JP7332943B2 - ホットスタンプ成形体 - Google Patents
ホットスタンプ成形体 Download PDFInfo
- Publication number
- JP7332943B2 JP7332943B2 JP2021543047A JP2021543047A JP7332943B2 JP 7332943 B2 JP7332943 B2 JP 7332943B2 JP 2021543047 A JP2021543047 A JP 2021543047A JP 2021543047 A JP2021543047 A JP 2021543047A JP 7332943 B2 JP7332943 B2 JP 7332943B2
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- JP
- Japan
- Prior art keywords
- chemical conversion
- hot
- plating layer
- coating
- less
- 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.)
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- 239000000126 substance Substances 0.000 claims description 89
- 238000007747 plating Methods 0.000 claims description 84
- 229910000831 Steel Inorganic materials 0.000 claims description 67
- 239000010959 steel Substances 0.000 claims description 67
- 238000006243 chemical reaction Methods 0.000 claims description 48
- 239000000463 material Substances 0.000 claims description 43
- 238000007739 conversion coating Methods 0.000 claims description 29
- 239000011701 zinc Substances 0.000 claims description 21
- LRXTYHSAJDENHV-UHFFFAOYSA-H zinc phosphate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LRXTYHSAJDENHV-UHFFFAOYSA-H 0.000 claims description 21
- 229910000165 zinc phosphate Inorganic materials 0.000 claims description 21
- 239000000203 mixture Substances 0.000 claims description 18
- 239000013078 crystal Substances 0.000 claims description 14
- 239000012535 impurity Substances 0.000 claims description 4
- 239000010410 layer Substances 0.000 description 65
- 239000011777 magnesium Substances 0.000 description 48
- 239000011575 calcium Substances 0.000 description 35
- 239000011248 coating agent Substances 0.000 description 29
- 238000000576 coating method Methods 0.000 description 29
- 229910052749 magnesium Inorganic materials 0.000 description 28
- 238000000034 method Methods 0.000 description 25
- 238000001816 cooling Methods 0.000 description 24
- 229910052791 calcium Inorganic materials 0.000 description 22
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 19
- 238000010438 heat treatment Methods 0.000 description 17
- 238000005260 corrosion Methods 0.000 description 16
- 230000007797 corrosion Effects 0.000 description 16
- 238000004519 manufacturing process Methods 0.000 description 13
- 229910052725 zinc Inorganic materials 0.000 description 12
- 230000000694 effects Effects 0.000 description 11
- 239000003973 paint Substances 0.000 description 11
- 229910052782 aluminium Inorganic materials 0.000 description 10
