CN107406988A - 热浸镀锌系钢板 - Google Patents
热浸镀锌系钢板 Download PDFInfo
- Publication number
- CN107406988A CN107406988A CN201680017833.6A CN201680017833A CN107406988A CN 107406988 A CN107406988 A CN 107406988A CN 201680017833 A CN201680017833 A CN 201680017833A CN 107406988 A CN107406988 A CN 107406988A
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- CN
- China
- Prior art keywords
- oxide
- steel plate
- hot dip
- galvanized steel
- dip galvanized
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D1/00—Processes for applying liquids or other fluent materials
- B05D1/28—Processes for applying liquids or other fluent materials performed by transfer from the surfaces of elements carrying the liquid or other fluent material, e.g. brushes, pads, rollers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/02—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by baking
- B05D3/0254—After-treatment
- B05D3/0272—After-treatment with ovens
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/14—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to metal, e.g. car bodies
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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
- B32B15/04—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
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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
- B32B15/04—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
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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
- B32B15/18—Layered products comprising a layer of metal comprising iron or steel
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/001—Ferrous alloys, e.g. steel alloys containing N
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
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- C—CHEMISTRY; METALLURGY
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- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/22—Ferrous alloys, e.g. steel alloys containing chromium with molybdenum or tungsten
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/26—Ferrous alloys, e.g. steel alloys containing chromium with niobium or tantalum
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
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- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
- C22C38/50—Ferrous alloys, e.g. steel alloys containing chromium with nickel with titanium or zirconium
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- C—CHEMISTRY; METALLURGY
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- C22C—ALLOYS
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- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
- C22C38/54—Ferrous alloys, e.g. steel alloys containing chromium with nickel with boron
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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
- C23C2/04—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
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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
- C23C2/04—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
- C23C2/12—Aluminium or alloys based thereon
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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
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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
- C23C2/28—Thermal after-treatment, e.g. treatment in oil bath
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- 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
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- C23C2/29—Cooling or quenching
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- C23C2/00—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
- C23C2/34—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor characterised by the shape of the material to be treated
- C23C2/36—Elongated material
- C23C2/40—Plates; Strips
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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
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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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- 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
