TWI490370B - 容器用鋼板及其製造方法 - Google Patents

容器用鋼板及其製造方法 Download PDF

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Publication number
TWI490370B
TWI490370B TW100133007A TW100133007A TWI490370B TW I490370 B TWI490370 B TW I490370B TW 100133007 A TW100133007 A TW 100133007A TW 100133007 A TW100133007 A TW 100133007A TW I490370 B TWI490370 B TW I490370B
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Taiwan
Prior art keywords
steel sheet
film
amount
layer
chemical conversion
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TW100133007A
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English (en)
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TW201224206A (en
Inventor
Takeshi Suzuki
Norihiko Nakamura
Yuka Miyamoto
Yoichi Tobiyama
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Jfe Steel Corp
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Publication of TW201224206A publication Critical patent/TW201224206A/zh
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    • C—CHEMISTRY; METALLURGY
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    • 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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    • B32B1/00—Layered products having a non-planar shape
    • B32B1/08—Tubular products
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    • 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
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    • B32B15/18—Layered products comprising a layer of metal comprising iron or steel
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Description

容器用鋼板及其製造方法
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。
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。
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。作為不使用鉻的無鍍錫薄鋼板的代替材有例如專利文獻1所揭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、O、F為主成份，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，為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地密接，尤其是作為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，在內容物填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
本發明進一步以提供高薄膜密接性優異的容器用鋼板為目的。
本發明人，為達成上述目的加以努力研究的結果，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。
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為金屬Zr量0.1~100mg/m2 、F量0.1mg/m2 以下的化學轉化處理膜，及在該化學轉化處理膜上，附著量為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，進一步為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5~1000mg/m2 或Sn量100~15000mg/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，上述鋼板為具有含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300~3000mg/m2 的Sn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法，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為金屬Zr量0.1~100mg/m2 ，F量0.1mg/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為70℃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℃以上溫度的水清洗，並加以乾燥。
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。
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，使用作為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。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100~15000mg/m2 為佳。
Sn可發揮優異的加工性、熔接性、抗蝕性，發現此一效果是金屬Sn在100mg/m2 以上為佳。為確保充分的熔接性是以200mg/m2 以上，為確保充分的加工性則是賦予1000mg/m2 以上為佳。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15000mg/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15000mg/m2 以下為佳。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 以上為佳。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1000mg/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10mg/m2 以上、1000mg/m2 以下為佳。
具體而言，以使用Ni或Sn的電鍍層為佳。從包含在其上所形成的Zr薄膜的化學轉化處理膜之均勻包覆性的點為佳的電鍍層是形成Fe-Sn-Ni合金層，或Fe-Sn合金層的單一層所成的中間層，或在最下層為Fe-Ni合金層，在其上面為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，表面處理鋼板為具有，含Ni為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100~3000mg/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，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。
電鍍層的Sn附著量小於100mg/m2 有抗蝕性劣化的傾向。另一方面，超過3000mg/m2 則電鍍層會變得過厚，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為逆流處理，在Sn電鍍之後，將溫度上升至Sn熔點的232℃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，在工業上極為有利。因此，化學轉化處理膜的賦予是以陰極電解處理為佳，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為佳。
又，陰極電解處理的處理液中的銨離子的濃度在100~10000質量ppm程度，硝酸離子的濃度在1000~20000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為0.05~50A/dm2 ，電解時間為0.01~10秒。
