜的附著量是以金屬 P量 0.lmg/m2〜8mg/m2爲佳，較佳的是磷酸薄膜的附著量爲金 屬 P量 lmg/m2〜6mg/m2。設磷酸薄膜的附著量在
S -12- 201224206 lmg/m2~6mg/m2的範圍，可確保蒸餾後的抗蝕性’並獲得 均質性高的化學轉化處理膜。 F是包含於形成化學轉化處理膜的水溶液中’所以和 Zr化合物一起被結合於薄膜中。薄膜中的F雖然對於塗 料密接性或薄膜密接性（第一密接性）不會有影響’但會造 成蒸餾處理等高溫殺菌處理時的密接性（第二密接性）與抗 鏽性或塗膜下腐蝕性劣化的原因。其理由可能是薄膜中的 F溶出於水蒸氣或腐蝕液，使得與有機薄膜的結合分解’ 或造成基底鋼板腐蝕的原因。薄膜中的F量一旦超過 0.1 mg/m2時，由於開始使得該等諸特性的劣化明顯化， 所以F量在〇.lmg/m2以下爲佳。設F量在0_lmg/m2以下 是只要在化學轉化處理膜上形成羥基酸處理層’乾燥後’ 藉溫水中的浸漬處理或噴灑處理進行清洗處理即可。藉著 高的該處理溫度或長的處理時間即可減少！^量。因此’爲 了設薄膜中的F量在0.1 mg/m2以下，以80°C以上的溫水 進行浸漬處理或噴灑處理爲佳。清洗處理之後乾燥。乾燥 溫度不加以限定但以70 °C以上爲佳。 此外，本發明有關的化學轉化處理膜中所含有的金屬 Zr量、P量、F量，例如可藉螢光X射線分析等的定量分 析法來測定。 4.羥基酸處理層 對於如上述所獲得的化學轉化處理膜上賦予羥基酸處 理層。雖不限定賦予的方法，但以將化學轉化處理膜鋼板 -13- 201224206 浸漬於羥基酸水溶液，或將羥基酸水溶液塗佈在化學轉化 處理膜上的方法爲佳。浸漬或塗佈後乾燥。乾燥溫度雖不 加以限定但以70°C以上爲佳。其理由爲可短時間充分埤 乾燥。 羥基酸爲1分子中具有羧基與醇式羥基的有機化合物 的總稱，本發明中，可使用從檸檬酸、酒石酸、乙醇酸、 乳酸、甘油酸及扁桃酸中所選擇至少一種的酸。也可以使 用1種羥基酸或混用2種以上。並可在羥基酸中混合酚醛 樹脂使用。設混合率小於有機物成份的5 0質量％。 該羥基酸處理層的形成方法是將上述的羥基酸溶解於 水或有機溶劑，以溶液塗佈於鋼板上之後，乾燥的方法爲 佳。塗佈的方法可使用各種習知的塗佈法。爲縮短乾燥時 間，依需要也可設置將鋼板加熱的步驟。並且，藉乾燥形 成薄膜之後，以經由清洗步驟將殘存在金屬上多餘的羥基 酸及/或F除去爲佳。此時，尤其不須以強力的清洗，只 要浸漬在水中或以水噴灑的程度即可。清洗後，再次乾燥 可供實用。 羥基酸處理層的附著量在C量小於0.05mg/m2時，樹 脂密接性的改善效果不充分，大於50mg/m2則在有機薄膜 中產生凝聚破壞，反而會有使得樹脂密接性降低之虞，因 此以0.05〜50mg/m2爲佳。再者，含於羥基酸處理層中的 C量可使用TOC(總有機碳分析儀），藉減去存在鋼板中的 C量來測定。 本發明的鋼板上具有Zr化學轉化處理膜與羥基酸處 -14-
S 201224206 理層的本發明的密接性薄膜是由於羥基酸處理層構成功能 基多的界面，因此進一步在上層形成樹脂包覆層時羥基酸 處理層與其上層的薄膜密接性高。 5.有機樹脂包覆（層疊） 本發明的容器用鋼板可在上述化學轉化處理膜上，包 覆樹脂以製造樹脂包覆鋼板。如上述，本發明的容器用鋼 板具有優異的高加工部的薄膜密接性（高薄膜密接性）。這 是由於羥基酸處理層具有多數的官能基，與樹脂薄膜（有 機樹脂）形成化學結合。 包覆於容器用鋼板原板或表面處理鋼板的樹脂尤其不 加以限定，但可舉例各種熱可塑性樹脂或熱固性樹脂。