TWI627289B - 罐用鋼板及其製造方法 - Google Patents

罐用鋼板及其製造方法 Download PDF

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Publication number
TWI627289B
TWI627289B TW105140900A TW105140900A TWI627289B TW I627289 B TWI627289 B TW I627289B TW 105140900 A TW105140900 A TW 105140900A TW 105140900 A TW105140900 A TW 105140900A TW I627289 B TWI627289 B TW I627289B
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Taiwan
Prior art keywords
chromium
steel sheet
electrolytic treatment
layer
cans
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TW105140900A
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TW201726941A (zh
Inventor
中川祐介
鈴木威
須藤幹人
小島克己
馬場雄也
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Ｊｆｅ鋼鐵股份有限公司
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    • 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
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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
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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
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Abstract

本發明提供表面外觀優異之罐用鋼板及其製造方法。上述罐用鋼板係於鋼板表面自上述鋼板側起依序具有金屬鉻層及鉻水合氧化物層，上述金屬鉻層之附著量為65~200mg/m2，上述鉻水合氧化物層之鉻換算之附著量為3~15mg/m2，上述金屬鉻層包含厚度為7nm以上之平板狀金屬鉻層、與具有於上述平板狀金屬鉻層之表面上形成之粒狀突起、上述粒狀突起之最大粒徑為100nm以下且上述粒狀突起之每單位面積之個數密度為10個/μm2以上之粒狀金屬鉻層。

Description

罐用鋼板及其製造方法
本發明關於罐用鋼板及其製造方法。
適用於飲料或食品之容器的罐，由於可長期保存內容物故已於全世界被使用。罐大致分為對金屬板施以拉深、鍛鍊、拉伸、彎曲加工，一體成形罐底部及罐體部後，藉由上蓋繞緊之2片式罐，及將金屬板加工成筒狀，以熔接(wire seam)方式熔接之罐體部與其兩端以蓋繞緊之3片式罐。
以往，作為罐用鋼板，雖廣泛使用鍍錫鋼板(所謂馬口鐵)，但近幾年來，具有金屬鉻層及鉻水合氧化物層之電解鉻酸鹽處理鋼板(以下亦稱為無錫鋼板(TFS))比馬口鐵便宜，且塗料密著性優異，故正擴大適用範圍。
