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TWI541381B - 容器用鋼板之製造方法 - Google Patents

容器用鋼板之製造方法 Download PDF

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Publication number
TWI541381B
TWI541381B TW100133002A TW100133002A TWI541381B TW I541381 B TWI541381 B TW I541381B TW 100133002 A TW100133002 A TW 100133002A TW 100133002 A TW100133002 A TW 100133002A TW I541381 B TWI541381 B TW I541381B
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Taiwan
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steel sheet
treatment
amount
layer
film
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TW100133002A
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TW201224205A (en
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鈴木威
中村紀彥
宮本友佳
飛山洋一
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Ｊｆｅ鋼鐵股份有限公司
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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/48—After-treatment of electroplated surfaces
    • C25D5/50—After-treatment of electroplated surfaces by heat-treatment
    • C25D5/505—After-treatment of electroplated surfaces by heat-treatment of electroplated tin coatings, e.g. by melting
    • 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 non-planar shape
    • 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
    • B32B15/01—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
    • B32B15/01—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
    • B32B15/015—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 the said other metal being copper or nickel or an alloy thereof
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • 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
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/02—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
    • C21D8/0278—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips involving a particular surface treatment
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    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/08—Ferrous alloys, e.g. steel alloys containing nickel
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    • C23C10/00—Solid state diffusion of only metal elements or silicon into metallic material surfaces