- C23C22/40—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 molybdates, tungstates or vanadates
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- C—CHEMISTRY; METALLURGY
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Abstract
更简便地提供热压制后的涂膜密合性优异的热浸镀锌系钢板。本发明的热浸镀锌系钢板具有作为基材的热浸镀锌系钢板、和在前述热浸镀锌系钢板的至少单面上形成的表面处理层,前述表面处理层以0.2g/m2以上且2g/m2以下的范围含有粒径为5nm以上且500nm以下的选自氧化锆、氧化镧、氧化铈和氧化钕中的1种或2种以上的氧化物。
Description
技术领域
本发明涉及热浸镀锌系钢板。
背景技术
近年,为了环境保护和防止全球变暖,抑制化石燃料消耗的要求增高,该要求正对各种制造业产生影响。例如:对于作为移动手段每天生活、活动不可或缺的汽车也不例外,要求通过车体的轻量化等实现燃油效率的提高等。然而,对于汽车来说,仅实现车体的轻量化在产品功能上不被允许,需要确保适当的安全性。
汽车的结构大多为铁系材料、尤其是由钢板形成,降低该钢板的重量对车体的轻量化是重要的。然而,如上所述,仅单纯地降低钢板的重量不被允许,要求同时确保钢板的机械强度。对这样的钢板的要求不仅是汽车制造业,在各种的制造业中也是同样。因此,对于通过提高钢板的机械强度,即便比以往使用的钢板薄壁化也可以维持或提高机械强度的钢板,正在进行研究开发。
一般,具有高机械强度的材料在弯曲加工等成形加工中存在形状保持性降低的倾向,难以成形加工成复杂的形状。作为解决对于该成形性的问题的手段之一,可列举出所谓的“热压制法(也称热冲压法、热压法、或模压淬火法。)”。热压制方法是将作为成形对象的材料暂时加热至高温,对通过加热而软化了的钢板进行冲压加工而成形后,进行冷却。根据该热压制方法,将材料暂时加热至高温、使其软化,因此可以容易地对作为对象的材料进行压制加工。进一步,通过成形后的冷却的淬火效果,可以提高材料的机械强度。因此,通过热压制方法可以得到兼顾良好的形状保持性和高机械强度的成形品。
然而,将该热压制方法应用于钢板时,钢板被加热到800℃以上的高温因此钢板的表面氧化,生成氧化皮(化合物)。因此,进行热压制加工后,需要去除该氧化皮的工序(所谓的除氧化皮工序),生产率降低。另外,对于需要耐腐蚀性的构件等,需要在加工后对构件表面进行防锈处理、金属覆盖,需要表面清净化工序和表面处理工序,生产率进一步降低。
作为抑制这样的生产率的降低的方法,例如可列举出对要进行热压制的钢板预先实施覆盖的方法。作为钢板上的覆盖,一般使用有机系材料、无机系材料等各种材料。其中,对于钢板具有牺牲性防蚀作用的镀锌(Zn)系钢板,从其防蚀性能和钢板生产技术的观点来看,在汽车钢板等中广泛被使用。
通过实施Zn系的金属覆盖,可以防止在钢板表面的氧化皮的生成,不需要除氧化皮等工序,因此成形品的生产率提高。另外,Zn系的金属覆盖还具有防锈效果,因此耐腐蚀性也提高。对具有规定的成分组成的钢板实施Zn系的金属覆盖的镀覆钢板进行热压制的方法公开有下述专利文献1~专利文献4。
下述专利文献1~专利文献3中,作为热压制用钢板,利用热浸镀Zn钢板或合金化热浸镀Zn钢板。将热浸镀Zn钢板或合金化热浸镀Zn钢板利用于热压制,由此表面未形成铁氧化物(即氧化皮)、可以成形结构构件。另外,下述专利文献4中公开有以下发明:镀Zn系钢板经热压制的热处理钢材的表面形成了厚厚的氧化Zn层,对热处理钢材的涂膜密合性、涂装后耐腐蚀性产生不良影响,因此对热处理钢材进行喷丸而去除氧化Zn层,或降低氧化Zn层的厚度后进行涂装。
另外,下述专利文献5和专利文献6中公开有改善镀Zn系钢板经热压制的热处理钢材的涂膜密合性、涂装后耐腐蚀性的发明。下述专利文献5中公开有将由有机硅树脂皮膜覆盖表面的热浸镀Zn钢板用作热压制用钢板的发明,另外,下述专利文献6中公开有将由含有磷(P)和硅(Si)的阻隔层(作为P例示出磷酸盐,作为Si例示出胶体二氧化硅。)覆盖的热浸镀Zn钢板用作热压制用钢板的发明。
另外,下述专利文献7中公开有镀Zn层中添加比Zn更易氧化的元素(易氧化性元素),在热压制时的升温中,这些易氧化性元素的氧化物层在镀Zn层的表层形成从而防止锌的挥发的技术。
根据下述专利文献5~专利文献7公开的发明,镀Zn层被前述阻隔层覆盖因此抑制Zn的蒸发,由此,中间涂膜、顶涂涂膜的密合性、涂装后耐腐蚀性良好。
现有技术文献
专利文献
专利文献1:日本特开2003-73774号公报
专利文献2:日本特开2003-129209号公报
专利文献3:日本特开2003-126921号公报
专利文献4:日本特开2004-323897号公报
专利文献5:日本特开2007-63578号公报
专利文献6:日本特开2007-291508号公报
专利文献7:日本特开2004-270029号公报
发明内容
发明要解决的问题
然而,对于镀Zn系钢板,尤其在将热浸镀Zn钢板或合金化热浸镀Zn钢板热压制时,有时难以附着由磷酸盐处理形成的磷酸盐皮膜(即磷酸盐处理性低)。除了铝(Al)为主要成分的镀Zn-Al系合金以外,对于作为本发明对象的热浸镀Zn系也在镀浴和镀层中含有Al。其理由如下。即镀浴的温度为440~480℃左右,在该温度域中,Zn与Fe接触则由于Fe与Zn连续地合金化而产生浮渣。通过使镀浴中含有Al,在发生Fe与Zn的反应之前,发生Fe与Al的反应,结果浮渣的产生受到抑制。从该理由来看,通常热浸镀Zn浴中含有Al。
一般,对于热浸镀Zn,镀浴中含有0.2~0.3%的Al,镀层中含有0.2~1.0质量%的Al,对于合金化热浸镀Zn,镀浴中含有0.1~0.2%的Al,镀层中含有0.1~0.5质量%的Al。
该镀层中的Al在镀膜形成时以及在热压制的加热时扩散并向镀层的表层移动,形成Al氧化膜。Al氧化膜不溶解于磷酸,因此Zn与磷酸盐(磷酸锌等)的反应受到阻碍,Al氧化膜形成的区域变得难以形成磷酸盐皮膜。结果,Al氧化膜形成的区域的磷酸盐处理性低。尤其,在热压制工序中,通电加热或感应加热将钢板急速加热至Ac3点以上后,迅速进行压制成形时,磷酸盐处理性明显降低。此时,涂装密合性也降低。
并且,本发明人等对上述专利文献5公开的将用有机硅树脂皮膜覆盖表面的热浸镀Zn钢板用作热压制用钢板而得到的热处理钢材进行追加试验,结果如后所述,弄清了在反复干湿环境的循环腐蚀试验中的涂装后耐腐蚀性虽良好,但涂装密合性未必良好。因此,通过上述专利文献5公开的发明得到的热处理钢材不适合直接用于例如结构上容易积水的部位、构件(例如:车门下部的袋状结构部位、发动机舱内的闭合截面构件等)。
另一方面,上述专利文献7公开的锌镀层中添加易氧化性元素需要在镀浴的温度管理、浮渣对策等作业上花费新功夫。
于是,本发明是鉴于上述问题而完成的,本发明的目的在于更简便地提供热压制后的涂膜密合性优异的热浸镀锌系钢板。
用于解决问题的方案
本发明人等基于对于以上述为目的的热压制用的镀覆钢板进行了深入研究的结果而得到的见解,想到如下的热浸镀锌系钢板。
本发明的主旨如下。
(1)一种热浸镀锌系钢板,其具备:作为基材的热浸镀锌系钢板、和在前述热浸镀锌系钢板的至少单面形成的表面处理层,前述表面处理层以每单面0.2g/m2以上且2g/m2以下的范围含有粒径为5nm以上且500nm以下的选自氧化锆、氧化镧、氧化铈和氧化钕中的1种或2种以上的氧化物。
(2)根据(1)所述的热浸镀锌系钢板,其中,前述表面处理层还以每单面的含量计按照以下所示范围含有:含磷化合物、含钒化合物、含铜化合物、含铝化合物、含硅化合物、或含铬化合物的至少任一者。
含磷化合物:以P换算为0.0g/m2以上且0.01g/m2以下
含钒化合物:以V换算为0.0g/m2以上且0.01g/m2以下
含铜化合物:以Cu换算为0.0g/m2以上且0.02g/m2以下
含铝化合物:以Al换算为0.0g/m2以上且0.005g/m2以下
含硅化合物:以Si换算为0.0g/m2以上且0.005g/m2以下
含铬化合物:以Cr换算为0.0g/m2以上且0.01g/m2以下
(3)根据(1)或(2)所述的热浸镀锌系钢板,其中,前述选自氧化锆、氧化镧、氧化铈和氧化钕中的1种或2种以上的氧化物的粒径为10nm以上且200nm以下。
(4)根据(1)~(3)中任一项所述的热浸镀锌系钢板,其中,前述选自氧化锆、氧化镧、氧化铈和氧化钕中的1种或2种以上的氧化物的含量为每单面0.4g/m2以上且1.5g/m2以下。
(5)根据(1)~(4)中任一项所述的热浸镀锌系钢板,其中,前述氧化物为氧化锆或氧化镧。
(6)根据(1)~(5)中任一项所述的热浸镀锌系钢板,其中,前述表面处理层还以每单面0.2g/m2以上且2g/m2以下的范围含有粒径为2nm以上且100nm以下的选自氧化钛、氧化镍和氧化锡(IV)中的1种或2种以上的氧化物。
(7)根据(6)所述的热浸镀锌系钢板,其中,前述选自氧化钛、氧化镍和氧化锡(IV)中的1种或2种以上的氧化物的粒径为5nm以上且50nm以下。
(8)根据(6)或(7)所述的热浸镀锌系钢板,其中,前述选自氧化钛、氧化镍和氧化锡(IV)中的1种或2种以上的氧化物的含量为每单面0.4g/m2以上且1.5g/m2以下。
(9)根据(6)~(8)中任一项所述的热浸镀锌系钢板,其中,前述氧化物为氧化钛。
(10)根据(1)~(9)中任一项所述的热浸镀锌系钢板,其中,前述表面处理层还以每单面0.2g/m2以上且5.0g/m2以下的范围含有氧化镁、氧化钙或氧化锌。
(11)根据(10)所述的热浸镀锌系钢板,其中,前述氧化镁、氧化钙或氧化锌的粒径为5nm以上且100nm以下。