- 239000011247 coating layer Substances 0.000 description 9
- 238000007654 immersion Methods 0.000 description 8
- 229910052748 manganese Inorganic materials 0.000 description 8
- 229910052804 chromium Inorganic materials 0.000 description 7
- 229910052759 nickel Inorganic materials 0.000 description 7
- 239000012071 phase Substances 0.000 description 7
- 230000007423 decrease Effects 0.000 description 6
- 229910000765 intermetallic Inorganic materials 0.000 description 6
- 229910052745 lead Inorganic materials 0.000 description 6
- 229910052718 tin Inorganic materials 0.000 description 6
- 229910052787 antimony Inorganic materials 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 5
- 229910052802 copper Inorganic materials 0.000 description 5
- 238000001704 evaporation Methods 0.000 description 5
- 230000008020 evaporation Effects 0.000 description 5
- 238000007731 hot pressing Methods 0.000 description 5
- 229910052742 iron Inorganic materials 0.000 description 5
- 229910052719 titanium Inorganic materials 0.000 description 5
- 238000004090 dissolution Methods 0.000 description 4
- 238000004070 electrodeposition Methods 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 238000009616 inductively coupled plasma Methods 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 3
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 230000002411 adverse Effects 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- KRVSOGSZCMJSLX-UHFFFAOYSA-L chromic acid Substances O[Cr](O)(=O)=O KRVSOGSZCMJSLX-UHFFFAOYSA-L 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- AWJWCTOOIBYHON-UHFFFAOYSA-N furo[3,4-b]pyrazine-5,7-dione Chemical compound C1=CN=C2C(=O)OC(=O)C2=N1 AWJWCTOOIBYHON-UHFFFAOYSA-N 0.000 description 2
- 239000003112 inhibitor Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000010791 quenching Methods 0.000 description 2
- 230000000171 quenching effect Effects 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- 229910052712 strontium Inorganic materials 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 229910018137 Al-Zn Inorganic materials 0.000 description 1
- 229910018573 Al—Zn Inorganic materials 0.000 description 1
- 229910000640 Fe alloy Inorganic materials 0.000 description 1
- 229910001335 Galvanized steel Inorganic materials 0.000 description 1
- 229910019018 Mg 2 Si Inorganic materials 0.000 description 1
- 229910000861 Mg alloy Inorganic materials 0.000 description 1