    • C23C10/28—Solid state diffusion of only metal elements or silicon into metallic material surfaces using solids, e.g. powders, pastes
    • 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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    • C23C22/00—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
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    • 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
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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
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    • 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
    • C23C22/361—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 containing titanium, zirconium or hafnium compounds
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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
    • C23C22/73—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 characterised by the process
    • 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
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    • C23C28/32—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer
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Description

容器用鋼板之製造方法
本發明是關於容器用鋼板之製造方法。
以往，在所有的罐種類中，皆對於罐所使用的鋼板(容器用鋼板)進行塗層，但是，近年來，從地球環保的觀點來看，著重於以層疊薄膜來取代塗層的技術而急速地擴展。
但是，以往，在層壓膜的基礎所使用的鋼板形成有鉻酸鹽轉化膜，但是，近年來開始呼籲鉛及鎘等有害物質的使用限制及對於製造工廠的勞動環境的關懷，而要求不使用鉻酸鹽轉化膜。
並在飲料容器市場中，罐在於成本與品質的點上，暴露在與PET瓶、瓶、紙袋等容器的競爭，對於層疊容器用鋼板，也要求具更優異的製罐加工性(尤其是薄膜密接性、加工薄膜密接性、抗蝕性等)。
滿足以上要求有例如專利文獻1中，『在含Zr離子、F離子、銨離子、硝酸離子的溶液中，具有藉浸漬或電解處理的進行形成在鋼板上的Zr化合物處理膜，上述Zr化合物處理膜的附著量是金屬Zr量為1~100mg/m2、F量為0.1mg/m2以下為特徵的容器用鋼板。』所揭示([申請專利範圍第1項])。
[先前技術文獻]
[專利文獻]
[專利文獻1]日本特開2010-13728號公報
如上述，近年來，在飲料容器市場品質競爭的激烈化，對於層疊容器用鋼板，也尋求更為優異的薄膜密接性。尤其是將罐縮頸加工後的頸部份的薄膜，由於一般較為容易剝離，因此期待即使在嚴苛的條件下該等部份也不致發生剝離的容器用鋼板。
本發明人利用專利文獻1所揭示的容器用鋼板，針對縮頸部份相關的薄膜密接性(以下，又稱「高薄膜密接性」)進行了研討，得知並未到達現今所要求的水準而有改良的必要。
因此，本發明係以提供可獲得具優異的高薄膜密封性之容器用鋼板的容器用鋼板之製造方法為目的。
本案發明人，為解決上述課題努力加以研討的結果，發現在鋼板上形成預定的化學轉化處理膜之後，以溫度80℃以上的水清洗進行乾燥，藉此獲得高薄膜密封性優異的容器用鋼板而完成本發明。
亦即，本發明提供以下的(1)~(6)。
(1)一種容器用鋼板之製造方法，係於鋼板上，具有金屬Zr量1~100mg/m2、F量0.1mg/m2以下的化學轉化處理膜的容器用鋼板之製造方法，藉著含Zr離子、F離子之處理液中的浸漬處理或使用該處理液的電解處理在上述鋼板上形成上述化學轉化處理膜，接著，將形成有上述化學轉化處理膜的上述鋼板以溫度80℃以上的水清洗進行乾燥。