(12)根据(10)或(11)所述的热浸镀锌系钢板,其中,前述氧化镁、氧化钙或氧化锌的含量为每单面0.4g/m2以上且2.5g/m2以下。
(13)根据(1)~(12)中任一项所述的热浸镀锌系钢板,其为热压制用热浸镀锌系钢板。
发明的效果
根据如上说明的本发明,可以提高与热压制后实施的涂膜的涂装密合性。
具体实施方式
以下对本发明适宜的实施方式进行详细地说明。
<1.热浸镀锌系钢板>
本发明的实施方式的热浸镀Zn系钢板在基材钢板上具备热浸镀Zn系层,进一步在该热浸镀Zn系层上的至少单面具备以下详述的表面处理层。该表面处理层以0.2g/m2以上且2g/m2以下的范围含有粒径为5nm以上且500nm以下的选自氧化锆、氧化镧、氧化铈和氧化钕中的1种或2种以上的氧化物。具有该结构的热浸镀Zn系钢板可以适宜使用之前所说明的热压制法。以下,对于该热浸镀Zn系钢板的结构详细说明。
(1)基材钢板
对于本实施方式的热浸镀Zn系钢板使用的基材钢板,没有特别的限定,可以使用具有公知的特性、化学组成的各种钢板。对钢板的化学组成没有特别的限定,优选可通过淬火得到高强度的化学组成。例如为了得到拉伸强度为980MPa以上的热处理钢材时,基材钢板可例示出由具有以下化学组成的淬火用钢形成:以质量%计含有C:0.05~0.4%、Si:0.5%以下、Mn:0.5~2.5%、P:0.03%以下、S:0.01%以下、sol.Al:0.1%以下、N:0.01%以下、B:0~0.005%、Ti:0~0.1%、Cr:0~0.5%、Nb:0~0.1%、Ni:0~1.0%、和Mo:0~0.5%,余量为Fe和杂质。
要得到淬火时的强度不足980MPa的强度较低的热处理钢材时,基材钢板的化学组成可以不处于上述范围。
从上述淬火时的淬火性的观点、以及形成加热后的氧化锌层中包含的Mn氧化物和Cr氧化物的观点来看,Mn含量和Cr含量优选为Mn+Cr:0.5~3.0%。进一步,Mn含量和Cr含量更优选为Mn+Cr:0.7~2.5%。
作为钢板的化学组成含有Mn和Cr,则热压制后在表层形成的氧化锌层的一部分为含有Mn和Cr的复合氧化物。形成这些含有Mn和Cr的复合氧化物,从而磷酸盐系的化学转化处理后的涂装密合性进一步提高。详细虽不明,但认为通过形成这些复合氧化物,与氧化锌相比较,形成的磷酸盐系的化学转化处理皮膜的耐碱性提高、体现良好的涂装密合性。
作为钢板的化学组成,含有Mn和Cr时,其含量如上所述,按照Mn+Cr以质量%计优选为0.5%以上且3.0%以下的范围,更优选以质量%计为0.7%以上且2.5%以下的范围。Mn+Cr的含量不足0.5%时,热压制后表层形成的氧化锌与含有Mn和Cr的复合氧化物变得不充分,有时难以体现更良好的涂装密合性。另一方面,Mn+Cr的含量超过3.0%时,关于涂装密合性没有问题但成本变高,另外有时点焊部的韧性的降低变得显著、镀覆的湿润性的劣化变得显著。
(2)热浸镀Zn系层
作为本实施方式的热浸镀Zn系层,没有特别的限定,可以使用一般已知的热浸镀Zn系。具体而言,作为本实施方式的热浸镀Zn系层可列举出:热浸镀Zn、合金化热浸镀Zn、镀Zn-55%Al、镀Zn-11%Al、镀Zn-11%Al-3%Mg、镀Zn-7%Al-3%Mg、镀Zn-11%Al-3%Mg-0.2%Si等。需要说明的是,如之前所说明,希望注意热浸镀Zn、还是合金化热浸镀Zn都含有Al。
作为本实施方式的具体镀覆操作,使钢板浸渍在保持有处于熔融状态的Zn或Zn合金镀浴,对钢板实施从该镀浴中提起的操作。对钢板的镀覆附着量的控制通过钢板的提起速度、从镀浴上方设置的擦拭喷嘴喷出的擦拭气体的流量、流速调节等来进行。另外,合金化处理如下进行,在如上所述的镀覆处理后,用燃气炉、感应加热炉、并用它们的加热炉等对镀覆后的钢板追加加热。对于该镀覆操作,可以通过卷材的连续镀覆法,或者截板单体的镀覆法中的任一者进行镀覆。
该热浸镀Zn系层的厚度(即热浸镀Zn系层的附着量)优选处于每单面20g/m2~100g/m2的范围。热浸镀Zn系层的厚度不足每单面20g/m2时,不能确保热压制后的有效Zn量而耐腐蚀性变得不充分,故不优选。另外,热浸镀Zn系层的厚度超过每单面100g/m2时,热浸镀Zn系层的加工性和密合性降低,故不优选。更优选的热浸镀Zn系层的厚度为每单面30g/m2~90g/m2的范围。
(3)表面处理层
在如上所述的热浸镀Zn系层上,进一步,形成有含有选自氧化锆(ZrO2)、氧化镧、氧化铈和氧化钕中的1种或2种以上的氧化物的表面处理层。
此处,“氧化锆”的含义如下:不是像碳酸锆、硝酸锆、硫酸锆的铵盐、钾盐、钠盐等等这样以溶解在处理液中的状态存在的物质,而是以一次粒径为数nm以上的固体的形式分散在处理液中的状态存在的以锆(Zr)的氧化物为主体的物质。通过使用以这样的固体状态分散在处理液中的氧化锆,可以提供在盐水浸渍的环境下的耐久性优异的热处理钢材。
需要说明的是,这些选自氧化锆、氧化镧、氧化铈和氧化钕中的1种或2种以上的氧化物在表面处理层中以颗粒的状态存在。
具体而言,如上所述的粒状的氧化锆、氧化镧、氧化铈和氧化钕的粒径(一次粒径)为5nm以上且500nm以下。在涂装后耐腐蚀性的方面,氧化锆、氧化镧、氧化铈和氧化钕的粒径越小越有利,粒径不足5nm的颗粒难以获得,在成本面是不利的。另外,氧化锆、氧化镧、氧化铈和氧化钕的粒径超过500nm时,氧化锆、氧化镧、氧化铈、氧化钕与镀覆钢板的接触面积变小,热压制时的加热时的氧化锆颗粒对钢板产生的影响变小,故不优选。氧化锆、氧化镧、氧化铈和氧化钕的粒径优选为10nm以上且200nm以下。
需要说明的是,如上所述的氧化锆、氧化镧、氧化铈和氧化钕的粒径(一次粒径)可以通过公知的方法测定,例如可以通过如下方法测定:制作包埋涂装后截面的样品,测定几处皮膜中的氧化锆、氧化镧、氧化铈和氧化钕的粒径,将得到的测定结果取平均值作为粒径。
本实施方式的热浸镀Zn系钢板具备的表面处理层以每单面0.2g/m2以上且2g/m2以下的范围含有具有如上所述的一次粒径的选自氧化锆、氧化镧、氧化铈和氧化钕中的1种或2种以上。该表面处理层中选自氧化锆、氧化镧、氧化铈和氧化钕中的1种或2种以上的含量处于每单面0.2g/m2以上且2g/m2以下的范围,使热压制前存在、且在热压制时形成的Al氧化物对加热时表面处理层中的氧化锆、氧化镧、氧化铈、氧化钕无害化。由此,热压制时的氧化锌的形成受到促进,热压制后的磷酸盐处理性提高、涂膜密合性提高。对于氧化锆、氧化镧、氧化铈、氧化钕的加热时的Al氧化物的无害化,详细虽不明,但考虑是在钢板表面形成的Al氧化物被氧化锆、氧化镧、氧化铈、氧化钕溶解,由此Al之后容易氧化的Zn在热压制时被氧化,其结果,促进化学转化性优异的氧化锌(ZnO)的生成。
表面处理层中的选自氧化锆、氧化镧、氧化铈和氧化钕中的1种或2种以上的含量不足每单面0.2g/m2时,热压制后不能存在充分的氧化锆、氧化镧、氧化铈、氧化钕,镀覆表面的Al氧化物的无害化效果变小,不能充分地确保热压制后的涂装密合性。另一方面,表面处理层中的氧化锆的含量超过每单面2g/m2时,认为本实施方式的热浸镀Zn系钢板的成本上升,并且表面处理层的内聚力变弱、热压制后表面处理层上形成的涂膜变得容易剥离。
该表面处理层中选自氧化锆、氧化镧、氧化铈和氧化钕中的1种或2种以上的含量优选为每单面0.4g/m2以上且1.5g/m2以下。
作为含有氧化锆、氧化镧、氧化铈和氧化钕的处理液,代表性可例示出:氧化锆溶胶、氧化镧溶胶、氧化铈溶胶、氧化钕溶胶,作为具体的市售产品,可例示出日产化学工业株式会社制造的NanoUse(注册商标)系列、多木化学株式会社制造的ceramace(セラメース)系列。
表面处理层的形成,可以将如上所述的氧化锆溶胶、氧化镧溶胶、氧化铈溶胶、氧化钕溶胶直接涂布在热浸镀Zn系钢板上,为了改善处理液的稳定性、表面处理层的密合性,在混合树脂、交联剂制成处理液后,涂布在热浸镀Zn系钢板上是优选的。
作为该树脂,在使用氧化锆溶胶、氧化镧溶胶、氧化铈溶胶、氧化钕溶胶时,优选使用水溶性或水分散性的树脂,作为树脂的种类,可列举出聚氨酯树脂、聚酯树脂、环氧树脂、(甲基)丙烯酸系树脂、聚烯烃树脂、酚醛树脂、或这些树脂的改性体等。对于使用氧化锆粉末时,在上述水系树脂的基础上,可以使用各种溶剂作为溶剂的溶剂系树脂。
作为该交联剂,可列举出碳酸锆化合物、有机钛化合物、噁唑啉聚合物、水溶性环氧化合物、水溶性三聚氰胺树脂、水分散封端异氰酸酯、水系氮丙啶化合物等。
另外,作为本实施方式的表面处理层中进一步含有的优选的其它成分,可列举出选自氧化钛、氧化镍和氧化锡(IV)中的1种或2种以上。
表面处理层中含有选自上述氧化钛、氧化镍和氧化锡(IV)中的1种或2种以上时,热压制后这些氧化物存在于钢板表面,从而对电沉积涂装时的电沉积涂膜的聚集析出有一些影响,由于氧化物与电沉积涂膜牢固地密合,因而即使有时化学转化处理(磷酸盐处理、FF化学转化处理)不充分,也能体现牢固的密合性。为了更有效地得到该效果,上述氧化物的粒径优选为2nm以上且100nm以下。
并且,这些氧化物之中,对于氧化钛,在上述特征之外,在热压制时,可以抑制过度的Zn的氧化、蒸发,在提高热压制后的涂膜密合性的基础上,还可以提高热压制后的耐腐蚀性。推测氧化钛通常以金属氧化物的状态稳定地存在,但会与热压制的加热时形成的氧化锌反应,形成与氧化锌的复合氧化物,由此抑制过度的Zn的氧化、蒸发。为了更有效地得到该效果,上述氧化钛的粒径优选为2nm以上且100nm以下。
需要说明的是,上述选自氧化钛、氧化镍和氧化锡(IV)中的1种或2种以上的粒径更优选为5nm以上且50nm以下。
表面处理层含有氧化钛、氧化镍和氧化锡(IV)时,其含量优选以每单面0.2g/m2以上且2g/m2以下的范围含有,更优选处于每单面0.4g/m2以上且1.5g/m2以下的范围。氧化钛、氧化镍和氧化锡(IV)的含量不足每单面0.2g/m2时,热压制后这些氧化物未充分存在,因此有时难以体现与电沉积涂膜更良好的密合性.
