JP2009293078A - AUTOMOTIVE MEMBER HAVING EXCELLENT CORROSION RESISTANCE AFTER COATING AND Al-PLATED STEEL SHEET FOR HOT PRESS - Google Patents
AUTOMOTIVE MEMBER HAVING EXCELLENT CORROSION RESISTANCE AFTER COATING AND Al-PLATED STEEL SHEET FOR HOT PRESS Download PDFInfo
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本発明は、塗装後耐食性に優れた自動車部材及び熱間プレス用Ａｌめっき鋼板に関し、特に、塗装後耐食性及び生産性に優れるホットプレス用Ａｌめっき鋼板及びそれにより製造された自動車部材に関する。 TECHNICAL FIELD The present invention relates to an automobile member and hot-pressed Al-plated steel sheet having excellent post-painting corrosion resistance, and more particularly to an Al-plated steel sheet for hot press having excellent post-painting corrosion resistance and productivity and an automobile member produced thereby.
近年、自動車用鋼板の用途（例えば、自動車のピラー、ドアインパクトビーム、バンパービーム等）などにおいて、高強度と高成形性を両立する鋼板が望まれており、これに対応するものの１つとして、残留オーステナイトのマルテンサイト変態を利用したＴＲＩＰ（Ｔｒａｎｓｆｏｒｍａｔｉｏｎ Ｉｎｄｕｃｅｄ Ｐｌａｓｔｉｃｉｔｙ）鋼がある。このＴＲＩＰ鋼により、成形性の優れた１０００ＭＰａ級程度の強度を有する高強度鋼板を製造することは可能であるが、さらに高強度、例えば１５００ＭＰａ以上といった超高強度鋼で成形性を確保することは困難である。 In recent years, in steel plate applications for automobiles (for example, automobile pillars, door impact beams, bumper beams, etc.) and the like, steel plates that have both high strength and high formability have been desired. There is TRIP (Transformation Induced Plasticity) steel using martensitic transformation of retained austenite. With this TRIP steel, it is possible to produce a high-strength steel sheet having excellent formability and a strength of about 1000 MPa, but it is possible to secure formability with ultra-high-strength steel having higher strength, for example, 1500 MPa or more. Have difficulty.
このような状況で、高強度及び高成形性を両立するものとして最近注目を浴びているのが、ホットプレス（熱間プレス、ホットスタンプ、ダイクエンチ、プレスクエンチ等とも呼称される。）である。このホットプレスは、鋼板を８００℃以上のオーステナイト域で加熱した後に熱間で成形することにより高強度鋼板の成形性を向上させ、成形後の冷却により焼きを入れて所望の材質を得るというものである。 Under such circumstances, hot press (also referred to as hot pressing, hot stamping, die quenching, press quenching, etc.) has recently been attracting attention as having both high strength and high formability. This hot press improves the formability of a high-strength steel sheet by heating it in an austenite region at 800 ° C. or higher and then forming it hot, and after it is formed, it is baked to obtain a desired material. It is.
ホットプレスは、超高強度の部材を成形する方法として有望であるが、通常は大気中で鋼板を加熱する工程を有しており、この際、鋼板表面に酸化物（スケール）が生成するため、スケールを除去する工程が必要であった。ところが、このような後工程には、スケールの除去能や環境負荷等の観点からの対応策の必要性等の問題があった。 Hot press is promising as a method of forming ultra-high strength members, but usually has a step of heating the steel plate in the atmosphere, and at this time, oxide (scale) is generated on the steel plate surface. The process of removing the scale was necessary. However, such post-processes have problems such as the necessity of countermeasures from the viewpoints of scale removal ability and environmental load.
これを改善する技術として、ホットプレス用の鋼板としてＡｌめっき鋼板を使用することにより、加熱時のスケールの生成を抑制する技術が提案されている（例えば、特許文献１〜３を参照）。
しかしながら、上記特許文献１〜３に記載された技術は、塗装後耐食性という観点で、十分でなく、更なる改善が求められていた。
However, the techniques described in
すなわちこれらの公知例によれば、成形時の合金化しためっき層の剥離が問題とされ、これを抑制するために拡散を進行させるような技術が開示されていたが、更なる検討の結果、このような条件においては、塗装後耐食性が低下することが判明した。これは拡散を進行させることで合金化しためっき層中のＦｅ濃度が高まり、耐食性に寄与するＡｌ濃度が低下したためと推定される。 That is, according to these known examples, peeling of the alloyed plating layer at the time of molding was a problem, and a technique for proceeding diffusion in order to suppress this was disclosed. Under such conditions, it has been found that the corrosion resistance after coating decreases. This is presumably because the Fe concentration in the alloyed plating layer was increased by the progress of diffusion, and the Al concentration contributing to corrosion resistance was decreased.