- 229910017706 MgZn Inorganic materials 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical class [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000010953 base metal Substances 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 238000011088 calibration curve Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000010960 cold rolled steel Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000002542 deteriorative effect Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 150000004673 fluoride salts Chemical class 0.000 description 1
- 150000002222 fluorine compounds Chemical class 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 239000008397 galvanized steel Substances 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- -1 zinc-aluminum-magnesium Chemical compound 0.000 description 1
Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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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- C—CHEMISTRY; METALLURGY
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- C22C18/00—Alloys based on zinc
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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
- 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
- C23C28/34—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates
- C23C28/345—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates with at least one oxide layer
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- B32B15/00—Layered products comprising a layer of metal
- B32B15/01—Layered products comprising a layer of metal all layers being exclusively metallic
- B32B15/012—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 aluminium or an aluminium alloy
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- B—PERFORMING OPERATIONS; TRANSPORTING
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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
- B32B15/043—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
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- B32B15/00—Layered products comprising a layer of metal
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- C22C—ALLOYS
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- C22C30/02—Alloys containing less than 50% by weight of each constituent containing copper
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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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- 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
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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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- 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
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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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- 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
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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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- Y10T428/12—All metal or with adjacent metals
- Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
- Y10T428/12771—Transition metal-base component
- Y10T428/12861—Group VIII or IB metal-base component
- Y10T428/12951—Fe-base component
- Y10T428/12972—Containing 0.01-1.7% carbon [i.e., steel]
- Y10T428/12979—Containing more than 10% nonferrous elements [e.g., high alloy, stainless]
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/27—Web or sheet containing structurally defined element or component, the element or component having a specified weight per unit area [e.g., gms/sq cm, lbs/sq ft, etc.]
Description
本願は、2019年08月29日に、日本に出願された特願2019-157205号に基づき優先権を主張し、その内容をここに援用する。
よって、鋼板の機械的強度を高めることにより、以前使用されていた鋼板より薄くしても機械的強度を維持又は高めることが可能な鋼板について、研究開発が行われている。このような鋼板に対する要請は、自動車製造業のみならず、様々な製造業でも同様になされている。
本発明者らが検討した結果、AlやZnを含むめっき層を有する鋼板にホットスタンプを行って得られた部材に、自動車用として一般的な化成処理であるりん酸亜鉛処理を行っても、りん酸亜鉛皮膜が形成されにくい、または形成されたとしても、さらに表面に電着塗膜等を形成した際の塗膜密着性が十分でない場合があることが分かった。
本発明は上記知見に基づいて完成され、その要旨は以下の通りである。
(2)上記(1)に記載のホットスタンプ成形体は、前記めっき層の前記化学組成が、質量%で、Al:25.00~35.00%、Mg:6.00~10.00%、の1種または2種を含有してもよい。
(3)上記(1)または(2)に記載のホットスタンプ成形体は、前記化成処理皮膜の前記片面付着量が、1.5~8.0g/m2であってもよい。
図1を参照し、本実施形態に係るホットスタンプ成形体1は、鋼からなる母材2と、母材2の表面に形成されためっき層3と、めっき層3の表面に形成された化成処理皮膜4とを備える。図1では、めっき層3と化成処理皮膜4とは母材2の片面にのみ形成されているが、両面に形成されていてもよい。
母材2は、鋼からなる。母材2は、例えば鋼板をホットスタンプして得られるホットスタンプ部材である。そのため、図1では、板形状をしているが、その形状は限定されない。
また、本実施形態に係るホットスタンプ成形体1は、めっき層3及び化成処理皮膜4が重要であり、母材2の化学組成等については特に限定されない。母材2は、適用される製品や要求される強度や板厚等によってめっき、ホットスタンプ及び化成処理に供する鋼を決定すればよい。例えば、母材としては、JIS G3193:2008に記載された熱延鋼板やJIS G3141:2017に記載された冷延鋼板を用いることができる。
[化学組成]
以下、めっき層、化成処理皮膜の化学組成に関する%は、断りがない限り質量%である。
Alは、めっき層3の耐食性を向上させるために必須な元素である。また、Al含有量が20.00%未満であると、ホットスタンプの加熱中にZn及びMgの蒸発を抑制するとともに化成処理層へのCaの供給源となる、CaとAlとを主体とした金属間化合物が、めっき層の表面に十分に生成されなくなる。その結果、めっき層3上に形成される化成処理皮膜4のスケが大きくなる。そのため、Al含有量を20.00%以上とする。好ましくは25.00%以上である。
一方、Al含有量が45.00%を超えても、ホットスタンプの加熱中に、めっき層3表面にCaとAlとを主体とした金属間化合物が生成しにくくなる。その結果、化成処理皮膜4のスケが大きくなる。そのため、Al含有量を45.00%以下とする。好ましくは35.00%以下である。
ホットスタンプ時に、めっき鋼板を加熱すると、Feが母材2からめっき層3に拡散するので、ホットスタンプ成形体1のめっき層3には必ずFeが含まれる。