另一方面,氧化钛、氧化镍和氧化锡(IV)的含量超过每单面2g/m2时,认为本实施方式的镀Zn系钢板的成本上升,并且表面处理层的内聚力变弱、热压制后表面处理层上形成的涂膜变得容易剥离。
并且,对于氧化钛,含量不足每单面0.2g/m2时,除了上述之外,不能形成足够的与氧化锌的复合氧化物,有时难以有效地抑制Zn的氧化、蒸发。
另外,作为本实施方式的表面处理层中进一步含有的优选的其它成分,可列举出氧化镁、氧化钙或氧化锌。
表面处理层中含有上述氧化镁、氧化钙或氧化锌,热压制后的表面处理层的表层存在这些氧化物,由此磷酸盐处理性提高。作为磷酸盐处理性提高的理由,认为氧化镁等在磷酸盐处理液中溶解,从而促进与磷酸盐的化学转化反应。为了更有效地得到该效果,上述氧化镁、氧化钙或氧化锌的粒径优选为5nm以上且100nm以下,进一步优选为10nm以上且50nm以下。
表面处理层含有氧化镁、氧化钙或氧化锌时,其含量优选以每单面0.2g/m2以上且5g/m2以下的范围含有,更优处于每单面0.4g/m2以上且2.5g/m2以下的范围。氧化镁、氧化钙和氧化锌的含量不足每单面0.2g/m2时,热压制后这些氧化物未充分存在,因此有时难以体现良好的磷酸盐处理性。另一方面,氧化镁、氧化钙和氧化锌的含量超过每单面2g/m2时,认为本实施方式的镀Zn系钢板的成本上升,并且表面处理层的内聚力变弱、热压制后表面处理层上形成的涂膜变得容易剥离。
本实施方式的表面处理层除了如上所述的氧化物之外也可以在规定的含量的范围内含有以下详述的含P化合物、含V化合物、含Cu化合物、含Al化合物、含Si化合物、或含Cr化合物的至少任一者。
含P化合物为含有磷作为构成元素的化合物。作为该含P化合物,例如可列举出:磷酸、亚磷酸、膦酸、亚膦酸、次膦酸、三价膦酸、氧化膦、膦等化合物、以这些化合物作为阴离子的离子化合物等。这些含P化合物均为市售的试剂或产品,可以容易地获得。这些含P化合物以溶解在处理液中的状态、或者以粉末的形式分散在处理液中的状态存在,在表面处理层中,以固体形式分散的状态存在。
含V化合物是含有钒作为构成元素的化合物。作为该含V化合物,例如可列举出:包含五氧化钒在内的钒氧化物、包含偏钒酸铵在内的偏钒酸系化合物、包含钒酸钠在内的钒化合物、和其它含V的化合物等。这些含V化合物均为市售的试剂或产品,可以容易地获得。这些含V化合物以溶解在处理液中的状态、或者以粉末的形式分散在处理液中的状态存在,在表面处理层中,以固体形式分散的状态存在。
本实施方式的表面处理层将选自如上所述的含P化合物和含V化合物中的1种或2种以上的化合物按照以P和以V换算计分别为每单面0.0g/m2以上且0.01g/m2以下的范围含有是优选的。
如上的选自的含P化合物和含V化合物中的1种或2种以上的化合物在热压制时被氧化成为氧化物,偏在于热浸镀Zn系层和表面处理层的界面,形成含有选自P或V的至少任一者的内聚力弱的氧化物层。选自含P化合物和含V化合物中的1种或2种以上的化合物的含量以P和V换算分别为每单面0.0g/m2以上且0.01g/m2以下的范围,由此热压制时形成的如上所述的内聚力弱的氧化物层的厚度变薄,热压制后的热浸镀Zn系层与表面处理层的密合性进一步提高。
表面处理层中选自含P化合物和含V化合物中的1种或2种以上的含量超过每单面0.01g/m2时,热压制时形成的内聚力弱的氧化物层的厚度变厚,热浸镀Zn系层与表面处理层的密合性降低,结果,电沉积涂装后的密合性也降低。从热压制后的热浸镀Zn系层与表面处理层的密合性的观点来看,表面处理层中选自含P化合物和含V化合物中的1种或2种以上的化合物的含量更优选为以P和V换算分别为每单面0.0g/m2以上且0.003g/m2以下。
含Cu化合物是含有铜作为构成元素的化合物。作为该含Cu化合物,例如可列举出:金属Cu、氧化铜、各种有机铜化合物、各种无机铜化合物、各种铜络合物等。这些含Cu化合物均为市售的试剂或产品,可以容易地获得。这些含Cu化合物以溶解在处理液中的状态、或者以粉末的形式分散在处理液中的状态存在,在表面处理层中,以固体形式分散的状态存在。
本实施方式的表面处理层优选以Cu换算为每单面0.0g/m2以上且0.02g/m2以下的范围含有选自如上所述的含Cu化合物中的1种或2种以上的化合物。
选自如上所述的含Cu化合物中的1种或2种以上的化合物在热压制时被氧化成为氧化物,偏在于热浸镀Zn系层和表面处理层的界面,形成含Cu的内聚力弱的氧化物层。选自含Cu化合物中的1种或2种以上的化合物的含量以Cu换算为每单面0.0g/m2以上且0.02g/m2以下的范围,由此热压制时形成的如上所述的内聚力弱的氧化物层的厚度变薄,热压制后的热浸镀Zn系层与表面处理层的密合性进一步提高。
表面处理层中的选自含Cu化合物中的1种或2种以上的含量超过每单面0.02g/m2时,热压制时形成的内聚力弱的氧化物层的厚度变厚,热浸镀Zn系层和表面处理层的界面的密合性降低,结果,电沉积涂装后的密合性也降低。并且,Cu是比作为基材钢板的主成分的Fe更贵的元素,因此对耐腐蚀性也存在降低倾向。从热压制后的热浸镀Zn系层与表面处理层的密合性的观点来看,表面处理层中的选自含Cu化合物中的1种或2种以上的化合物的含量更优选以Cu换算为每单面0.0g/m2以上且0.005g/m2以下。
含Al化合物是含有铝作为构成元素的化合物。作为该含Al化合物,例如可列举出:金属Al、氧化铝、氢氧化铝、以铝离子为阳离子的离子化合物等。这些含Al化合物均为市售的试剂或产品,可以容易地获得。这些含Al化合物以溶解在处理液中的状态、或者以粉末的形式分散在处理液中的状态存在,在表面处理层中,以固体形式分散的状态存在。
含Si化合物是含有硅作为构成元素的化合物。作为该含Si化合物,例如可列举出:Si单质、二氧化硅(氧化硅)、有机硅烷、用作粘合剂树脂的有机硅树脂、以及其它含Si的化合物。这些含Si化合物均为市售的试剂或产品,可以容易地获得。这些含Si化合物以溶解在处理液中的状态、或者以粉末的形式分散在处理液中的状态存在,在表面处理层中,以固体形式分散的状态存在。
本实施方式的表面处理层优选以Al和Si换算分别为每单面0.0g/m2以上且0.005g/m2以下的范围含有选自如上所述的含Al化合物和含Si化合物中的1种或2种以上的化合物。
如上所述,选自含Al化合物和含Si化合物中的1种或2种以上的化合物在热压制时被氧化成为氧化物,在表面处理层的表面富集。选自含Al化合物和含Si化合物中的1种或2种以上的化合物的含量处于以Al和Si换算分别为每单面0.0g/m2以上且0.005g/m2以下的范围,由此在热压制时表面处理层的表面形成的含有Al或Si的氧化物的存在比率变小,热压制后的表面处理层与电沉积涂膜的密合性进一步提高。