(2)如上述(1)項記載的容器用鋼板之製造方法，上述乾燥的溫度為70℃以上。
(3)如上述(1)或(2)記載的容器用鋼板之製造方法，上述處理液，進一步含磷酸離子，上述化學轉化處理膜中的P量為0.1~50mg/m2。
(4)如上述(3)記載的容器用鋼板之製造方法，上述處理液，進一步含酚醛樹脂，上述化學轉化處理膜中的C量為0.1~50mg/m2。
(5)如上述(1)~(4)的其中之一記載的容器用鋼板之製造方法，上述鋼板至少在單面具有含金屬Ni量10~1000mg/m2的Ni或金屬Sn量100~15000mg/m2的Sn的表面處理層。
(6)如上述(1)~(4)的其中之一記載的容器用鋼板之製造方法，上述鋼板是在其表面施以Ni電鍍或Fe-Ni合金電鍍形成基底Ni層，並在上述基底Ni層上施以Sn電鍍，藉熔融熔錫處理使得該Sn電鍍的一部份與上述基底Ni層的一部份或全部合金化形成含島狀Sn的Sn電鍍層，上述基底Ni層是含金屬Ni量5~150 mg/m2的Ni，上述Sn電鍍層是含金屬Sn量300~3000mg/m2的Sn。
根據本發明，可提供獲得高薄膜密接性優異的容器鋼板的容器用鋼板之製造方法。
本發明的容器用鋼板之製造方法是在鋼板上，具有金屬Zr量1~100mg/m2、F量0.1mg/m2以下的化學轉化處理膜的容器用鋼板之製造方法，藉著含Zr離子、F離子、銨離子、硝酸離子之處理液中的浸漬處理或使用該處理液的電解處理在上述鋼板上形成上述化學轉化處理膜，接著，將形成有上述化學轉化處理膜的上述鋼板以溫度80℃以上的水清洗進行乾燥的容器用鋼板之製造方法。
以下，針對本發明容器用鋼板之製造方法詳細說明。
＜鋼板＞
本發明所使用的鋼板尤其不加以限定，通常，可使用作為容器材料所使用的鋼板原板。並且，該鋼板原板的的製造方法、材質等有不加以特別限制，可使用從通常的鋼片製造步驟經熱軋、酸洗、冷軋、退火、冷精軋等的各步驟製造之物。
本發明所使用的鋼板也可以在至少單面具有含鎳(Ni)及/或含錫(Sn)的表面處理層。
上述的表面處理層為Ni電鍍層、Sn電鍍層、Sn-Ni合金電鍍層等。
Ni對於塗料密接性、薄膜密接性、抗蝕性、熔接性等可發揮其效果。此時，表面處理層中，金屬Ni量從為了使該等的特性更為優異的理由及經濟性的觀點，以10~1000mg/m2為佳。
Sn對於加工性、熔接性、抗蝕性等可發揮其效果。此時，表面處理層中，金屬Sn量從為了使該等的特性更為優異的理由及經濟性的觀點，以100~15000mg/m2為佳，使熔接性更為優異的理由是以200~15000mg/m2為佳，使加工性更為優異的理由則是以1000~15000mg/m2更佳。
形成表面處理層(電鍍層)的方法尤其不加以限定，例如可使用電鍍法、浸漬電鍍法、真空蒸鍍法、濺鍍法等習知的方法，且為了形成擴散層也可以組合加熱處理。
Ni電鍍層除了施以金屬鎳所形成的層之外，也可施以鐵(Fe)-鎳(Ni)合金電鍍所形成的Fe-Ni合金電鍍層。
Sn電鍍層雖是藉金屬Sn施以電鍍(Sn電鍍)所形成，但是本發明的「Sn電鍍」是在金屬Sn內含混入有不可逆雜質的電鍍層及在金屬Sn添加微量元素的電鍍層。
又，本發明中，也可形成含島狀Sn的Sn電鍍層。此時，在鋼板的表面施以Ni電鍍或Fe-Ni合金電鍍以形成基底Ni層，在基底Ni層上施以Sn電鍍，藉熔融熔錫處理使得該Sn電鍍的一部份與上述基底Ni層的一部份或全部合金化形成含島狀Sn的Sn電鍍層。
藉熔融熔錫處理(逆流處理)，使Sn熔解而與鋼板或基底Ni層合金化，形成Sn-Fe合金層或Sn-Fe-Ni合金層，提升合金層的抗蝕性，並形成島狀的Sn合金。島狀的Sn合金可以適當控制熔融熔錫處理形成。
Ni為高抗蝕金屬，可提升藉熔融熔錫處理所形成的含Fe及Sn金屬層的抗蝕性。
基底Ni層中的金屬Ni量從抗蝕性的觀點及經濟性的觀點，以5~150mg/m2為佳。
作為基底Ni層在施以加熱處理形成擴散層的場合，也可在加熱處理的前後或與加熱處理同時，進行氮化處理。
Sn的優異抗蝕性是從金屬Sn量為300mg/m2以上顯著地提升，Sn的含量越多，也可增加抗蝕性提升的程度。因此，含島狀Sn的Sn電鍍層的金屬Sn量是以300mg/m2以上為佳。抗蝕性提升效果一旦金屬Sn量超過3000mg/m2時即為飽和，從經濟性的觀點，Sn含量是以3000mg/m2以下為佳。
又，電阻低的Sn柔軟，熔接時在電極間藉著使Sn加壓而擴展，可確保穩定的通電區域，尤其可發揮優異的熔接性。該優異的熔接性只要金屬量Sn在100mg/m2以上即可發揮。又，顯示上述優異抗蝕性之金屬Sn量的範圍中，該熔接性的提升效果並不致於飽和。因此，為確保優異的抗蝕性極熔接性，以金屬Sn量為300mg/m2以上3000mg/m2以下為佳。
再者，表面處理層中的金屬Ni量或金屬Sn量，例如可藉螢光X射線法來測定。此時，使用金屬Ni量為已知的Ni附著量樣本，預先特定金屬Ni量的相關測量線，利用該測量線相對地特定金屬Ni量。金屬Sn量的場合也相同，使用金屬Sn量為已知的Sn附著量樣本，預先特定金屬Sn量的相關測量線，利用該測量線相對地特定金屬Sn量。
＜化學轉化處理膜＞
化學轉化處理膜為形成在上述鋼板的處理膜，金屬Zr量1~100mg/m2、F量0.1mg/m2以下的處理膜。