Fe含有量が10.0%未満である場合、スポット溶接性、および溶着性が悪化する傾向にあるので、Fe含有量を、10.00%以上とする。
一方、Fe含有量が高すぎる場合、耐食性が悪化する傾向にあるので、Fe含有量を、45.00%以下とする。
Mgは、めっき層3の耐食性の向上に寄与する元素である。また、Mgは、ホットスタンプの加熱時に、めっき層3中のZn成分と結合して液相Znの発生を防止するので、LME割れを抑制する効果も有する。また、本実施形態に係るホットスタンプ成形体1では、Mgは化成処理皮膜4に拡散し、塗膜密着性を高める元素である。これらの効果を得るため、Mg含有量を4.50%以上とする。Mg含有量が4.50%未満であると、塗膜密着性が低下する。Mg含有量は好ましくは6.0%以上である。
一方、Mg含有量が15.00%を超えると、過度に犠牲防食が働き、めっき層3の耐食性が低下する傾向がある。また、めっき層3中に化成処理性を低下させるMg系の金属間化合物が多量に形成し、その結果、化成処理皮膜4のスケが大きくなるとともに、塗膜密着性が低下する。そのため、Mg含有量を15.00%以下とする。好ましくは10.00%以下である。
Siは、Mgとともに化合物を形成して、耐食性の向上に寄与する元素である。また、Siは、鋼板上にめっき層を形成するにあたり、鋼板表面とめっき層との間に形成される合金層が過剰に厚く形成されることを抑制して、鋼板とめっき層との密着性を高める効果を有する元素でもある。Si含有量が0.10%未満ではこれらの効果が十分に得られない。そのため、Si含有量を0.10%以上とする。
一方、Si含有量が3.00%を超えると、Mg2Si、Mg2Ca、あるいは(Mg,Ca)2Siが形成されて、化成処理皮膜4に含有されるMg含有量ならびにCa含有量が不足し、塗膜密着性が低下する。また、Si相が過剰に生成すると、耐チッピング性、耐焼付き性が低下する。そのため、Si含有量を3.00%以下とする。
本実施形態に係るホットスタンプ成形体1では、Caは化成処理皮膜4に拡散し、塗膜密着性を高める元素である。Ca含有量が0.05%未満では、化成処理皮膜4のスケが大きくなる。そのため、Ca含有量を0.05%以上とする。
一方、Ca含有量が3.00%を超えると、化成処理性を低下させるCaを主体とする金属間化合物が形成されることで、化成処理皮膜のMg含有量、Ca含有量が不足するとともにスケが大きくなり、塗膜密着性が低下する。そのため、Ca含有量を3.00%以下とする。
しかしながら、めっき層3は、上記の元素に加えて、Sb、Pb、Cu、Sn、Ti、Sr、Cr、Ni、Mnを下記の範囲で含有してもよい。これらの元素は必ずしも含有する必要がないので、下限は0%である。また、これらの元素の合計含有量は、5.00%以下であることが好ましい。
Pb:0~0.50%
Cu:0~1.00%
Sn:0~1.00%
Ti:0~1.00%
Sb、Pb、Cu、SnおよびTiは、めっき層3中でZnと置換され、MgZn2相内で固溶体を形成するが、所定の含有量の範囲内であれば、ホットスタンプ成形体1の特性に悪影響を及ぼさない。よって、これらの元素がめっき層3中に含まれていてもよい。しかしながら、それぞれの元素の含有量が過剰な場合、ホットスタンプの加熱時に、これらの元素の酸化物が析出し、ホットスタンプ成形体1の表面性状が悪化して化成処理性が低下する傾向がある。また、Pb、Snの含有量が過剰な場合には、溶着性および耐LME性も劣化する。
そのため、SbおよびPbの含有量は、それぞれ0.50%以下、Cu、SnおよびTiの含有量はそれぞれ1.00%以下とする。SbおよびPbの含有量は0.20%以下とするのが好ましい。Cu、SnおよびTiの含有量は、0.80%以下が好ましく、0.50%以下がより好ましい。
Srは、製造時にめっき浴上に形成されるトップドロスの生成を抑制するために有効な元素である。また、Srは、ホットスタンプの熱処理時に、大気酸化を抑制するので、熱処理後のめっき鋼板の色変化を抑制する元素である。そのため、Srを含有させてもよい。上記の効果を得るためには、Sr含有量は0.05%以上とするのが好ましい。
一方、Srは、含有量が過剰な場合、腐食試験において塗膜膨れ幅および流れ錆に悪影響を与える。そのため、Sr含有量は0.50%以下とする。Sr含有量は、0.30%以下とするのが好ましく、0.10%以下とするのがより好ましい。
Ni:0~1.00%
Mn:0~1.00%
Cr、NiおよびMnは、めっき鋼板においては、めっき層と母材との界面付近に濃化し、めっき層表面のスパングルを消失させるなどの効果を有する元素である。よって、Cr、NiおよびMnから選択される一種以上が、めっき層3中に含まれていてもよい。これらの効果を得る場合、Cr、NiおよびMnの含有量は、それぞれ0.01%以上とするのが好ましい。
一方、これらの元素の含有量が過剰な場合には、塗膜膨れ幅および流れ錆が大きくなり、耐食性が悪化する傾向にある。よって、Cr、NiおよびMnの含有量は、それぞれ1.00%以下とする。Cr、NiおよびMnの含有量は、それぞれ、0.50%以下とするのが好ましく、0.10%以下とするのがより好ましい。
[質量%で、Mg:5.0~50.0%、Ca:0.5~5.0%を含有するりん酸亜鉛結晶からなる]
通常、Alを含むめっき層を有する鋼材をホットスタンプして得られたホットスタンプ成形体の表面(めっき層の表面)には、主としてAl2O3からなる酸化物が形成される。めっき層表面に形成されたAl2O3は化成処理皮膜の形成を妨げるので、表面にAl2O3が形成されためっき鋼材に化成処理を行うと、ホットスタンプ成形体において、化成処理皮膜のスケの割合が大きくなる。