又，基於減少洗淨廢液及CO2之環境對應觀點，作為可省略塗裝步驟及燒烤步驟之替代技術，使用層合有PET(對苯二甲酸乙二酯)等之有機樹脂薄膜之鋼板的罐備受 矚目，於該方面，與有機樹脂薄膜之密著性優異之TFS可預測於往後之應用亦將擴大。
另一方面，由於TFS與馬口鐵相較，熔接性較差，故現狀係在熔接前藉由機械研磨去除絕緣皮膜即表層之鉻水合氧化物層而成為可熔接。
然而，於工業生產中，有研磨後之金屬粉混入內容物之風險，且製罐裝置之清潔等維護負荷增加、因金屬粉而發生火災之風險等之問題亦多。
因此，用以藉無研磨熔接TFS之技術已提案於例如專利文獻1。專利文獻1所示之技術係藉由於前段與後段之陰極電解處理之間實施陽極電解處理，而於金屬鉻層形成多數缺陷部，藉由後段之陰極電解處理，將金屬鉻形成為粒狀突起狀之技術。依據該技術，金屬鉻之粒狀突起於熔接時，藉由破壞表層之熔接阻礙因子即鉻水合氧化物層，而減低接觸電阻，而可改善熔接性。
〔先前技術文獻〕 〔專利文獻〕
[專利文獻1]日本特開昭63-186894號公報
本發明人等針對專利文獻1中具體記載之罐用鋼板進行檢討之結果，有表面外觀劣化之情況。
因此，本發明之目的在於提供表面外觀優異之罐用鋼板及其製造方法。
本發明人等為達成上述目的而積極檢討之結果，發現藉由使金屬鉻之粒狀突起小徑化而使表面外觀良化，因而完成本發明。
亦即，本發明提供以下之[1]~[9]。
[1]一種罐用鋼板，係於鋼板表面自上述鋼板側起依序具有金屬鉻層及鉻水合氧化物層，上述金屬鉻層之附著量為65~200mg/m2，上述鉻水合氧化物層之鉻換算之附著量為3~15mg/m2，上述金屬鉻層包含厚度為7nm以上之平板狀金屬鉻層、與具有於上述平板狀金屬鉻層之表面上形成之粒狀突起、上述粒狀突起之最大粒徑為100nm以下且上述粒狀突起之每單位面積之個數密度為10個/μm2以上之粒狀金屬鉻層。
[2]如上述[1]之罐用鋼板，其中上述粒狀突起之最大粒徑為50nm以下。
[3]如上述[2]之罐用鋼板，其中上述粒狀突起之最大粒徑為30nm以下。
[4]如上述[1]~[3]中任一項之罐用鋼板，其中上述粒狀突起之每單位面積之個數密度為50個/μm2以上。
[5]如上述[4]之罐用鋼板，其中上述粒狀突起之每單位面積之個數密度為100個/μm2以上。
[6]如上述[1]~[5]中任一項之罐用鋼板，其中上述平板狀金屬鉻層之厚度為10nm以上。
[7]一種罐用鋼板之製造方法，其係獲得如上述[1]~[6]中任一項之罐用鋼板者，且使用Cr量為0.5mol/L以上、F量為超過0.10mol/L且除不可避免混入之硫酸以外未添加硫酸之水溶液對鋼板進行前段陰極電解處理，接著，以電量密度為0.1C/dm2以上且未達5.0C/dm2之條件進行陽極電解處理，進而接著進行後段陰極電解處理。
[8]如上述[7]之罐用鋼板之製造方法，其中上述後段陰極電解處理係最終電解處理。
[9]如上述[7]或[8]之罐用鋼板之製造方法，其中上述前段陰極電解處理、上述陽極電解處理及上述後段陰極電解處理中，僅使用一種上述水溶液。
依據本發明，可提供表面外觀優異之罐用鋼板及其製造方法。
[罐用鋼板]
本發明之罐用鋼板係於鋼板表面自上述鋼板側起依序具有金屬鉻層及鉻水合氧化物層，上述金屬鉻層之附著量為50~200mg/m2，上述鉻水合氧化物層之鉻換算之附著量 為3~15mg/m2，上述金屬鉻層包含厚度為7nm以上之平板狀金屬鉻層、與具有於上述平板狀金屬鉻層之表面上形成之粒狀突起、上述粒狀突起之最大粒徑為100nm以下且上述粒狀突起之每單位面積之個數密度為10個/μm2以上之粒狀金屬鉻層。
本發明之罐用鋼板因粒狀金屬鉻層之粒狀突起之最大粒徑為100nm以下，故表面外觀優異。
又，本發明中，附著量為鋼板每單面之附著量。
以下，針對本發明之各構成更詳細說明。
[鋼板]