例 如聚乙烯、聚丙烯、乙烯-丙烯共聚物、乙烯-乙烯乙酸共 聚物、乙烯-丙烯酸酯共聚物、離子鍵聚合物等的烯烴系— 樹脂薄膜，或聚對苯二甲酸丁二醇酯等的聚酯薄膜，或尼 龍6、尼龍6’ 6、尼龍11、尼龍12等的聚醯亞胺、聚氯 乙烯薄膜 '聚亞氯乙烯薄膜等的熱可塑性樹脂薄膜的未延 伸或雙軸延伸的薄膜。層疊時使用黏接劑的場合，以使用 聚氨酯系黏接劑、環氧系黏接劑、酸變性烯烴系樹脂黏接 劑、共聚醯胺系黏接劑、共聚酯系黏接劑（厚度： 〇· 1〜5·0μιη)等爲佳。另外，也可將熱固性塗料以厚度 〇· 05 ~2μιη的範圍塗佈於表面處理鋼板側或薄膜側，以此 作爲黏接劑。 另外，也可以酚醛環氧、氨基環氧等的變性環氧塗料 -15- 201224206 、氯乙烯-乙酸乙烯共聚物、氯乙烯-乙酸乙烯共聚體皂化 物、氯乙烯·乙酸乙烯-順酐共聚物、環氧變性·、環氧胺 變性-、環氧酚醛變性-乙烯塗料或變性乙烯塗料、丙烯塗 料、苯乙烯丁二烯共聚物等合成橡膠系塗料等的熱可塑性 或熱固性塗料的單獨或2種以上的組合* 樹脂包覆層的厚度爲3〜50μιη，尤其以設5~40μιη的 範圍爲佳。厚度低於上述範圍時則抗蝕性不足，厚度大於 上述範圍時在加工性的點容易產生問題。 本發明對羥基酸處理鋼板之樹脂包覆層的形成是可以 任意的手段進行。例如可藉擠壓塗層法、澆注薄膜熱黏接 法、雙軸向延伸薄膜熱黏接法等進行。擠壓塗層法的場合 ’可以樹脂熔融狀態擠壓塗層於表面處理鋼板之上，藉熱 黏接來製造。亦即，在以擠壓機使樹脂熔融混練之後，從 Τ模呈薄膜狀擠壓出，使擠壓後的熔融樹脂膜和表面處理 鋼板一起通過一對的層壓輥間在冷卻下擠壓形成一體化， 接著急速冷卻。在多層的樹脂包覆層進行擠壓塗層的場合 ，使用複數的各層用的擠壓機，使來自各擠壓機的樹脂流 在多重多層模內合流，以後以和單層樹脂的場合同樣進行 擠壓塗層即可。又，在一對層壓輥間使表面處理鋼板垂直 地通過，朝其兩側供應熔融樹脂帶，藉此在表面處理鋼板 兩面形成樹脂包覆層。’ 如此的樹脂包覆鋼板可運用於具有側面接頭之三片罐 或無縫罐（兩片罐）。並可運用於留置式拉環的易開罐蓋或 全開式的易開罐蓋等。 -16-
S .201224206 6.金屬罐及罐蓋 金屬罐的製造方法是僅限於上述的樹脂包覆鋼板所形 成，可使用任意的製罐法。該金屬罐也可以是具有側面接 頭的三片罐，但一般是以無縫罐（兩片罐）爲佳。該無縫罐 可以拉深暨再拉深加工、拉深暨再拉深進行的彎曲延展加 工（延伸加工）、拉深暨再拉深進行之彎曲延展暨旋轉加工 ’或者拉深暨旋轉加工，頸部的縮頸加工等習知的加工方 法製造使樹脂包覆鋼板的有機樹脂的包覆面形成罐內面側 〇 又，罐蓋是僅限於上述的樹脂包覆鋼板所形成，可使 用以往習知任意的製蓋法。一般可以留置式拉環的易開罐 蓋或全開式的易開罐蓋的加工方法製造。 上述的說明僅是說明本發明的實施形態的一例，可在 本發明的申請專利範圍內加以種種的變更。 〔實施例〕 以下，表示實施例具體說明本發明。本發明不限於此 <鋼板上的表面處理層> 使用以下的處理法（1)〜（6)的方法，對板厚 0.17〜0.23 mm的鋼板上賦予表面處理層。 (處理法1)冷軋後，對退火、調壓後的原板脫脂、 酸洗後，使用電鍍浴進行Sn電鍍，製作Sn電鍍鋼板❶ 201224206 (處理法2)冷軋後，使用瓦特浴施以Ni電鏟，退火 時形成Ni擴散層，製作Ni電鍍鋼板。 (處理法3)冷軋後，將退火、調壓後的原板脫脂、 酸洗後，使用電鍍浴施以Sn電鍍，隨後，進行逆流處理 ，製作具有Sn合金層的Sn電鍍鋼板》 (處理法4)冷軋後，將退火、調壓後的原板脫脂、 酸洗後，使用硫酸鹽酸浴施以Fe-Ni合金電鍍，接著， 使用電鍍浴施以Sn電鍍，製作Ni、Sn電鍍鋼板。 (處理法5)冷軋後，將退火、調壓後的原板脫脂、 酸洗後，使用硫酸-鹽酸浴施以Sn-Ni合金電鍍，製作Ni 、S η電鑛鋼板。 (處理法6)冷軋後，將厚度0.17~0.23mm的鋼基材（ 鋼板）脫脂及酸洗之後，使用瓦特浴施以Ni電鍍，藉退火 形成Ni擴散層後，接著，使用電鍍浴施以Sn電鍍，隨後 進行熔融熔錫處理，製作具有Sn-Ni合金層的Sn電鍍鋼 板。 島狀Sn形成狀況以光學顯微鏡觀察表面，可確認在 實施例7、8整體形成有島。 <化學轉化處理膜形成法> 以上述的處理賦予表面處理層之後，藉以下的處理法 賦予化學轉化薄膜。 (A法）將上述鋼板浸漬在溶解氟化Zr4 000質量ppm 、磷酸300質量ppm、酣酸樹脂0或700質量ppm、硝酸
S -18- 201224206 銨10000質量ppm的處理液中，形成Zr化合物-酚醛樹脂 薄膜。 (8法）在溶解氟化Zrl500質量ppm、磷酸400質量 ppm、酚醛樹脂〇或5〇〇質量ppm、硝酸銨5000質量ppm 的處理液中，浸漬、陰極電解上述鋼板賦予Zr化合物·酣 醛樹脂薄膜。將陰極電解處理的電流密度（A/dm2)與時間（ 秒）顯示於表1。「_」是表示未處理或未能檢測出。 (C法）在溶解氟化Zr鉀1500〜4300質量ppm、磷酸 300~1500質量ppm、硝酸銨1000〜7000質量ppm的處理 液中’浸漬或陰極電解上述鋼板賦予具有Zr化合物的化 學轉化處理膜（實施例）。將陰極電解處理的電流密度 (A/dm2)與時間（秒）顯示於表1。 <羥基酸處理層的賦予> 在所形成的化學轉化處理膜上，將表1顯示經基酸之 表1的濃度的水溶液使用輥塗機予以塗層。或浸漬後進行 滾軋。 <清洗處理> 藉上述處理賦予羥基酸處理層之後，以下述步驟乾燥 進行清洗，控制薄膜中的F量，並隨後乾燥》 (W1法）以70°C乾燥，並浸漬在80°C的水中，以40 °C乾燥。 (W2法）以40°C乾燥，並浸漬在85°C的水中，以70 -19- 201224206 °c乾燥。 (W3法）以30°C乾燥，並浸漬在80°C的水中，以40 °C乾燥。 (W4法）以70°C乾燥，並浸漬在80°C的水中，以70 °C乾燥。 再者，本實施例中，表面處理層中的金屬Ni量及金 屬S η量是藉螢光x射線法來測定，使用檢量線予以特定 。又，Zr化合物薄膜中含有的金屬Zr量、P量、F量是 以螢光X射線分析等的定量分析法來測定。羥基酸處理 層中含有的C量是使用TOC (總有機碳分析儀），藉減去存 在鋼板中的C量來測定。 <性能評估〉 針對進行上述處理的試驗材，對以下所示（A)〜（G)的 各項目進行性能評估。針對（A)的高薄膜密接性，實施例 的剝離面積小於1 %，具有優異的薄膜密接性，但是比較 例的剝離面積率皆是在1 %以上’高加工部的薄膜密接性 有問題。對於（B)~(G)的各項目，實施例和比較例同樣地 優異。 (A)藉以下的試驗評估高薄膜密接性。 在試驗材的兩面使用厚度20μιη的延伸倍率3.1x3.1、 厚度25μιη、共聚合比12莫耳％、熔點224°C的間苯二甲 酸共聚合聚對苯二甲酸乙二醇酯薄膜，使得薄膜的雙軸定 -20- 201224206 向度（BO値）形成150的層疊條件，即鋼板的進 40m/min、橡膠輥的夾持長：17mm、壓接後水冷 間：以1 sec層疊，製作實施例、比較例的樹脂 。在此，夾持長爲橡膠輥與鋼板連接部份的搬運 度。將所獲得的樹脂包覆鋼板進行拉深旋轉加工 體，罐胴體的頸部的加工（縮頸加工），將此罐體 °C、30分鐘的蒸餾處理，觀察罐胴體的頸部之 的剝離狀況，從剝離面積率以5階段（◎:剝離丘 、〇：剝離面積率小於1 %、△:剝離面積率 :剝離面積率超過2%〜10%、X :剝離面積率超站 行評估。