また、特許文献４には、酸化物重量が５００ｍｇ／ｄｍ２以下である電着塗装用アルミニウムめっき構造部材が開示されている。しかし、酸化物重量が５００ｍｇ／ｄｍ２を酸化膜厚さに換算すると約１３μｍになるが、これほど酸化膜が厚いと塗料と反応しない酸化膜が厚く残存してしまい、塗膜が剥離しやすい場合があることがあった。 Patent Document 4 discloses an aluminum plating structural member for electrodeposition coating having an oxide weight of 500 mg / dm 2 or less. However, when the oxide weight is converted to an oxide film thickness of 500 mg / dm 2 , it becomes about 13 μm. However, when the oxide film is so thick, the oxide film that does not react with the paint remains thick and the coating film is easily peeled off. There was a case.
そこで、本発明は、このような問題に鑑みてなされたもので、塗装後耐食性に優れた自動車部材及び熱間プレス用Ａｌめっき鋼板を提供することを課題とする。 Then, this invention is made | formed in view of such a problem, and makes it a subject to provide the automotive member excellent in the corrosion resistance after coating, and the Al plating steel plate for hot press.
本発明者らは、上記課題を解決するために鋭意研究を重ねた結果、ホットプレス工程直前の加熱条件を適正化することで塗装後耐食性を確保できることを見出し、このような知見に基づいて本発明を完成するに至った。 As a result of intensive studies to solve the above problems, the present inventors have found that post-coating corrosion resistance can be ensured by optimizing the heating conditions immediately before the hot press process. The invention has been completed.
すなわち、本発明の要旨とするところは、特許請求の範囲に記載した通りの下記内容である。
（１）鋼成分として質量％で、Ｃ：０．１〜０．４％、Ｓｉ：０．０１〜０．６％、Ｍｎ：０．５〜３％、Ｔｉ：０．０１〜０．１％、Ｂ：０．０００１〜０．０１％を含有し、体積％で９０％以上がマルテンサイトである鋼材の表面に、複数の相からなるＡｌ−Ｆｅ金属間化合物層を有し、更にその表面に厚みが０．０５〜１μｍの酸化膜を有し、Ａｌ−Ｆｅ金属間化合物層と鋼材の界面にＡｌを含有し厚みが２．５〜１０μｍのｂｃｃ層を有することを特徴とする、塗装後耐食性に優れた自動車部材。
（２）鋼成分として質量％で、Ｃ：０．１〜０．４％、Ｓｉ：０．０１〜０．６％、Ｍｎ：０．５〜３％、Ｔｉ：０．０１〜０．１％、Ｂ：０．０００１〜０．０１％を含有し、残部がＦｅ及び不可避的不純物からなる鋼板の表面に片面当たり２０〜１００ｇ／m2のＡｌめっきを施し、更にその表面に０．１〜１ｇ／m2の油を塗布したことを特徴とする、熱間プレス用Ａｌめっき鋼板。
したことを特徴とする、熱間プレス用Ａｌめっき鋼板。
That is, the gist of the present invention is the following contents as described in the claims.
(1) Mass% as a steel component, C: 0.1-0.4%, Si: 0.01-0.6%, Mn: 0.5-3%, Ti: 0.01-0.1 %, B: 0.0001 to 0.01%, and 90% or more by volume% of the steel material having martensite has an Al—Fe intermetallic compound layer composed of a plurality of phases, It has an oxide film with a thickness of 0.05 to 1 μm on the surface, contains Al at the interface between the Al—Fe intermetallic compound layer and the steel material, and has a bcc layer with a thickness of 2.5 to 10 μm, Automotive parts with excellent corrosion resistance after painting.
(2) By mass% as a steel component, C: 0.1 to 0.4%, Si: 0.01 to 0.6%, Mn: 0.5 to 3%, Ti: 0.01 to 0.1 %, B: 0.0001 to 0.01%, with the balance being Fe and unavoidable impurities, the surface of the steel plate is subjected to Al plating of 20 to 100 g / m 2 per side, and further 0.1 to the surface. An Al-plated steel sheet for hot pressing, characterized in that ˜1 g / m 2 of oil is applied.
A hot-pressed Al-plated steel sheet characterized by the above.