鋼板種類並未特別限定。通常，可使用作為容器材料使用之鋼板(例如低碳鋼板、極低碳鋼板)。該鋼板之製造方法、材質等並未特別限定。可自通常之鋼片製造步驟後，經過熱壓延、酸洗、冷壓延、燒鈍、調質壓延等之步驟製造。
[金屬鉻層]
本發明之罐用鋼板係於上述鋼板表面具有金屬鉻層。
一般TFS中之金屬鉻的角色在於抑制成為材料之鋼板表面露出且提高耐腐蝕性。金屬鉻量過少時，無法避免鋼板露出，有使耐腐蝕性劣化之情況。
本發明中，基於使罐用鋼板之耐腐蝕性優異之理由，金屬鉻層之附著量為65mg/m2以上，基於耐腐蝕性更優異 之理由，較好為70mg/m2以上，更好為80mg/m2以上。
另一方面，金屬鉻量過多時，成為高熔點之金屬鉻覆蓋鋼板全面，而有熔接時熔接強度降低或塵埃顯著發生、使熔接性劣化之情況。
本發明中，基於罐用鋼板之熔接性優異之理由，金屬鉻層之附著量為200mg/m2以下，基於熔接性更優異之理由，較好為180mg/m2以下，更好為160mg/m2以下。
<附著量之測定方法>
金屬鉻之附著量及後述之鉻水合氧化物層之鉻換算附著量係如下測定。
首先，針對形成有金屬鉻層及鉻水合氧化物層之罐用鋼板，使用螢光X射線裝置，測定鉻量(總鉻量)。其次，將罐用鋼板於90℃之6.5N-NaOH中浸漬10分鐘進行鹼處理後，再次使用螢光X射線裝置，測定鉻量(鹼處理後之鉻量)。將鹼處理後鉻量設為金屬鉻層之附著量。
其次，計算(鹼可溶鉻量)=(總鉻量)-(鹼處理後鉻量)，將鹼可溶鉻量設為鉻水合氧化物層之鉻換算之附著量。
此種金屬鉻層包含平板狀金屬鉻層與具有於平板狀金屬鉻層表面形成之粒狀突起之粒狀金屬鉻層。
其次針對包含金屬鉻層之各層詳細說明。
<平板狀金屬鉻層>
平板狀金屬鉻層主要係被覆鋼板表面擔負提高耐腐蝕性之角色。
且，本發明中之平板狀金屬鉻層必須具有除了確保一般TFS所要求之耐腐蝕性以外，亦須確保於處理時不可避免之罐用鋼板彼此接觸時設於表層之粒狀突起狀金屬鉻不會破壞平板狀金屬鉻層而使鋼板露出般之充分厚度。
本發明人等基於該等觀點，進行罐用鋼板彼此之擦過試驗，調查耐銹性之結果，發現若平板狀金屬鉻層之厚度為7nm以上，則耐銹性優異。亦即，平板狀金屬鉻層之厚度基於罐用鋼板之耐銹性優異之理由而為7nm以上，基於耐銹性更優異之理由，較好為9nm以上，更好為10nm以上。
另一方面，平板狀金屬鉻層之厚度上限並未特別限定，但為例如20nm以下，較好為15nm以下。
(厚度之測定方法)
平板狀金屬鉻層之厚度係如下測定。
首先，以集束離子束(FIB)法製作形成有金屬鉻層及鉻水合氧化物層之罐用鋼板之剖面樣品，以掃描透過電子顯微鏡(TEM)以20000倍觀察。接著藉亮視野像之剖面形狀觀察，注目於僅存在無粒狀突起之平板狀金屬鉻層之部分，藉由能量分散型X射線分光法(EDX)之線分析，自鉻及鐵之強度曲線(橫軸：距離，縱軸：強度)求出平板狀金屬鉻層厚度。此時，更詳細而言，於鉻之強度 曲線中，強度為最大值之20%的點作為最表層，與鐵之強度曲線之交叉點作為與鐵之交界點，將兩點間之距離設為平板狀金屬鉻層之厚度。
又，基於罐用鋼板之耐銹性優異之理由，平板狀金屬鉻層之附著量較好為10mg/m2以上，更好為30mg/m2以上，又更好為40mg/m2以上。
(粒狀金屬鉻層)
粒狀金屬鉻層係具有於上述平板狀金屬鉻層之表面上形成之粒狀突起之層，且主要擔負減低罐用鋼板彼此之接觸電阻並提高熔接性之角色。推測使接觸電阻降低之機制記述於以下。
被覆於金屬鉻層上之鉻水合氧化物層由於係不導體皮膜，故電氣阻抗大於金屬鉻，成為熔接之阻礙因子。於金屬鉻層之表面形成粒狀突起時，因熔接時之罐用鋼板彼此之接觸時面壓，而使粒狀突起破壞鉻水合氧化物層，處於熔接電流之通電點，接觸電阻大幅降低。
粒狀金屬鉻層之粒狀突起過少時，有熔接時之通電點減少無法使接觸電阻降低而使熔接性劣化之情況。