表面处理层中选自含Al化合物和含Si化合物中的1种或2种以上的含量超过每单面0.005g/m2时,热压制时形成的含Al或Si的氧化物的存在比率变大。这些含Al或Si的氧化物阻碍化学转化处理皮膜的形成、并且还使热压制后的表面处理层与电沉积涂膜的密合性降低,因此由于热压制时形成的含Al或Si的氧化物的存在比率变大,表面处理层与电沉积涂膜的密合性降低。从热压制后的表面处理层与电沉积涂膜的密合性(即涂装后密合性)的观点来看,表面处理层中选自含Al化合物和含Si化合物中的1种或2种以上的化合物的含量更优选以Al和Si换算分别为每单面0.0g/m2以上且0.002g/m2以下。
含Cr化合物是含有铬作为构成元素的化合物。作为该含Cr化合物,例如可列举出:金属Cr、具有各种价数的铬化合物、以及以具有各种价数的铬离子为阳离子的离子化合物等。这些含Cr化合物以溶解在处理液中的状态、或者以粉末的形式分散在处理液中的状态存在,在表面处理层中,以固体形式分散的状态存在。
含Cr化合物根据价数而性能和性质不同,对于6价铬化合物,存在多种有害的化合物。鉴于最近强烈要求对于环境保护的关照的倾向,本实施方式的表面处理层优选尽量不含有如上所述的含Cr化合物,更优选无铬。
从如上所述的的观点来看,本实施方式的表面处理层优选以Cr换算为每单面0.0g/m2以上且0.01g/m2以下的范围含有选自如上所述的含Cr化合物中的1种或2种以上的化合物,更优选不含含Cr化合物。
另外,只要不阻碍基于含有选自氧化锆、氧化镧、氧化铈和氧化钕中的1种或2种以上的本发明的效果,表面处理层还可以含有炭黑、二氧化钛等颜料、涂装钢板使用的各种防锈颜料等。此时,表面处理层以每单面0.2g/m2以上且2g/m2以下的范围含有粒状的氧化锆等。
通过添加这些颜料,虽不能直接改善热压制后的涂膜密合性、耐腐蚀性,但炭黑、二氧化钛等颜料在炉中热压制加热时提高钢板表面的辐射率,从而加热时间可以为短时间。防锈颜料可以抑制热压制加热前钢板腐蚀。
需要说明的是,该表面处理层的形成方法将含有粒状的选自氧化锆、氧化镧、氧化铈和氧化钕中的1种或2种以上的处理液涂布在镀锌钢板表面,进行干燥和烘烤即可。
涂布方法并不限定于特定的方法,例示出:将基材钢板浸渍在处理液中,或在基材钢板的表面喷雾处理液后,通过辊、气体吹送控制附着量成为规定附着量的方法:用辊涂机、棒涂机涂布的方法。
另外,干燥、烘烤方法只要是可以使分散介质(主要为水)挥发的方法,就不限定于特定的方法。此处,担心过高温下加热则表面处理层的均匀性降低,反之担心过低温下加热则生产率降低。因此,为了稳定且有效地制造具有优异特性的表面处理层,将涂布后的表面处理层在80℃~150℃左右的温度下加热5秒~20秒左右是优选的。
另外,表面处理层的形成在镀覆钢板的生产线中在线进行是经济的、优选,也可以在另一生产线形成、或者在进行用于成形的冲切后形成。
此处,表面处理层中的氧化锆、氧化镧、氧化铈、氧化钕、氧化钛、氧化镍、氧化锡(IV)、氧化镁、氧化钙、氧化锌的含量可以通过公知的方法测定,例如:可以事前用截面能量分散型X射线(Energy Dispersive X-ray:EDX)分析等确认各种化合物为氧化锆、碱土金属的氧化物,之后溶解皮膜,使用ICP(Inductively Coupled Plasma、电感耦合等离子体)发射光谱分析法等来测定。另外,对于表面处理层中的上述含P化合物、含V化合物、含Cu化合物、含Al化合物、含Si化合物、和含Cr化合物的含量也可以通过同样的方法测定。
<2.关于热压制工序>
之前所说明的热浸镀Zn系钢板应用于热压制法时,热浸镀Zn系钢板被加热至规定的温度后,进行压制成形。本实施方式的热浸镀Zn系钢板的情况,由于进行热压制成形,通常加热至700~1000℃,急速冷却后变为马氏体单相、或马氏体以体积率计为90%以上时,加热温度的下限温度设定为Ac3点以上是重要的。本发明的情况由于包含急速冷却后马氏体/铁素体的2相域的情况,因此作为加热温度优选如上所述设定为700~1000℃。
热压制法中,有利用缓加热的热压制和利用急速加热的热压制这2种方法。作为使用的加热方法,可列举出电炉、燃气炉、火焰加热、通电加热、高频加热、感应加热等,对加热时的气氛也没有特别的限定,作为可以使本发明的效果显著的加热方法,优选使用作为急速加热的通电加热、感应加热等。
利用缓加热的热压制法中利用加热炉的辐射加热。首先,将本实施方式的热浸镀Zn系钢板用作热压制用钢板,装入加热炉(燃气炉、电炉等)。在加热炉内,将热压制用钢板加热至700~1000℃,根据条件,保持该加热温度(均热)。由此,热浸镀Zn系层中的熔融Zn与Fe键合,变为固相(Fe-Zn固溶体相)。使热浸镀Zn系层中的熔融Zn与Fe键合而固相化后,从加热炉抽出钢板。需要说明的是,也可以利用均热使热浸镀Zn系层中的熔融Zn与Fe键合,在以Fe-Zn固溶体相和ZnFe合金相的方式固相化后,从加热炉抽出钢板。
与其相对,也可以将热浸镀Zn系钢板加热至700~1000℃,无保持时间、或保持时间为短时间,从加热炉抽出钢板。该情况下,将钢板加热至700~1000℃后,不利用压制成形等对钢板赋予应力地冷却至热浸镀Zn系层中的熔融Zn与Fe键合形成固相(Fe-Zn固溶体相或ZnFe合金相)为止。具体而言,至少冷却至钢板的温度为782℃以下。冷却后,如以下说明那样,使用模具一边对钢板进行压制一边进行冷却。
利用急速加热的热压制也同样,将本实施方式的热浸镀Zn系钢板用作热压制用钢板,急速加热至700~1000℃。急速加热通过例如通电加热或感应加热实施。该情况下的平均加热速度为20℃/秒以上。急速加热时,热浸镀Zn系钢板加热至700~1000℃后,直至熔融Zn系镀层中的熔融Zn与Fe键合成为固相(Fe-Zn固溶体相或ZnFe合金相),不通过压制成形等对钢板赋予应力地冷却。具体而言,至少冷却直至钢板的温度为782℃以下。冷却后,如以下说明那样,使用模具一边对钢板进行压制一边进行冷却。
抽出的钢板使用模具压制。压制钢板时,钢板被模具冷却。模具内,循环冷却介质(例如水等),模具排热而将钢板冷却。根据以上工序,利用通常加热制造热压制钢材。
使用本实施方式的具有表面处理层的热浸镀Zn系钢板制造的热压制钢材具有优异的磷酸盐处理性和涂装密合性。尤其,本实施方式的热浸镀Zn系钢板在利用急速加热的热压制、利用缓加热的热压制下加热至700~1000℃且无保持时间、或保持时间为短时间的情况下,显著地发挥效果。
使用现有的镀覆钢板,利用通常加热实施热压制时,钢板在加热炉中均热。此时,热压制用钢板的镀层的表层形成Al氧化膜,由于长时间的均热而Al氧化膜某种程度破裂、断开,因此对化学转化处理性的不良影响较小。另一方面,利用急速加热实施热压制时,均热时间极短。所以,在最表面形成的Al氧化膜难以被破坏。所以,使用现有的镀覆钢板时,利用急速加热的热压制与利用通常加热的热压制相比较,热压制钢材的磷酸盐处理性和涂装密合性低。