本発明によれば、塗装後耐食性に優れ、かつ強度の高い自動車用部材及びそれに用いるホットプレス用Ａｌめっき鋼板を提供することができるなど、産業上有用な著しい効果を奏する。 ADVANTAGE OF THE INVENTION According to this invention, there exists an industrially useful remarkable effect, such as being able to provide the automotive member excellent in corrosion resistance after coating, and high intensity | strength, and the Al-plated steel plate for hot presses used for it.
以下に添付図面を参照しながら、本発明の好適な実施の形態について詳細に説明する。
［本発明に係るホットプレス用Ａｌめっき鋼材の概要］
上述したように、上記特許文献１〜３に記載された技術では、成形時のめっきの脱離を抑制することに着目し、これにより優れた塗装後耐食性が得られるとしているが、実際にはめっきの脱離による耐食性低下はこの材料においては顕著でなく、寧ろ脱離が多少起こりえても、合金化しためっき層中のＡｌ濃度を最大限高く保つことがより重要であるとの結論を得た。
Exemplary embodiments of the present invention will be described below in detail with reference to the accompanying drawings.
[Outline of Al-plated steel for hot press according to the present invention]
As described above, the techniques described in
ここで、Ａｌめっき鋼材を加熱することにより得られる合金層の構造について説明する。なお、図１は、Ａｌめっき鋼板を加熱合金化した後の断面組織の構造例を示す光学顕微鏡写真である。 Here, the structure of the alloy layer obtained by heating the Al-plated steel material will be described. FIG. 1 is an optical micrograph showing a structural example of a cross-sectional structure after heat-alloying an Al-plated steel sheet.
図１に示すように、Ａｌめっき鋼板を加熱合金化した後のＦｅ−Ａｌ合金層は、一般に５層構造となることが多い。これら５層を図１では、めっき鋼板表面から順に、１層〜５層で表している。第１層、第３層の層中のＡｌ濃度は約５０質量％、第２層中のＡｌ濃度は約３０質量％、第４層、第５層中のＡｌ濃度はそれぞれ１５〜３０質量％、１〜１５質量％の幅を持つ組成となる。残部はＦｅ及びＳｉである。第４層と第５層の界面付近にボイドの生成が観察されることもある。なお、第５層の下部の組織は鋼素地であり、マルテンサイトを主体とする焼入組織となっている。 As shown in FIG. 1, the Fe—Al alloy layer after heat-alloying an Al-plated steel sheet generally has a five-layer structure in many cases. In FIG. 1, these five layers are represented by 1 to 5 layers in order from the surface of the plated steel sheet. The Al concentration in the first and third layers is about 50% by mass, the Al concentration in the second layer is about 30% by mass, and the Al concentrations in the fourth and fifth layers are 15 to 30% by mass, respectively. The composition has a width of 1 to 15% by mass. The balance is Fe and Si. Void formation may be observed near the interface between the fourth layer and the fifth layer. In addition, the structure below the fifth layer is a steel base, which is a hardened structure mainly composed of martensite.
図２に、Ｆｅ−Ａｌの二元系状態図を示す。この図２を参照すれば、第１層、第３層はＦｅＡｌ２を主成分とし、第４層、第５層はそれぞれＦｅＡｌ、αＦｅに対応するものと判断できる。また、第２層はＦｅ−Ａｌ二元系状態図から説明できないＳｉを含有する層でその詳細な組成は明らかではないが、本発明者らは、ＦｅＡｌ２とＦｅ−Ａｌ−Ｓｉ化合物が微細に混じりあったようなものであると推定している。 FIG. 2 shows a binary phase diagram of Fe—Al. Referring to FIG. 2, it can be determined that the first layer and the third layer have FeAl 2 as a main component, and the fourth layer and the fifth layer correspond to FeAl and αFe, respectively. In addition, the second layer is a layer containing Si that cannot be explained from the Fe—Al binary phase diagram, and its detailed composition is not clear, but the present inventors have found that the FeAl 2 and Fe—Al—Si compounds are fine. It is presumed that it was mixed.