これに対し、本実施形態に係るホットスタンプ成形体では、後述するような方法でめっきを行うことで、化成処理に供するホットスタンプ後のめっき鋼材の表面に、Ca、Mgを主体とする酸化物皮膜が形成される。この鋼材に対し、りん酸亜鉛処理(化成処理)を行うと、化成処理皮膜にMg及びCaが拡散し、質量%で、Mg:5.0~50.0%、Ca:0.5~5.0%を含有するりん酸亜鉛結晶からなる化成処理皮膜4が形成される。図2に本実施形態に係るホットスタンプ成形体1の化成処理皮膜4の代表的な組織写真を示す。この化成処理皮膜4は、Mg:5.0~50.0%、Ca:0.5~5.0%を含有するりん酸亜鉛結晶11からなり、りん酸亜鉛結晶11は、結晶粒径が長径10μm以下、短径5μm以下の鱗片状である。また、このようなりん酸亜鉛結晶11が形成される場合、スケの割合が10%以下になる。また、Mgを含有する化成処理皮膜は、それ自体が耐食性に優れるので、Mgを含有しない化成処理皮膜に比べて塗装後密着性(塗膜密着性)の向上に寄与する。
化成処理を行う鋼材の表面にMg、Caの酸化物皮膜が十分に形成されないと、Al酸化物が生成し、化成処理皮膜4のスケが大きくなる。化成処理皮膜中のMg、Ca含有量が少ないと、化成処理皮膜の耐食性が低下するので、塗膜密着性が低下する。
一方、Mg、Ca含有量が多いと、化成処理皮膜の耐食性がかえって低下するので、塗膜密着性が低下する。
ホットスタンプの条件やめっき層の厚みによっては、合金化によってめっき層に拡散したFeが、りん酸亜鉛結晶の化成処理皮膜中に存在することがある。
化成処理皮膜4の片面付着量が0.1g/m2未満では、塗膜密着性(化成処理皮膜の表面に塗膜を形成した際の密着性)の向上効果が十分に得られない。一方、片面付着量が10g/m2を超えると、曲げ加工などを受けた際に化成処理皮膜内で亀裂を生じやすくなり、塗膜剥離の原因となる。そのため、片面付着量を0.1~10g/m2とする。好ましくは、1.5~8.0g/m2である。
蛍光X線で測定する場合は、片面のみの付着量が求められる。
本実施形態に係るホットスタンプ成形体は、製造方法に依らず、上記の特徴を有していればその効果が得られる。しかしながら、以下の工程を含む製造方法によれば安定して製造することができるので好ましい。
すなわち、本実施形態に係るホットスタンプ成形体は、
(I)鋼材をめっき浴に浸漬してめっき層を有するめっき鋼材を得るめっき工程と、
(II)めっき工程後のめっき鋼材にホットスタンプを行うホットスタンプ工程と、
(III)ホットスタンプ後のめっき鋼材に化成処理を行う化成処理工程と、
を備え、
(IV)めっき工程において、めっき浴浸漬後の冷却過程で、浴温~450℃の平均冷却速度を10℃/秒以上とし、450~350℃の平均冷却速度を7℃/秒以下とし、350~150℃の平均冷却速度を4℃/秒以下とするように、室温まで冷却する、
製造方法によって得ることができる。
[めっき浴への浸漬]
めっき工程では、原板となる鋼板等の鋼材を、めっき浴に浸漬することで、表面にめっき層を形成させる。
めっき浴への浸漬の条件については、例えば、600~940℃でめっき原板の表面を加熱還元処理し、N2ガスで空冷して鋼材の温度が浴温+20℃に到達した後、500~750℃の浴温のめっき浴に約0.2~6秒浸漬する。
浸漬時間が0.2秒未満では、めっき層が十分に形成されない場合がある。一方、浸漬時間が6秒超では、めっき層と鋼材とが過剰に合金化し、めっき層中に多量のFeが含有されることとなる。過剰のFeがめっき層に含有された場合、ホットスタンプの加熱中にZn及びMgの蒸発を抑制することが困難となる。そのため、浸漬時間が6秒超の場合には、その後の化成処理工程によって、所定の組成を有する化成処理皮膜が得られなくなり、ホットスタンプ成形体の塗膜密着性が低下する。
めっき浴は目的とするめっき層3の組成に応じて、Zn、Al、Mg及びその他の元素を含むように設定すればよい。めっき浴の組成は、例えば、Al:30.00~75.00%、Mg:4.00~17.00%、Si:0.20~2.00%を含み、必要に応じてめっき層に含有させたい任意元素を含み、残部がZnと不純物である。
浴温~450℃の平均冷却速度:10℃/秒以上
本実施形態に係るホットスタンプ成形体の製造方法では、めっき浴からめっき鋼材を引上げた後、450℃までの温度域の平均冷却速度が10℃/秒以上となるように冷却する。この温度域での平均冷却速度を10℃/秒以上とすることで、めっき鋼材の表面にAl酸化物が形成されることを抑制できる。
上記冷却に引き続き、450℃~350℃の温度域の平均冷却速度が7℃/秒以下となるように冷却を行う。
この温度域での冷却速度を低くして凝固組織を制御することで、引き続いて行われるホットスタンプ工程において、表面にAl含有量の少ない(例えば10%以下)、Mg、Caの酸化物が形成される。その結果、化成処理を行った場合に、スケが少なく、Mg、Caを含む化成処理皮膜が得られる。
また、亜鉛系のめっき層の場合、ホットスタンプによってZn(亜鉛)が蒸発することが懸念されるが、上記の通り制御された凝固組織では、詳細な機構は明らかでないものの、蒸気圧が高い元素であるZn及びMgの蒸発を抑制する効果を有するAl、Zn、Ca及び/またはSiを含有する金属間化合物がめっき層の表面近傍に優先的に生成することで、引き続き行われるホットスタンプの加熱時のZn及びMgの蒸発を抑制することができる。
上記冷却に引き続き、350℃~150℃の平均冷却速度を4℃/秒以下とすると、凝固組織に含有されるAlとZnとの固溶体がAl相とZn相とに分離することでめっき層の融点が低下し、Al、Zn、Ca及び/またはSiを含有する金属間化合物がホットスタンプ加熱中に溶融状態にあるめっき層の表面に移動しやすくなる。その結果として、より効率的にZn及びMgの蒸発を抑制することが可能となり、MgとCaとを含有した化成処理皮膜の形成が可能となる。