本發明中，基於罐用鋼板之熔接性優異之理由，粒狀突起之每單位面積之個數密度為10個/μm2以上，基於熔接性更優異之理由，較好為15個/μm2以上，更好為20個/μm2以上，再更好為30個/μm2以上，特佳為50個/μm2 以上，最好為100個/μm2以上。
又，粒狀突起之每單位面積之個數密度之上限，若每單位面積之個數密度過高則有對色調造成影響之情況，故基於罐用鋼板之表面外觀更優異之理由，較好為10000個/μm2以下，更好為5000個/μm2以下，又更好為1000個/μm2以下，特佳為800個/μm2以下。
不過，本發明人等發現金屬鉻層之粒狀突起之最大粒徑過大時，對罐用鋼板之色調造成影響，而成為褐色花樣，有表面外觀差之情況。此認為係基於下述等理由：因為粒狀突起吸收短波長側(藍色系)之光，因其反射光衰減，而呈現紅棕色系之顏色；粒狀突起使反射光散射，而減低全體之反射率因此變暗。
因此，本發明中，粒狀金屬鉻層之粒狀突起之最大粒徑為100nm以下。藉此，罐用鋼板之表面外觀優異。此認為係因為粒狀突起小徑化，而抑制短波長側之光之吸收，而抑制反射光之散射之故。
基於使罐用鋼板之表面外觀更優異之理由，粒狀金屬鉻層之粒狀突起之最大粒徑較好為80nm以下，更好為50nm以下，又更好為30nm以下。
又，最大粒徑之下限並未特別限定，較好為例如10nm以上。
(粒狀突起之粒徑及每單位面積之個數密度之測定方法)
粒狀金屬鉻層之粒狀突起之粒徑及每單位面積之個數 密度係如下測定。
首先，於形成有金屬鉻層及鉻水合氧化物層之罐用鋼板表面進行碳蒸鍍，藉由萃取複製法製作觀察用樣品，隨後，以掃描透過電子顯微鏡(TEM)以20000倍拍攝照片，使用圖形軟體(商品名：ImageJ)將拍攝之照片二值化，進行圖像解析，自粒狀突起所佔之面積反推，求出以真圓換算之粒徑及每單位面積之個數密度。且最大粒徑係設為以20000倍於5視野拍攝之觀察視野之最大粒徑，每單位面積之個數密度係設為5視野之平均。
[鉻水合氧化物層]
於鋼板表面，鉻水合氧化物與金屬鉻同時析出，主要擔負提高耐腐蝕性之角色。本發明中，基於確保罐用鋼板之耐腐蝕性之理由，鉻水合氧化物層之鉻換算附著量設為3mg/m2以上。
另一方面，鉻水合氧化物與金屬鉻相較導電率較差，若過量，則熔接時成為過大電阻，引起塵埃或飛濺之發生及伴隨過熔接之吹蝕孔等之各種熔接缺陷，而有罐用鋼板之熔接性差之情況。
因此，本發明中，鉻水合氧化物層之鉻換算之附著量，基於罐用鋼板之熔接性優異之理由，為15mg/m2以下，基於熔接性更優異之理由，較好為13mg/m2以下，更好為10mg/m2以下，又更好為8mg/m2以下。
又，鉻水合氧化物層之鉻換算附著量之測定 方法係如上述。
[罐用鋼板之製造方法]
其次，說明本發明之罐用鋼板之製造方法。
本發明之罐用鋼板之製造方法(以下簡稱為「本發明之製造方法」)係獲得上述本發明之罐用鋼板之罐用鋼板之製造方法，係使用Cr量為0.5mol/L以上、F量為超過0.10mol/L且除不可避免混入之硫酸以外未添加硫酸之水溶液對鋼板進行前段陰極電解處理，接著，以電量密度為0.1C/dm2以上且未達5.0C/dm2之條件進行陽極電解處理，進而接著進行後段陰極電解處理。
一般於含六價鉻化合物之水溶液中之陰極電解處理係於鋼板表面發生還原反應，析出金屬鉻及於其表面對金屬鉻之中間產物即鉻水合氧化物。該鉻水合氧化物藉由斷續進行電解處理，於六價鉻化合物之水溶液中長期浸漬，而不均一地溶解，藉隨後之陰極電解處理形成金屬鉻之粒狀突起。
本發明中，於陰極電解處理之期間進行陽極電解處理，使鋼板全面且多發地溶解金屬鉻，成為隨後之以陰極電解處理形成之金屬鉻之粒狀突起之起點。藉陽極電解處理前進行之陰極電解處理即前段陰極電解處理，析出平板狀金屬鉻層，藉陽極電解處理後進行之陰極電解處理即後段陰極電解處理而析出粒狀金屬鉻層(粒狀突起)。
各析出量可藉各電解處理中之電解條件而控制。