形成化學轉化處理膜的方法，可舉例如：藉著將鋼板浸漬在熔解Zr離子、F離子後之處理液(酸性溶液)的浸漬處理進行的方法；藉著在含Zr離子、F離子的處理液中之陰極電解處理進行的方法等，從可獲得均一處理膜的理由，以藉陰極電解處理進行的方法為佳。
尤其在陰極電解處理中，以硝酸離子與銨離子共存於處理液中為佳。藉此，可以數秒至數十秒程度的短時間處理，並可形成抗蝕性與密接性之提升效果優異的化學轉化處理膜。
又，處理液中也可含有磷酸離子。
再者，進行陰極電解處理的場合，陰極電解處理的浴溫從處理膜的形成效率、成本、所形成處理膜組織的均一性等的觀點，以10~40℃為佳(低溫陰極電解處理)。又，陰極電解處理的電解電流密度從處理膜附著量的降低抑制、穩定處理膜的形成、處理時間、處理膜特性的降低抑制等的觀點，以0.05~50A/dm2為佳。另外，陰極電解處理的通電時間從處理膜附著量的降低抑制、穩定處理膜的形成、處理時間、處理膜特性的降低抑制等的觀點，則以0.01~5秒為佳。
化學轉化處理膜含有Zr化合物。在此，Zr化合物的功能為抗蝕性及密接性的確保。Zr化合物則可考慮Zr氫氧化物及Zr磷氧化物，該等Zr化合物具有優異的抗蝕性及密接性。此外，「Zr氫氧化物」是意味著Zr氧化物與Zr氫氧化物混合的狀態。
化學轉化處理膜中的金屬Zr量在1mg/m2以上時，實用上，可確保無問題的抗蝕性與密接性。又，金屬Zr量一旦超過100mg/m2時，隨著化學轉化處理膜密接性的劣化的同時使電阻上升而使得溶接性劣化。因此，化學轉化處理膜中的金屬Zr量為1~100mg/m2，並以1~20mg/m2為佳，最好是1~10mg/m2。
又，Zr磷氧化物增加時可發揮更具優異之抗蝕性與密接性，但可明確認知其效果是在P量為0.1mg/m2以上的場合。又，P量超過50mg/m2時隨著密接性劣化的同時使電阻上升而使得溶接性劣化。因此化學轉化處理膜中的P量為0.1~50mg/m2，並以0.1~20mg/m2為佳，最好是0.1~10mg/m2。
F包含於處理液中，所以和Zr化合物一起進入處理膜中。處理膜中的F雖然對於塗料或薄膜通常的密接性不會有影響，但會造成蒸餾處理等高溫殺菌處理時的密接性與抗鏽性或者塗膜下腐蝕性劣化的原因。其理由可能是處理膜中的F溶出於水蒸氣或腐蝕液，使得與有機處理膜的結合分解，或造成基底鋼板腐蝕的原因。
化學轉化處理膜的F量一旦超過0.1mg/m2時，由於開始使得該等的諸特性明顯劣化，所以在0.1mg/m2。
為了設化學轉化處理膜的F量在0.1mg/m2以下，在形成化學轉化處理膜之後，藉溫水中的浸漬處理或噴灑處理進行清洗處理即可。此時，可藉著高的處理溫度或長的處理時間可減少F量。
例如，為了設化學轉化處理膜中的F量為0.1mg/m2以下，以40℃以上的溫水進行0.5秒以上的浸漬處理或噴灑處理即可。
化學轉化處理膜中的金屬Zr量、P量、F量，例如可藉螢光X射線分析等的定量分析來測定。
在處理液中的銨離子的濃度為100~10000ppm左右，硝酸離子的濃度為1000~20000ppm左右的範圍，對應生產設備與生產速度(能力)適當調整即可。
又，處理液中也可含有酚醛樹脂。酚醛樹脂成分可舉例如N,N-二乙醇胺變性後的水溶性酚醛樹脂。
使用含酚醛樹脂的處理液，賦予Zr化合物與酚醛樹脂的複合處理膜。酚醛樹脂本身為有機物，所以可使層疊膜形成良好的密接性。
此時，化學轉化處理膜的C量小於0.1mg/m2時，不能確保實用位準的密接性。又，C量超過50mg/m2時，電阻上升使得溶接性劣化。因此，化學轉化處理膜中的C量是以0.1~50mg/m2為佳，並以0.1~10mg/m2更佳，最好是0.1~8mg/m2。
再者，化學轉化處理膜中的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。
＜清洗＞
本發明是在形成化學轉化處理膜之後，將形成化學轉化處理膜的鋼板，以溫度80℃以上，最好是溫度90℃以上的水清洗，隨後進行乾燥。藉以上的清洗所獲得的容器用鋼板可使化學轉化處理膜的表面適當地粗面化，並可獲得良好的高薄膜密接性。
又，藉進行上述的清洗，也可見除去存在於化學轉化處理膜中的F量並減少F量等點的效果。
此時，清洗的方法尤其不加以限於，如可舉例，將形成有化學轉化處理膜的鋼板浸漬在水中的方法，或使用噴灑等將水塗佈於形成有化學轉化處理膜的鋼板的方法等。
並且，浸漬的場合，浸漬時間雖不加以限定，但以1秒以上為佳。
又，乾燥的溫度雖不加以限定，但以70℃以上為佳。
[實施例]
以下，雖舉實施例具體說明本發明，但本發明不僅限於此。
＜表面處理層＞
使用以下的處理法(1-0)~(1-7)的方法，在板厚0.17~0.23mm的鋼板上形成表面處理層。
(1-0)冷軋後，製作對退火、調壓後的原板施以脫脂、酸洗的鋼板。
(1-1)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。
(1-2)冷軋後，將退火、調壓後的原板脫脂、酸洗後，使用瓦特浴施以Ni電鍍，製作Ni電鍍鋼板。
(1-3)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。
(1-4)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，製作Sn電鍍鋼板。