ただし、350℃~150℃の平均冷却速度が4℃/秒以下であっても、一部の温度域の冷却速度が速いと好ましい金属組織が得られなくなる。そのため、350℃~150℃の平均冷却速度が4℃/秒以下であって、350℃~250℃の平均冷却速度が4℃/秒以下、かつ250~150℃の平均冷却速度が4℃/秒以下であることが好ましい。
めっき工程後のめっき鋼材(母材とその表面上に形成されためっき層とを有する鋼材)にホットスタンプを行う。
ホットスタンプの条件は限定されないが、例えば、めっき鋼板を750~1200℃に加熱し、0~8分保持した後、室温程度の温度にある平板金型でめっき鋼板を挟み込んで急冷する方法が挙げられる。
ホットスタンプ後の成形体に対して、化成処理を行う。化成処理については限定されず、公知のりん酸亜鉛処理とすればよい。
めっき浴浸漬前、酸素濃度20ppm以下の炉内においてN2-5%H2ガス雰囲気にて800℃でめっき原板表面を加熱還元処理し、N2ガスで空冷して浸漬板温度が浴温+20℃に到達した後、表2に示す浴温のめっき浴に約3秒浸漬した。めっき浴浸漬後、引上速度20~200mm/秒で引上げた。
引上げ時、N2ワイピングガスでめっき付着量を表2のように制御した。めっき浴から鋼板を引上げた後、表2に示す条件でめっき浴温から室温まで冷却した。
作製しためっき鋼板に対し、ホットスタンプ加熱と金型急冷とを施した。加熱条件は、900℃の加熱炉中にめっき鋼板を挿入し、めっき鋼板の温度が炉内温度-10℃に到達してから0~8分保定した後、室温程度の温度にある平板金型でめっき鋼板を挟み込み、急冷することで成形品を作製した。
上述した方法で調査した結果、ホットスタンプ後のめっき層の化学組成は、表1に示す通りであった。
No.31は、市販の合金化溶融亜鉛めっき鋼板に対しホットスタンプを行った。
化成処理皮膜を調査するため、作製したサンプルを20%クロム酸で溶解し、化成処理皮膜が溶解した溶液をICP分析し、化成処理皮膜の平均組成を測定した。また、溶解前後の重量変化から片面当たり付着量を測定した。
また、化成処理皮膜が形成されためっき鋼板の表面をSEM観察することで、化成処理皮膜のスケの割合(面積%)を測定した。その際、SEM観察視野において、鋼板が露出した領域の面積率をスケの割合と定義した。スケの割合が10面積%以下であれば、スケが抑制されていると判断した。
なお、化成処理後のサンプルを25mm(C方向)×15mm(L方向)に切断し、サンプル表面のSEM像を得た。このSEM像に基づいて、りん酸亜鉛結晶の形状を観察した。その結果、発明例では、りん酸亜鉛結晶の、結晶粒径が長径10μm以下、短径5μm以下の鱗片状であることが確認された。
ホットスタンプ成形体の塗膜密着性は、上述のようにサンプル50×100mmを、りん酸亜鉛処理(SD5350システム:日本ペイント・インダストリアルコーディング社製規格)に従い実施した後、電着塗装(PN110パワーニクスグレー-:日本ペイント・インダストリアルコーディング社製規格)を、塗膜厚が20μmとなるように実施して、焼き付け温度150℃、20分で焼き付けを行った後、地鉄に到達するクロスカット傷(40×√2mm 2本)を付けた塗装めっき鋼板を、55℃の5%NaCl塩水に1000h浸漬した後、テープ剥離により電着塗膜を剥離させ、剥離が生じた部分の面積率と赤錆発生状況とから評価した。
剥離面積が5%以下の場合は「AA」、剥離面積が5%超~10%の場合は、「A」、剥離面積が10%超の場合または赤錆が生じていた場合は「B」とした。
図2は、表1~表3中、No.10のSEM像(BSE像)である。サンプル表面にはりん酸亜鉛結晶が形成されており、りん酸亜鉛結晶が形成されていないスケは見られなかった。ICP分析した結果、りん酸亜鉛結晶にはMgが33.5%、Caが2.6%含有されていた。
一方、めっき層の化学組成が本発明範囲外、または、製造方法が好ましくなかった比較例では、化成処理皮膜の組成及び/またはスケの面積率が大きくなり、塗膜密着性が低かった。例えば、No.12では、図3に示すように、りん酸亜鉛皮膜13にはCa、Mgが含まれず、またスケ12も多く見られた。
また、市販の合金化溶融亜鉛めっき鋼板に対しホットスタンプを行ったNo.28でも塗膜密着性は劣位であった。
2 母材
3 めっき層
4 化成処理皮膜
11 MgとCaとを含有するりん酸亜鉛結晶
12 スケ
13 MgとCaとを含有しないりん酸亜鉛結晶
Claims (3)
- 鋼からなる母材と、
前記母材の表面に形成されためっき層と、
前記めっき層の表面に形成された化成処理皮膜と、
を備え、
前記めっき層の化学組成が、質量%で、
Al:20.00~45.00%、
Fe:10.00~45.00%、
Mg:4.50~15.00%、
Si:0.10~3.00%、
Ca:0.05~3.00%、
Sb:0~0.50%、
Pb:0~0.50%、
Cu:0~1.00%、
Sn:0~1.00%、
Ti:0~1.00%、
Sr:0~0.50%、
Cr:0~1.00%、
Ni:0~1.00%、
Mn:0~1.00%、
を含み、残部がZnおよび不純物であり、
前記化成処理皮膜が、質量%で、Mg:5.0~50.0%、Ca:0.5~5.0%を含有するりん酸亜鉛結晶からなり、
前記化成処理皮膜の片面付着量が、0.1~10.0g/m2である、
ことを特徴とするホットスタンプ成形体。 - 前記めっき層の前記化学組成が、質量%で、
Al:25.00~35.00%、
Mg:6.00~10.00%、
の1種または2種を含有することを特徴とする、
請求項1に記載のホットスタンプ成形体。 - 前記化成処理皮膜の前記片面付着量が、1.5~8.0g/m2である、
ことを特徴とする請求項1または2に記載のホットスタンプ成形体。
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