以下針對本發明之製造方法所用之水溶液及各電解處理詳細說明。
[水溶液]
本發明之製造方法所用之水溶液係Cr量為0.5mol/L以上、F量為超過0.10mol/L且除不可避免混入之硫酸以外未添加硫酸之水溶液。
水溶液中之F量對浸漬時之鉻水合氧化物之溶解及陽極電解處理時之金屬鉻之溶解造成影響，對隨後陰極電解處理所析出之金屬鉻之形態亦造成較大影響。同樣效果於硫酸亦可能。然而，效果變過度時，以鉻水合氧化物之不均一溶解為起因而局部形成巨大之粒狀突起，於陽極電解處理之金屬鉻溶解激烈進行，有難以形成微細粒狀突起之情況。因此，本發明中之水溶液中除了不可避免混入之硫酸以外，並未添加硫酸。
又，三氧化鉻等原料由於在工業生產過程不可避免會混入硫酸，故使用該等原料時，會於水溶液中混入不可避免之硫酸。不可避免混入水溶液中之硫酸之混入量較好未達0.001mol/L，更好未達0.0001mol/L。
接著，本發明之水溶液為了可長時間安定且高效率地析出金屬鉻，而將Cr量設為0.5mol/L以上。
此外，本發明之水溶液之F量設為超過0.10mol/L。 藉此，於陽極電解處理時全面均一地發生微細金屬鉻之溶解，獲得於後段陰極電解處理中之微細粒狀突起之發生部位。
又，前段陰極電解處理、陽極電解處理及後段陰極電解處理中，較好僅使用1種水溶液。
<六價鉻化合物>
水溶液較好含有六價鉻化合物。水溶液中所含之六價鉻化合物並未特別限定，但舉例為例如三氧化鉻(CrO3)；重鉻酸鉀(K2Cr2O7)等之重鉻酸鹽；鉻酸鉀(K2CrO4)等之鉻酸鹽；等。
水溶液中之六價鉻化合物之含量以Cr量計，較好為0.5~5.0mol/L，更好為0.5~3.0mol/L。
<含氟化合物>
水溶液較好含有含氟化合物。水溶液中所含之含氟化合物並未特別限定，但舉例為例如氫氟酸(HF)、氟化鉀(KF)、氟化鈉(NaF)、矽氟化氫酸(H2SiF6)及/或其鹽等。作為矽氟化氫酸之鹽舉例為例如矽氟化鈉(Na2SiF6)、矽氟化鉀(K2SiF6)、矽氟化銨((NH4)2SiF6)等。
水溶液中之含氟化合物含量以F量計較好超過0.10mol/L、4.0mol/L以下，更好為0.15~3.0mol/L，又更好0.20~2.0mol/L。
各電解處理中之水溶液液溫較好為20~80℃,更好為40~60℃。
[前段陰極電解處理]
藉陰極電解處理而析出金屬鉻及鉻水合氧化物。
此時，基於成為適當析出量之觀點及基於確保平板狀金屬鉻層之適當厚度之觀點，前段陰極電解處理之電量密度(電流密度與通電時間之乘積)較好為20~50C/dm2，更好為25~45C/dm2。
電流密度(單位：A/dm2)及通電時間(單位：秒)係基於上述電量密度而適當設定。
又，前段陰極電解處理亦可非連續電解處理。亦即前段陰極電解處理亦可於工業生產上分為複數電極電解而不可避免存在無通電浸漬時間之斷續電解處理。斷續電解處理時，總電量密度較好在上述範圍內。
[陽極電解處理]
陽極電解處理係擔負將前段陰極電解處理所析出之金屬鉻溶解，並於後段陰極電解處理中形成金屬鉻之粒狀突起之發生部位之角色。此時，陽極電解處理之溶解過強時，發生部位減少而使粒狀突起之每單位面積之個數密度減少，而進行不均一溶解而於粒狀突起分布產生不均，使平板狀金屬鉻層之厚度減少而低於7nm之情況。
前段陰極電解處理及陽極電解處理所形成之 金屬鉻層主要為平板狀金屬鉻層。為了將平板狀金屬鉻層之厚度設為7nm以上，必須確保前段陰極電解處理及陽極電解處理後之金屬鉻量為50mg/m2以上。
基於以上觀點，陽極電解處理之電量密度(電流密度與通電時間之乘積)較好為0.1C/dm2以上且未達5.0C/dm2。陽極電解處理之電量密度之下限較好超過0.3C/dm2。陽極電解處理之電量密度之上限較好為3.0C/dm2以下，更好為2.0C/dm2以下。
電流密度(單位：A/dm2)及通電時間(單位：秒)係基於上述電量密度而適當設定。