將結果顯示於表1。 (B)加工性 在試驗材的兩面以200 °C層疊厚度20 μηι的 ，階段性進行拉深加工與旋轉加工的製罐加工， 的瑕疵、突起、剝離而從該等的面積率評估成形 未見有薄膜的瑕疵、突起、剝離® (C)熔接性 使用絲縫焊接機以焊絲速度80m/min的條件 流進行試驗材的焊接，可從獲得充分焊接強度的 値與塵埃及焊接噴濺等焊接缺陷開始明顯的最大 構成適當電流範圍的大小進行綜合性判斷，評估 結果，第二次側的適當電流範圍在1 5 00A以上。 給速度： 爲止的時 包覆鋼板 方向的長 ，製作罐 進行1 2 0 樹脂薄膜 5積率0% -2% > Δ X s 10%)進 PET薄膜 觀察薄膜 的結果， ，變更電 最小電流 電流値所 焊接性的 -21 - 201224206 (D) 第一次塗料密接性 在試驗材塗佈環氧酹醛樹脂，以200°C、30min烘乾 後，以1 mm間隔切割成到達基底鐵深度的圍棋格，以膠 帶剝離，觀察剝離狀況，並從剝離面積率評估的結果，剝 離面積率爲〇 %。 (E) 第二次塗料密接性 在試驗材塗佈環氧酣醒樹脂，以200°C、30min烘乾 後，以1 m m間隔切割成到達基底鐵深度的圍棋格，隨後 ，進行125°C、30min的蒸餾處理，乾燥後以膠帶剝離， 觀察剝離狀況，並從剝離面積率以4階段評估的結果，剝 離面積率爲0%。 (F) 塗膜下抗蝕性 在試驗材塗佈環氧酚醛樹脂，以20(TC、30min烘乾 後，進行切入到達基底鐵深度的交叉切割，並在1.5質量 %檸檬酸-1.5質量％食鹽混合液所成的試驗液，進行45°C 、72小時浸漬，清洗、乾燥後，進行'帶剝離，觀察交叉 切割部的塗膜下腐蝕狀況與平板部的腐蝕狀況，從塗膜下 腐蝕的寬度及平板部的腐蝕面積率的兩評估，評估的結果 ，塗膜下腐蝕寬度小於0.2mm且平板部腐蝕面積率爲〇% (G)蒸餾抗鏽性
S -22- 201224206 將試驗材以125°C、30min進行蒸餾處理，觀察鏽的 產生狀況，從鏽產生面積率評估的結果，鏽產生面積率爲 0%。 -23- 201224206 ί 高薄膜 密接性 I_ <1 <1 X < X < X 0 ◎ ◎ 〇 〇 ◎ ◎ 〇 〇 乾燥· 水洗 1 1 1 1 1 1 eg 寸 CM r~ CO 寸 CO 4ς 棚 1 1 1 1 1 1 |1 装e |i 髮S 水溶液 浸漬 |i 装垢· 水溶液| 浸漬! 装拒· |1 幽 mil 脚 魆 m 種類•濃 度 1 1 1 1 1 1 乙醇酸 1-1g/l 乙醇酸 7：3g/l 乙醇酸 0. 47 κ/ 1 乙醇酸 乙醇酸 15.8^/ I K)〇 o o 糊 勘 c附著 量 (mg/m 2) 1 1 1 1 1 1 CO LO evi LO Osl o .oo o 鋰 m m 窗 鎰 箨 έ m ΓΤΜΐ Ρ η 截 齔 υ Μ-ξ. 趙Sg枷 麄越銮W«T CM m CM LO C\i m I I I 1 I I 1 I P附著 量 (mg/m CO r» OO C\J o OO oo o oo o F附著量 (mg/m 2) 10.01以下1 10.01以下1 s 〇 S CD 10.01以下1 g o 0.01以下 0.01以下 0.01以下 g o 0.01以下 0.01以下 0.01以下 0.01以下 ^l^ScT CM 对 CNJ 寸 LO 寸 CN 对 o ΙΟ CO oo CSJ o exj 清洗處 理法 I P LT5 GO P ID 〇〇 o° o o° o P