Zr化合物的功能為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1mg/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Zr量1~100mg/m2 。
鋯薄膜的附著量是以金屬鋯量0.1mg/m2 ~9mg/m2 為佳。更佳的是鋯薄膜的附著量是為金屬鋯量1mg/m2 ~8mg/m2 。設鋯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為金屬P量在0.1mg/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 為佳。磷酸薄膜的附著量是以金屬P量0.1mg/m2 ~8mg/m2 為佳，較佳的是磷酸薄膜的附著量為金屬P量1mg/m2 ~6mg/m2 。設磷酸薄膜的附著量在1mg/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0.1mg/m2 時，由於開始使得該等諸特性的劣化明顯化，所以F量在0.1mg/m2 以下為佳。設F量在0.1mg/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F量。因此，為了設薄膜中的F量在0.1mg/m2 以下，以80℃以上的溫水進行浸漬處理或噴灑處理為佳。清洗處理之後乾燥。乾燥溫度不加以限定但以70℃以上為佳。
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為佳。浸漬或塗佈後乾燥。乾燥溫度雖不加以限定但以70℃以上為佳。其理由為可短時間充分地乾燥。
羥基酸為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50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，乾燥的方法為佳。塗佈的方法可使用各種習知的塗佈法。為縮短乾燥時間，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除去為佳。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 為佳。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：0.1~5.0μm)等為佳。另外，也可將熱固性塗料以厚度0.05~2μm的範圍塗佈於表面處理鋼板側或薄膜側，以此作為黏接劑。
另外，也可以酚醛環氧、氨基環氧等的變性環氧塗料、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。
樹脂包覆層的厚度為3~50μm，尤其以設5~40μm的範圍為佳。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T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。
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)為佳。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。
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0.17~0.23mm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。
(處理法2)　冷軋後，使用瓦特浴施以Ni電鍍，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、Sn電鍍鋼板。
(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Zr4000質量ppm、磷酸300質量ppm、酚醛樹脂0或700質量ppm、硝酸銨10000質量ppm的處理液中，形成Zr化合物-酚醛樹脂薄膜。
(B法)　在溶解氟化Zr1500質量ppm、磷酸400質量ppm、酚醛樹脂0或500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-酚醛樹脂薄膜。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顯示羥基酸之表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℃乾燥，並浸漬在80℃的水中，以40℃乾燥。
(W2法)　以40℃乾燥，並浸漬在85℃的水中，以70℃乾燥。
(W3法)　以30℃乾燥，並浸漬在80℃的水中，以40℃乾燥。
(W4法)　以70℃乾燥，並浸漬在80℃的水中，以70℃乾燥。
再者，本實施例中，表面處理層中的金屬Ni量及金屬Sn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20μm的延伸倍率3.1×3.1、厚度25μm、共聚合比12莫耳%、熔點224℃的間苯二甲酸共聚合聚對苯二甲酸乙二醇酯薄膜，使得薄膜的雙軸定向度(BO值)形成150的層疊條件，即鋼板的進給速度：40m/min、橡膠輥的夾持長：17mm、壓接後水冷為止的時間：以1sec層疊，製作實施例、比較例的樹脂包覆鋼板。在此，夾持長為橡膠輥與鋼板連接部份的搬運方向的長度。將所獲得的樹脂包覆鋼板進行拉深旋轉加工，製作罐體，罐胴體的頸部的加工(縮頸加工)，將此罐體進行120℃、30分鐘的蒸餾處理，觀察罐胴體的頸部之樹脂薄膜的剝離狀況，從剝離面積率以5階段(◎：剝離面積率0%、○：剝離面積率小於1%、△：剝離面積率1~2%、△×：剝離面積率超過2%~10%、×：剝離面積率超過10%)進行評估。將結果顯示於表1。
(B)　加工性
在試驗材的兩面以200℃層疊厚度20μm的PET薄膜，階段性進行拉深加工與旋轉加工的製罐加工，觀察薄膜的瑕疵、突起、剝離而從該等的面積率評估成形的結果，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，變更電流進行試驗材的焊接，可從獲得充分焊接強度的最小電流值與塵埃及焊接噴濺等焊接缺陷開始明顯的最大電流值所構成適當電流範圍的大小進行綜合性判斷，評估焊接性的結果，第二次側的適當電流範圍在1500A以上。
(D)　第一次塗料密接性
在試驗材塗佈環氧酚醛樹脂，以200℃、30min烘乾後，以1mm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，剝離面積率為0%。
(E)第二次塗料密接性
在試驗材塗佈環氧酚醛樹脂，以200℃、30min烘乾後，以1mm間隔切割成到達基底鐵深度的圍棋格，隨後，進行125℃、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，剝離面積率為0%。
(F)塗膜下抗蝕性
在試驗材塗佈環氧酚醛樹脂，以200℃、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℃、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為0%。
(G)　蒸餾抗鏽性
將試驗材以125℃、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，鏽產生面積率為0%。

Claims (7)

  1. 一種容器用鋼板，其特徵為，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為金屬Zr量0.1~100mg/m2 、F量0.1mg/m2 以下的化學轉化處理膜，及在該化學轉化處理膜上，附著量為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量為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項或第2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5~1000mg/m2 或Sn量100~15000mg/m2 之表面處理層的表面處理鋼板。
  5. 如申請專利範圍第1項或第2項記載的容器用鋼板，其中，上述鋼板為表面處理鋼板，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300~3000mg/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. 一種容器用鋼板之製造方法，係申請專利範圍第 1~5項中任一項記載的容器用鋼板之製造方法，其特徵為：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為金屬Zr量0.1~100mg/m2 ，F量0.1mg/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，以70℃以上使其乾燥。
  7. 一種容器用鋼板之製造方法，係申請專利範圍第1~5項中任一項記載的容器用鋼板之製造方法，其特徵為：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為金屬Zr量0.1~100mg/m2 ，F量0.1mg/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，然後以80℃以上溫度的水清洗，並進一步乾燥。
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