另一方面,本实施方式的热压制用的热浸镀Zn系钢板在表面处理层中含有选自氧化锆、氧化镧、氧化铈和氧化钕中的1种或2种以上,从而使热压制时Al氧化无害化而促进氧化锌的生成,因此可以发挥良好的磷酸盐处理性和涂装密合性。
实施例
以下,一边示出实施例,一边更具体地说明本发明的实施方式的热浸镀Zn系钢板的作用效果。需要说明的是,以下示出的实施例只不过是本发明的热浸镀Zn系钢板的一例,本发明的热浸镀Zn系钢板并不限定于下述实施例。
<基材钢板>
以下,首先,制造具有以下表1所示的化学组成的钢水。其后,使用制造的各钢水通过连铸法制造板坯。将得到的板坯热轧,制造热轧钢板。接着,将热轧钢板酸洗后,实施冷轧,制造冷轧钢板,制作具有表1记载的化学组成的钢#1~#8的钢板。如表1所示,各钢种的钢板的板厚均为1.6mm。
[表1]
<热浸镀Zn系层>
对钢#1~#8的钢板进行热浸镀Zn处理,其后,实施合金化处理。合金化处理中的最高温度均为530℃,加热约30秒后,冷却至室温,制造合金化热浸镀Zn钢板(GA)。另外,使用钢#1进行热浸镀Zn处理,不进行合金化处理地制造热浸镀Zn钢板(GI)。
进一步,对于钢#1,使用熔融Zn-55%Al、熔融Zn-6%Al-3%Mg、熔融Zn-11%Al-3%Mg-0.2%Si这3种类的镀浴进行各种热浸镀Zn,制造热浸镀Zn系钢板A1~A3。
A1:熔融Zn-55%Al
A2:熔融Zn-6%Al-3%Mg
A3:熔融Zn-11%Al-3%Mg-0.2%Si
需要说明的是,对于上述热浸镀Zn系钢板的镀膜中的Al浓度利用如下方法求出。即从各热浸镀Zn系钢板采集样品。将采集的样品的热浸镀Zn系层用10%HCl水溶液溶解,通过ICP发射光谱分析法进行热浸镀Zn系层的组成分析。基于得到的分析结果,求出每单面的Al浓度(质量%)。得到的结果一并示于以下表3。
<表面处理层>
接着,为了制造按照固体成分比率达到表2的组成的化学溶液,将下述化合物和药剂用水混合。用棒涂机涂布得到的处理液,在最高到达温度100℃下保持8秒钟这样的条件下,使用烘箱进行干燥来制造热压制用镀覆钢板。对于处理液的附着量,按照处理液中的不挥发分的总附着量为表3所示的数值的方式通过液体的稀释和棒涂机的档位来调节。以下表2中,各成分的固体成分浓度记载为“氧化物A”等各成分的不挥发分相对于处理液总体的不挥发分的比率(单位:质量%)。
表2中的各成分(符号)如下。
需要说明的是,如后所述,还研究可作为氧化锆、氧化镧、氧化铈和氧化钕以外的粒状物质含有氧化铝(溶胶)的处理液,此时将氧化铝视为“氧化物A”。同样,氧化钛、氧化镍和氧化锡(IV)记为“氧化物B”,氧化镁、氧化钙和氧化锌记为“氧化物C”。
(氧化物A)氧化锆、氧化镧、氧化铈、氧化钕、氧化铝
ZB:氧化锆溶胶(日产化学工业株式会社NanoUse(注册商标)ZR-40BL)、粒径70~110nm(目录值)
ZA:氧化锆溶胶(日产化学工业株式会社NanoUse(注册商标)ZR-30AL)、粒径70~110nm(目录值)
ZP:氧化锆粉末(高纯度化学研究所制造氧化锆、粒径约1μm
La:氧化镧溶胶(多木化学株式会社Biral La-C10)、粒径40nm(目录值)
Ce:氧化铈溶胶(多木化学株式会社needralP-10)、粒径20nm(目录值)
Nd:氧化钕溶胶(多木化学株式会社Biral Nd-C10)、粒径40nm(目录值)
AZ:氧化铝溶胶(日产化学工业株式会社氧化铝溶胶200)、粒径约10nm
(氧化物B)氧化钛、氧化镍、氧化锡(IV)
Ti:氧化钛溶胶(TAYCA Corporation TKS-203)、粒径约6nm
Ni:氧化镍(IoLiTec氧化镍)、粒径20nm
Sn:氧化锡(IV)溶胶(多木化学株式会社ceramaceC-10)、粒径10nm
(氧化物C)氧化镁、氧化钙、氧化锌
Mg:氧化镁(IoLiTec制造)、粒径35nm(目录值)
Ca:氧化钙(关东化学公司制造)
※在添加树脂的水中分散,用球磨机将颜料粉碎后使用。
Zn:氧化锌(IoLiTec制造)、粒径20nm(目录值)
(iii)树脂
A:氨基甲酸酯系树脂乳液(第一工业制药株式会社Superflex(注册商标)150)
B:氨基甲酸酯系树脂乳液(第一工业制药株式会社Superflex(注册商标)E-2000)
C:聚酯树脂乳液(TOYOBO Co.,Ltd.Vylonal(注册商标)MD1480)
(iv)交联剂
M:三聚氰胺树脂(MITSUI Cytec CYMEL(注册商标)325)
Z:碳酸锆铵(KISHIDA CHEMICAL Co.,Ltd.碳酸锆铵溶液)
S:硅烷偶联剂(NICHIBI TRADING Co.,Ltd.Sila-Ace S510)(含Si化合物)
(v)颜料
CB:炭黑(三菱化学株式会社三菱(注册商标)炭黑#1000)
T:氧化钛(石原产业株式会社氧化钛R-930)、粒径250nm(目录值)
需要说明的是,对于此处记载的“T”氧化钛,主要使用涂料中的白色颜料等,为粒径为200~400nm的颜料,与(氧化物B)相比较,由于粒径大,因此不能满足由氧化物B得到的性能。
PA:缩合磷酸Al(TAYCA aluminium triphosphate K-WHITE ZF150W)(含P、Al化合物)
PZ:亚磷酸锌(东邦颜料株式会社NP-530)(含P化合物)
Si1:二氧化硅颗粒(FUJI SILYSIACHEMICAL LTD.sylomask02)(含Si化合物)
Si2:胶体二氧化硅(日产化学工业株式会社snowtexO)(含Si化合物)
Al:氧化铝溶胶(日产化学工业株式会社AS-200)(含Al化合物)
V:钒酸钾(一般试剂)(含V化合物)
Cr:氧化Cr(VI)(一般试剂)(含Cr化合物)
Cu:氧化铜(II)(一般试剂)(含Cu化合物)
[表2]
[表3]
[表4]
[表5]
[表6]
[表7]
<热压制工序>
在表面处理层的形成工序后,对各试验号码的钢板用炉加热和通电加热这2种类的加热方式进行热压制加热,实施热压制。对于炉加热,炉内气氛设定为910℃、空燃比设定为1.1,钢板温度到达900℃后迅速从炉内取出。对于通电加热,加热速度设定为85℃/秒和42.5℃/秒,加热至870℃。需要说明的是,以下,将比炉加热更短时间的加热的通电加热的结果示于表3,炉加热的结果示于表4。
热压制加热后,冷却直至钢板温度为650℃。冷却后,利用具备水冷夹套的平板模具夹持钢板而制造热压制钢材(钢板)。热压制时冷却速度慢的部分也是以50℃/秒以上的冷却速度的方式冷却至马氏体相变开始点的360℃左右、进行淬火。