又，陽極電解處理亦可非連續電解處理。亦即陽極電解處理亦可於工業生產上分為複數電極電解而不可避免存在無通電浸漬時間之斷續電解處理。斷續電解處理時，總電量密度較好在上述範圍內。
[後段陰極電解處理]
如上述，藉陰極電解處理，析出金屬鉻及鉻水合氧化物。尤其藉後段陰極電解處理，以上述發生部位為起點，生成金屬鉻之粒狀突起。此時，若電量密度過大，則金屬鉻之粒狀突起急遽成長，而有粒徑變粗大之情況。
基於以上觀點，於後段陰極電解處理中，電量密度較好未達30.0C/dm2，更好為25.0C/dm2以下，又更好7.0C/dm2以下。下限並未特別限制，但較好為1.0C/dm2以上，更好為2.0C/dm2以上。
通電時間(單位：秒)係基於上述電流密度及電量密度而適當設定。
又，後段陰極電解處理亦可非連續電解處理。亦即後段陰極電解處理亦可於工業生產上分為複數電極電解而不可避免存在無通電浸漬時間之斷續電解處理。斷續電解處理時，總電量密度較好在上述範圍內。
後段陰極電解處理較好為最終電解處理。亦即，後段陰極電解處理後，更好不進行另外之電解處理(陰極電解處理或陽極電解處理，尤其是陰極電解處理)。且，作為電解處理，更好僅使用1種水溶液，進行前段陰極電解處理、陽極電解處理及後段陰極電解處理。
藉由將後段陰極電解處理作為最終電解處理，可抑制鉻水合氧化物層之鉻換算附著量過於增加、抑制粒狀金屬鉻層之粒狀突起之最大粒徑過於變大。
不過，後段陰極電解處理為最終電解處理時，於後段陰極電解處理後，以鉻水合氧化物層之量的控制及改質等為目的，亦可進行將鋼板以無電解浸漬於含六價鉻化合物之水溶液中之浸漬處理。即使進行此種浸漬處理，對於平板狀金屬鉻層之厚度、以及粒狀金屬鉻層之粒狀突起之粒徑及個數密度完全不造成影響。
浸漬處理所用之水溶液中所含之六價鉻化合物並未特別限定，但舉例為例如三氧化鉻(CrO3)；重鉻酸鉀(K2Cr2O7)等之重鉻酸鹽；鉻酸鉀(K2CrO4)等之鉻酸鹽；等。
[實施例]
以下列舉實施例具體說明本發明。惟，本發明不限定於此。
[罐用鋼板之製作]
對於以0.22mm之板厚製造之調質度T4CA之鋼板施以通常之脫脂及酸洗，其次，以流動胞藉由泵以相當於100mpm循環下述表1所示之水溶液，使用鉛電極，以下述表2所示條件施以電解處理，製作TFS的罐用鋼板。製作之罐用鋼板經水洗，使用吹風機於室溫乾燥。
更詳細而言，僅比較例2，使用第1液(水溶液E)進行前段陰極電解處理、陽極電解處理及後段陰極電解處理後，使用第2液(水溶液F)進行陰極電解處理。針對其以外之例，僅使用第1液(水溶液A~E)，進行前段陰極電解處理、陽極電解處理及後段陰極電解處理。
[附著量]
針對製作之罐用鋼板，測定金屬鉻層(金屬Cr層)之附著量及鉻水合氧化物層(Cr水合氧化物層)之鉻換算附著量(下述表2中僅記述為「附著量」)。測定方法如上述，結果示於下述表2。
[金屬Cr層構成]
針對製作之罐用鋼板之金屬Cr層，測定平板狀金屬鉻層(平板狀金屬Cr層)之厚度及粒狀金屬鉻層(粒狀金屬Cr層)之粒狀突起之最大粒徑及每單位面積之個數密度。測定方法如上述，結果示於下述表2。
[評價]
針對製作之罐用鋼板進行以下評價。評價結果示於下述表2。
<耐銹性>
自製作之罐用鋼板切出2個樣品，將一樣品(30mm×60mm)固定於摩擦測試器作為評價用樣品，將另一樣品(10mm見方)固定於測試頭上，以1kgf/cm2之面壓，設為擦過速度1往返1秒，以60mm長度進行10衝程。隨後將評價用樣品於氣溫40℃、相對濕度80%之恆溫恆濕庫內經時7天。隨後，自以光學顯微鏡低倍率觀察之照片藉由圖像解析，確認擦過部之生銹面積率，以下述基準進行評價。實用上，若為「◎◎」、「◎」或「○」，則可評價為耐銹性優異者。
◎◎：生銹未達1%
◎：生銹1%以上未達2%
○：生銹2%以上未達5%