(1-5)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，隨後進行熔融熔錫處理(逆流處理)，製作具有Sn合金層的Sn電鍍鋼板。
(1-6)冷軋後，在原板脫脂、酸洗後，使用瓦特浴施以Ni電鍍，在退火時形成Ni擴散層，並在脫脂、酸洗後，使用電鍍浴施以Sn電鍍，並隨後進行熔融熔錫處理，製作具有Sn合金層的Ni、Sn電鍍鋼板。
(1-7)冷軋後，將退火、調壓後的原板脫脂、酸洗，使用硫酸-鹽酸浴施以F2-Ni合金電鍍，接著，使用電鍍浴施以Sn電鍍，並隨後進行熔融熔錫處理(逆流處理)，製作具有Sn合金層的Ni、Sn電鍍鋼板。
此外，進行(1-6)及(1-7)的處理的場合，以光學顯微鏡觀察表面，評估島狀Sn狀況時，可確認出整體形成有島狀。
＜化學轉化處理膜＞
藉上述的處理形成表面處理層之後，藉以下的處理法(2-1)~(2-3)形成化學轉化處理膜。
(2-1)使K2ZrF6(4.3g/L)熔解添加硝酸銨，將上述鋼板浸漬在PH調整為2.65的處理液，在浴溫30℃，以第1表顯示的條件陰極電解形成化學轉化處理膜。
(2-2)使K2ZrF6(4.3g/L)與磷酸(1.2g/L)熔解添加硝酸銨，將上述鋼板浸漬在PH調整為2.65的處理液，在浴溫30℃，以第1表顯示的條件陰極電解形成化學轉化處理膜。
(2-3)使K2ZrF6(4.3g/L)與磷酸(1.4g/L)與酚醛樹脂(0.7g/L)熔解添加磷酸，將上述鋼板浸漬在PH調整為2.65的處理液，在浴溫30℃，以第1表顯示的條件陰極電解形成化學轉化處理膜。
此外，酚醛樹脂是使用上述N,N-二乙醇胺變性後的水溶性酚醛樹脂(重量平均分子量：5000)。
＜清洗＞
藉上述的處理形成化學轉化處理膜之後，藉以下的處理法(3-1)~(3-3)進行清洗。
(3-1)在75℃的水中浸漬2秒鐘之後，以75℃乾燥。
(3-2)在80℃的水中浸漬2秒鐘之後，以75℃乾燥。
(3-3)在95℃的水中浸漬2秒鐘之後，以75℃乾燥。
再者，其中之一的實施例及比較例中，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，使用測量線予以特定。又，化學轉化處理膜中含有的金屬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。且化學轉化處理膜中含有的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，進行高薄膜密接性的評估。
首先，在實施例及比較例的各試驗材的兩面，將厚度20μm的PET薄膜以20℃層疊之後，進行拉深旋轉加工製作罐體，對製作的罐體施以縮頸加工形成縮頸部。並將該罐體以120℃進行30分鐘的蒸餾處理，評估縮頸部的薄膜的剝離狀況。
具體評估，完全無剝離的狀況為「◎」，產生實用上沒有問題程度的極些微剝離的狀況為「○」，部份產生剝離實用上有問題的狀況為「△」，而大部份產生剝離的狀況為「×」。將結果顯示於第1表。
從第1表顯示的結果，在形成化學轉化膜之後以溫度75℃的水進行清洗的比較例1~10可得知高薄膜密接性皆為不良。
相對於此，可得知在形成化學轉化膜之後以溫度80℃的水進行清洗的實施例1~13皆具有高薄膜密接性。
此時，具有表面處理層的實施例2~13較未具有表面處理層的實施例1具有優異的高薄膜密皆性。
並將實施例1與實施例2對比時，可得知以溫度90℃的水進行清洗的實施例2較以溫度80℃的水進行清洗的實施例1更具有優異的高薄膜密接性。對此，可得知實施例10與實施例11，及實施例12與實施例13也有同樣的傾向。

Claims (4)

  1. 一種容器用鋼板之製造方法，係於鋼板上，具有金屬Zr量1~100mg/m2、F量0.1mg/m2以下的化學轉化處理膜，其特徵為：藉著含Zr離子、F離子之處理液中的浸漬處理或使用該處理液的電解處理在上述鋼板上形成上述化學轉化處理膜，接著，將形成有上述化學轉化處理膜的上述鋼板以溫度90℃以上的水清洗進行乾燥，上述鋼板係下述(i)或(ii)的鋼板，(i)上述鋼板至少在單面具有含金屬Ni量10~1000mg/m2的Ni或金屬Sn量100~15000mg/m2的Sn的表面處理層(ii)上述鋼板是在其表面施以Ni電鍍或Fe-Ni合金電鍍形成基底Ni層，並在上述基底Ni層上施以Sn電鍍，藉熔融熔錫處理使得該Sn電鍍的一部份與上述基底Ni層的一部份或全部合金化形成含島狀Sn的Sn電鍍層，上述基底Ni層是含金屬Ni量5~150mg/m2的Ni，上述Sn電鍍層是含金屬Sn量300~3000mg/m2的Sn。
  2. 如申請專利範圍第1項記載的容器用鋼板之製造方法，其中，上述乾燥的溫度為70℃以上。
  3. 如申請專利範圍第1項或第2項記載的容器用鋼板之製造方法，其中，上述處理液，進一步含磷酸離子，上述化學轉化處理膜中的P量為0.1~50mg/m2。
  4. 如申請專利範圍第3項記載的容器用鋼板之製造方法，其中，上述處理液，進一步含酚醛樹脂， 上述化學轉化處理膜中的C量為0.1~50mg/m2。
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