<评价方法>
[磷酸盐处理性评价试验]
对于以下表3~表4记载的各试验号码的板状的热压制钢材,使用NihonParkerizing制造的表面调节处理剂PREPALENEX(商品名),在室温下实施20秒表面调节。进一步,使用Nihon Parkerizing制造的磷酸锌处理液Parbond3020(商品名)实施磷酸盐处理。处理液的温度设定为43℃,将板状的热压制钢材在处理液中浸渍120秒钟后,进行水洗、干燥。
磷酸盐处理后的热压制钢材的表面用1000倍的扫描型电子显微镜(SEM)观察任意5个视野(125μm×90μm),得到反射电子图像(BSE像)。反射电子图像中,将观察区域用灰度图像表示。反射电子图像内,形成了作为化学转化皮膜的磷酸盐皮膜的部分和未形成磷酸盐皮膜的部分的对比度不同。其中,未形成磷酸盐皮膜的部分的亮度(多级)的数值范围X1预先由SEM和EDS(能量分散型X射线分光器)决定。
各视野的反射电子图像中,通过图像处理,求出表示数值范围X1内的对比度的区域的面积A1。并且,基于以下式(1),求出各视野的透明面积率TR(%)。
TR=(A1/A0)×100···(1)
此处,上述式(1)中,A0为视野的总面积(11250μm2)。将5个视野的透明面积率TR(%)的平均定义为该试验号码的热压制钢材的透明面积率(%)。
表3~表4中的“磷酸盐处理性”栏的“M”是透明面积率为30%以上的含义。“L”是透明面积率为25%以上且不足30%的含义。“K”是透明面积率为20%以上且不足25%的含义。“J”是透明面积率为15%以上且不足20%的含义。“I”是透明面积率为13%以上且不足15%的含义。“H”是透明面积率为11%以上且不足13%的含义。“G”是透明面积率为10%以上且不足11%的含义。“F”是透明面积率为18%以上且不足10%的含义。“E”是透明面积率为6%以上且不足8%的含义。“D”是透明面积率为5%以上且不足6%的含义。“C”是透明面积率为2.5%以上且不足5%的含义。“B”是透明面积率为1%以上且不足2.5%的含义。“A”是透明面积率不足1%的含义。透明评价中为“I”、“H”、“G”、“F”、“E”、“D”、“C”、“B”或“A”时,判断磷酸盐处理性优异。
[涂装密合性评价试验]
实施上述磷酸盐处理后,对各试验号码的板状的热压制钢材,将NIPPONPAINTCo.,Ltd.制造的阳离子型电沉积涂料在电压160V的斜坡通电下电沉积涂装,进一步,在烘烤温度170℃下烘烤涂装20分钟。对于电沉积涂装后的涂料的膜厚的平均,所有试验号码均为10μm。
电沉积涂装后,将热压制钢材在具有50℃的温度的5%NaCl水溶液中浸渍500小时。浸渍后,试验面60mm×120mm的区域(面积A10=60mm×120mm=7200mm2)全面贴附聚酯制胶带。其后,揭下胶带。求出因胶带的揭下而剥离的涂膜的面积A2(mm2),基于式(2)求出涂膜剥离率(%)。
涂膜剥离率=(A2/A10)×100···(2)
表3~表4中的“涂装密合性”栏的“M”是涂膜剥离率为50.0%以上的含义。“L”是涂膜剥离率为35%以上且不足50%的含义。“K”是涂膜剥离率为20%以上且不足35%的含义。“J”是涂膜剥离率为10%以上且不足20%的含义。“I”是涂膜剥离率为8%以上且不足10%的含义。“H”是涂膜剥离率为6%以上且不足8%的含义。“G”是涂膜剥离率为5%以上且不足6%的含义。“F”是涂膜剥离率为4%以上且不足5%的含义。“E”是涂膜剥离率为3%以上且不足4%的含义。“D”是涂膜剥离率为2.5%以上且不足3%的含义。“C”是涂膜剥离率为1.3%以上且不足2.5%的含义。“B”是涂膜剥离率为0.5%以上且不足1.3%的含义。“A”是涂膜剥离率不足0.5%的含义。涂装密合性评价中为“I”、“H”、“G”、“F”、“E”、“D”、“C”、“B”或“A”时,判断涂装密合性优异。
[循环腐蚀试验]
对于评价面的涂装,用切刀(载荷500gf、1gf约为9.8×10-3N。)划痕,将下述循环条件的循环腐蚀试验实施180个循环。
○循环条件
盐水喷雾(SST、5%NaCl、35℃气氛)2小时→干燥(60℃)2小时→湿润(50℃、98%RH)4小时作为1个循环实施。
其后,观察有无在自切割部宽1cm左右的区域产生的涂膜膨胀。
表3~表4中的“耐腐蚀性”栏的“E”是产生3.0mm以上的涂膜膨胀的含义。“D”是产生2.0mm以上且不足3.0mm的涂膜膨胀的含义。“C”是产生1.0mm以上且不足2.0mm的涂膜膨胀的含义。“B”是产生0.5mm以上且不足1mm的微小的涂膜膨胀的含义。“A”是产生不足0.5mm的极微小的涂膜膨胀的含义。在该循环腐蚀试验中为“C”、“B”或“A”时,判断耐腐蚀性优异。
[表8]
[表9]
[表10]
[表11]
[表12]
[表13]
另外,对于以下表5记载的各试验号码的板状的热压制钢材,代替上述磷酸锌处理,使用含有Zr离子和/或Ti离子、和氟、且含有100~1000ppm的游离氟离子的水溶液(以下称FF化学转化处理液。)实施处理,验证得到的试验片的涂装密合性和耐腐蚀性。
上述FF化学转化处理液溶解游离氟(以下简称FF。)、Al氧化皮膜和Zn氧化皮膜。所以,FF一边将Al氧化皮膜和Zn氧化皮膜的一部分或全部溶解,一边将热冲压工序中形成的含Zn层蚀刻。其结果,形成包含Zr和/或Ti的氧化物、或者Zr和/或Ti的氧化物与氟化物的混合物的化学转化处理层(以下称特定化学转化处理层。)。控制在可以蚀刻Al氧化皮膜和Zn氧化皮膜的FF浓度,则Al氧化皮膜和Zn氧化皮膜被蚀刻,形成特定化学转化处理层。
为了得到该FF化学转化处理液,将H2ZrF6(六氟锆酸)、H2TiF6(六氟钛酸)按照规定的金属浓度加入容器,用离子交换水稀释。其后,将氢氟酸和氢氧化钠水溶液加入容器,将溶液中的氟浓度和游离氟浓度调节到规定值。游离氟浓度的测定使用市售的浓度测定器进行。调节后,将容器用离子交换水定容,制成FF化学转化处理液。
FF化学转化处理如下实施。首先,作为事前处理,使用碱脱脂剂(NIPPONPAINTCo.,Ltd.制造的EC90),在45℃下实施2分钟浸渍脱脂。其后,在以下表6所示的FF化学转化处理液中40℃下浸渍120秒,实施化学转化处理。化学转化处理后,将试验片水洗、干燥。
[表14]
[表15]
表6 FF化学转化处理液
对于得到的试验材,特定化学转化处理层的化学转化处理性用荧光X射线分析测定Zr或者Ti的附着量,附着量的测定值为10~100mg/m2者为“A”,附着量的测定值不足10mg/m2或超过100mg/m2者为“B”,将得到的结果一并示于表5。需要说明的是,对于含氧化锆的体系,预先用荧光X射线分析测定在实施Zr系FF处理前的附着量,从化学转化处理后的Zr附着量减去处理前的Zr附着量为Zr系FF化学转化处理的附着量。另外,对得到的试验材的涂装密合性评价试验和循环腐蚀试验的方法和评价基准,与对形成有上述磷酸盐皮膜的试验材实施的涂装密合性评价试验和循环腐蚀试验同样。