o P 导 P LO OO P to 〇〇 P LO OO P s o° § 〇υ CO oo P LO P g 電解時 間 (sec) s 1 CSi 1 Osl 1 1 I CM o 1 Osl CsJ 5 CNJ d 電流密 度2 (A/dm2 ) 1 CsJ 1 CSI 1 1 I CM l〇 CO 1 s g CO lO »剧链 < ffl < CD < < < 〇 o < ffl o o ◦ _ mil _ Hi IS m Ni量 (mg/m 2) T— 1 g I s 对 s I in s § C\i g s Sn量 (mg/m 2) S 0¾ OO 〇〇 s σ> oo OO 7800 1 s σ> oo 00 7800 S r-· r— I o o o 2800 f^ril 卿 蜮班 m LO CO cvj in CO CO CM L〇 to CO 編號 I cvj CO LD to C\J CO 寸 LD CO 卜 00 比較例 實施例 s • 24-

Claims (1)

  1. 201224206 七、申請專利範圍： 1·—種容器用鋼板，其特徵爲，具有：在含Zr離子 、F離子的溶液中，浸漬或電解處理鋼板所形成的附著量 爲金屬Zr量0.1~100mg/m2、F量O.lmg/m2以下的化學轉 化處理膜，及在該化學轉化處理膜上，附著量爲C量 0.05〜50mg/m2的羥基酸處理層。 2.如申請專利範圍第1項記載的容器用鋼板，其中， 上述溶液中，進一步含磷酸離子，上述化學轉化處理膜的 附著量，進一步含P量爲0.1〜50mg/m2。 3 ·如申請專利範圍第1項或第2項記載的容器用鋼板 ，其中，上述羥基酸是從檸檬酸、酒石酸、乙醇酸、乳酸 、甘油酸及扁桃酸中所選擇的至少一種。 4.如申請專利範圍第1項至第3項中任一項記載的容 器用鋼板，其中，上述鋼板在至少單面上，具有含Ni量 5〜1 000mg/m2或Sn量1 00〜1 5 00 0mg/m2之表面處理層的表 面處理鋼板β 5 .如申請專利範圍第1項至第4項中任一項記載的容 器用鋼板，其中，上述鋼板爲表面處理鋼板，具有：含Ni 量5〜150mg/m2，Ni電鍍或Fe-Ni合金電鍍相的基底Ni層 ，及在上述基底Ni層上施以30 0〜3000mg/m2的Sn電鍍， 藉熔融熔錫處理使上述基底Ni層的一部份或全部與上述 Sn電鍍層的一部份合金化，而由上述Sn電鍍層之未加以 合金化的剩餘部所形成的島狀Sn電鍍層。 6.—種容器用鋼板之製造方法，係申請專利範圍第 -25- 201224206 1〜5項中任一項記載的容器用鋼板之製造方法，其特徵爲 在含Zr離子、F離子的溶液中，浸漬或電解處理鋼板 ， 在鋼板上形成附著量爲金屬Zr量0.1〜i〇〇mg/m2, f 量0.1 mg/m2以下的化學轉化處理膜，並將具有該化學轉 化處理膜的鋼板浸漬在含羥基酸的水溶液中，或在該化學 轉化處理膜上塗抹含羥基酸的水溶液，使其乾燥。 7.如申請專利範圍第6項記載的容器用鋼板之製造方 法，其中，上述乾燥步驟的溫度爲70°C以上。 8 .如申請專利範圍第6項或第7項記載的容器用鋼板 之製造方法，其中，在上述乾燥步驟之後，以80°C以上溫 度的水清洗，並進一步乾燥。 -26- S 201224206 四、指定代表圖： (一） 本案指定代表圖為：無 (二） 本代表圖之元件符號簡單說明：無 201224206 五 本案若有化學式時，請揭示最能顯示發明特徵的化學 式：無 -4- S
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