△：生銹5%以上未達10%
×：生銹10%以上，或從擦過部以外之生銹
<色調>
針對製作之罐用鋼板，基於舊JIS Z 8730(1980)中規定之圖案式色差測定，測定L值，以下述基準進行評價。實用上，若為「◎◎」、「◎」或「○」，則可評價為表面外觀優異者。
◎◎：L值70以上
◎：L值67以上未達70
○：L值65以上未達67
○~△：L值63以上未達65
△：L值60以上未達63
×：L值未達60
<接觸電阻>
針對製作之罐用鋼板，進行模擬有機樹脂薄膜層合之熱壓著及後加熱之熱處理後，測定接觸電阻。更詳言之，首先，將罐用鋼板之樣品於薄膜層合裝置中，以輥加壓4kg/cm2、供板速度40mpm、輥通過後之板的表面溫度為160℃之方式使板通過，其次，於批式爐中進行後加熱(於到達板溫210℃保持120秒)，重疊熱處理後之樣品。其次將DR型1質量%Cr-Cu電極加工為前端徑為6mm，曲率R40mm，以該電極，夾入重疊之樣品，設為加壓力1kgf/cm2保持15秒後，進行10A通電，測定板-板間之接觸電阻。進行10點測定，將平均值設為接觸電 阻值，以下述基準進行評價。實用上，若為「◎◎」、「◎」或「○」，則可評價為熔接性優異者。
◎◎：接觸電阻為50μΩ以下
◎：接觸電阻超過50μΩ且100μΩ以下
○：接觸電阻超過100μΩ且300μΩ以下
△：接觸電阻超過300μΩ且1000μΩ以下
×：接觸電阻超過1000μΩ
如由上述表2所示之結果所明瞭，可知實施例1~13之罐用鋼板之表面外觀優異。
相對於此，使用水溶液D(NaF：0.10mol/L)之比較例1，粒狀金屬鉻層之粒狀突起之每單位面積之個數最大粒徑為160nm而較大，表面外觀差。
且，使用第1液之電解處理(前段陰極電解處理、陽極電解處理及後段陰極電解處理)後，進而使用第2液進行陰極電解處理之比較例2，例如粒狀金屬鉻層之粒狀突起之最大粒徑為120nm而較大，表面外觀差。
且，比較例3係粒狀金屬鉻層之粒狀突起之最大粒徑為1000nm而較大，表面外觀差。

Claims (9)

  1. 一種罐用鋼板，係於鋼板表面自上述鋼板側起依序具有金屬鉻層及鉻水合氧化物層，前述金屬鉻層之附著量為65~200mg/m2，前述鉻水合氧化物層之鉻換算之附著量為3~15mg/m2，前述金屬鉻層包含厚度為7nm以上之平板狀金屬鉻層、與具有於前述平板狀金屬鉻層之表面上形成之粒狀突起、前述粒狀突起之最大粒徑為100nm以下且前述粒狀突起之每單位面積之個數密度為10個/μm2以上之粒狀金屬鉻層。
  2. 如請求項1之罐用鋼板，其中前述粒狀突起之最大粒徑為50nm以下。
  3. 如請求項2之罐用鋼板，其中前述粒狀突起之最大粒徑為30nm以下。
  4. 如請求項1~3中任一項之罐用鋼板，其中前述粒狀突起之每單位面積之個數密度為50個/μm2以上。
  5. 如請求項4之罐用鋼板，其中前述粒狀突起之每單位面積之個數密度為100個/μm2以上。
  6. 如請求項1~5中任一項之罐用鋼板，其中前述平板狀金屬鉻層之厚度為10nm以上。
  7. 一種罐用鋼板之製造方法，其係獲得如請求項1~6中任一項之罐用鋼板者，且使用Cr量為0.5mol/L以上、F量為超過0.10mol/L且除不可避免混入之硫酸以外未添加硫酸之水溶液對鋼板進行前段陰極電解處理，接著，以電量密度為0.1C/dm2以上且未達5.0C/dm2之條件進行陽極電解處理，進而接著進行後段陰極電解處理。
  8. 如請求項7之罐用鋼板之製造方法，其中前述後段陰極電解處理係最終電解處理。
  9. 如請求項7或8之罐用鋼板之製造方法，其中前述前段陰極電解處理、前述陽極電解處理及前述後段陰極電解處理中，僅使用一種前述水溶液。
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