另外,为了验证表面处理层中存在的含P化合物、含V化合物、含Cu化合物、含Al化合物、含Si化合物、含Cr化合物产生的影响,利用表2的No.97~No.164所示的处理液,制造热压制用镀覆钢板。此时,用棒涂机涂布表2的No.97~No.164所示的处理液,在最高到达温度100℃下保持8秒钟的条件下使用烘箱使其干燥。处理液的附着量按照处理液中的不挥发分的总附着量为表7所示的数值的方式通过液体的稀释和棒涂机的档位来调节。
表面处理层的形成工序后,对各试验号码的钢板用通电加热方式进行热压制加热,实施热压制。此时,加热速度设定为85℃/秒和42.5℃/秒,加热至870℃。
热压制加热后,冷却直至钢板温度为650℃。冷却后,利用具备水冷夹套的平板模具夹持钢板地制造热压制钢材(钢板)。热压制时冷却速度慢的部分也是以50℃/秒以上的冷却速度的方式冷却至马氏体相变开始点的360℃左右、进行淬火。
对于以下表7记载的各试验号码的板状的热压制钢材,使用日本Parkerizing制造的表面调节处理剂PREPALENEX(商品名),在室温下实施20秒表面调节。进一步,使用日本Parkerizing制造的磷酸锌处理液Parbond3020(商品名),实施磷酸盐处理。处理液的温度设定为43℃,将板状的热压制钢材在处理液浸渍30秒钟后,进行水洗·干燥。其后,与表3所示情况同样实施磷酸盐处理性评价试验。
另外,对以下表7记载的各试验号码的板状的热压制钢材与表3所示情况同样,分别实施涂装密合性评价试验、和、循环腐蚀试验。各试验的试验方法和评价基准与表3所示情况同样。
[表16]
[表17]
由上述表3、表4、表5和表7表明可知,本发明的热浸镀锌系钢板不仅具有优异的热压制后的涂膜密合性,还具有优异的化学转化处理性和耐腐蚀性。
以上对本发明适宜的实施方式进行详细地说明,但本发明并不限定于这些例子。只要是在本发明所属技术领域中具有通常的知识的人员,则显然可在权利要求书所记载的技术思想的范畴内想到各种的变更例或修正例,应当理解的是这些当然也包含在本发明的技术范围内。
Claims (13)
1.一种热浸镀锌系钢板,其具备:
作为基材的热浸镀锌系钢板;和
在所述热浸镀锌系钢板的至少单面形成的表面处理层,
所述表面处理层以每单面0.2g/m2以上且2g/m2以下的范围含有粒径为5nm以上且500nm以下的选自氧化锆、氧化镧、氧化铈和氧化钕中的1种或2种以上的氧化物。
2.根据权利要求1所述的热浸镀锌系钢板,其中,所述表面处理层还以每单面的含量计按照以下所示范围含有:含磷化合物、含钒化合物、含铜化合物、含铝化合物、含硅化合物、或含铬化合物的至少任一者,
含磷化合物:以P换算为0.0g/m2以上且0.01g/m2以下,
含钒化合物:以V换算为0.0g/m2以上且0.01g/m2以下,
含铜化合物:以Cu换算为0.0g/m2以上且0.02g/m2以下,
含铝化合物:以Al换算为0.0g/m2以上且0.005g/m2以下,
含硅化合物:以Si换算为0.0g/m2以上且0.005g/m2以下,
含铬化合物:以Cr换算为0.0g/m2以上且0.01g/m2以下。
3.根据权利要求1或2所述的热浸镀锌系钢板,其中,所述选自氧化锆、氧化镧、氧化铈和氧化钕中的1种或2种以上的氧化物的粒径为10nm以上且200nm以下。
4.根据权利要求1~3中任一项所述的热浸镀锌系钢板,其中,所述选自氧化锆、氧化镧、氧化铈和氧化钕中的1种或2种以上的氧化物的含量为每单面0.4g/m2以上且1.5g/m2以下。
5.根据权利要求1~4中任一项所述的热浸镀锌系钢板,其中,所述氧化物为氧化锆或氧化镧。
6.根据权利要求1~5中任一项所述的热浸镀锌系钢板,其中,所述表面处理层还以每单面0.2g/m2以上且2g/m2以下的范围含有粒径为2nm以上且100nm以下的选自氧化钛、氧化镍和氧化锡(IV)中的1种或2种以上的氧化物。
7.根据权利要求6所述的热浸镀锌系钢板,其中,所述选自氧化钛、氧化镍和氧化锡(IV)中的1种或2种以上的氧化物的粒径为5nm以上且50nm以下。
8.根据权利要求6或7所述的热浸镀锌系钢板,其中,所述选自氧化钛、氧化镍和氧化锡(IV)中的1种或2种以上的氧化物的含量为每单面0.4g/m2以上且1.5g/m2以下。
9.根据权利要求6~8中任一项所述的热浸镀锌系钢板,其中,所述氧化物为氧化钛。
10.根据权利要求1~9中任一项所述的热浸镀锌系钢板,其中,所述表面处理层还以每单面0.2g/m2以上且5.0g/m2以下的范围含有氧化镁、氧化钙或氧化锌。
11.根据权利要求10所述的热浸镀锌系钢板,其中,所述氧化镁、氧化钙或氧化锌的粒径为5nm以上且100nm以下。
12.根据权利要求10或11所述的热浸镀锌系钢板,其中,所述氧化镁、氧化钙或氧化锌的含量为每单面0.4g/m2以上且2.5g/m2以下。
13.根据权利要求1~12中任一项所述的热浸镀锌系钢板,其为热压制用热浸镀锌系钢板。
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TWI655320B (zh) | 2019-04-01 |
TW201700788A (zh) | 2017-01-01 |
MX2017011815A (es) | 2017-12-07 |
US10549506B2 (en) | 2020-02-04 |
JP6551519B2 (ja) | 2019-07-31 |
EP3272906A4 (en) | 2018-12-05 |
US20180079174A1 (en) | 2018-03-22 |
WO2016159307A1 (ja) | 2016-10-06 |
CN107406988B (zh) | 2019-12-17 |
EP3272906A1 (en) | 2018-01-24 |
JPWO2016159307A1 (ja) | 2017-11-30 |
EP3272906B1 (en) | 2020-03-25 |
TW201842228A (zh) | 2018-12-01 |
KR20170118860A (ko) | 2017-10-25 |
KR102002238B1 (ko) | 2019-07-19 |
BR112017020271A2 (pt) | 2018-05-22 |
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