本願で規定するＡｌを含有するｂｃｃ層とは、ここで言う第５層に相当する。この層は、Ａｌを固溶したαＦｅで、Ａｌはフェライト安定化元素であるため、Ａｌめっき層よりＡｌが拡散した結果としてホットプレス工程の加熱時にオーステナイト変態しなかったものと解釈できる。この層の厚みはＡｌめっき層から拡散するＡｌ量に依存し、Ａｌめっき層から拡散するＡｌ量はホットプレス工程の熱履歴に依存するため、結果としてこの層の厚みはホットプレスでの熱履歴をよく反映している。 The bcc layer containing Al specified in the present application corresponds to the fifth layer referred to herein. This layer is αFe in which Al is dissolved, and since Al is a ferrite stabilizing element, it can be interpreted that austenite transformation did not occur during heating in the hot press process as a result of Al diffusion from the Al plating layer. The thickness of this layer depends on the amount of Al diffused from the Al plated layer, and the amount of Al diffused from the Al plated layer depends on the thermal history of the hot press process, and as a result, the thickness of this layer is the thermal history of the hot press. Is well reflected.
本願において、このＡｌを含有するｂｃｃ層厚みを２．５〜１０μｍに限定するものとする。これは即ちホットプレス工程における鋼板への熱負荷をある一定の範囲に限定することに相当する。熱履歴は昇温、保定、降温の３ステップ、あるいはこれらの複合から成るが、詳細な履歴は規定せず、熱負荷のみを規定する。塗装後耐食性に影響するのは、結果として生成した合金層構造に依存するためである。このような被覆層の組成や結晶構造は、電子線マイクロアナライザ（ＥＰＭＡ）、走査型電子顕微鏡−エネルギー分散型Ｘ線分析装置（ＳＥＭ−ＥＤＳ）、透過型電子顕微鏡（ＴＥＭ）等を用いて分析することにより特定することができる。 In the present application, the thickness of the bcc layer containing Al is limited to 2.5 to 10 μm. This corresponds to limiting the heat load on the steel plate in the hot pressing process to a certain range. The thermal history is composed of three steps of temperature rising, holding, and temperature falling, or a combination of these, but the detailed history is not defined, and only the thermal load is defined. The influence on post-coating corrosion resistance is due to the dependence on the resulting alloy layer structure. The composition and crystal structure of such a coating layer are analyzed using an electron beam microanalyzer (EPMA), a scanning electron microscope-energy dispersive X-ray analyzer (SEM-EDS), a transmission electron microscope (TEM), or the like. Can be specified.
Ａｌを含有するｂｃｃ層厚みが２．５μｍ以下では、Ａｌめっきと鋼板との拡散が十分に進行せず、金属間化合物に変化しないＡｌ層が表面に残存する懸念がある。表面に金属間化合物に変化しないＡｌ層が残存すると、スポット溶接性、塗装後耐食性を大きく劣化させる。これはＡｌ自体が電極の銅と反応しやすいこと、あるいはＡｌが塩害環境において優先的に腐食して塗膜膨れが起こりやすくなるためである。 When the thickness of the bcc layer containing Al is 2.5 μm or less, the diffusion between the Al plating and the steel sheet does not proceed sufficiently, and there is a concern that an Al layer that does not change to an intermetallic compound remains on the surface. If an Al layer that does not change to an intermetallic compound remains on the surface, spot weldability and post-coating corrosion resistance are greatly degraded. This is because Al itself easily reacts with the copper of the electrode, or Al preferentially corrodes in a salt-damaged environment and the coating bulges easily.
一方で１０μｍを超えるような場合には、鋼板への熱負荷が大きいことを意味する。図１の５層構造において、第１、３層のＡｌ濃度は約５０％と高く、第２、４、５層のＡｌ濃度は３０％以下と低い。加熱によりＦｅとＡｌの相互拡散が進行すると、表層のＦｅ濃度は高まり、第１、３層のＡｌ濃度の高い層が厚みを減じ、替わって第２、４、５層のＡｌ濃度の低い層の厚みが増大する。図１において、第５層の厚みは１５μｍ程度に成長し、このときには第１、３層の厚みは全体の半分以下まで減じている。先述したようにこの合金層の塗装後耐食性はＡｌで確保されているもので、このＡｌ量の高い第１、３層の厚みが塗装後耐食性に大きく寄与する。従ってＡｌを含有するｂｃｃ層、つまり５層が１０μｍ以上に成長するような場合、第１、３層厚みが減じて塗装後耐食性の確保が困難となる。 On the other hand, when exceeding 10 micrometers, it means that the heat load to a steel plate is large. In the five-layer structure of FIG. 1, the Al concentration of the first and third layers is as high as about 50%, and the Al concentration of the second, fourth, and fifth layers is as low as 30% or less. When interdiffusion of Fe and Al proceeds by heating, the Fe concentration in the surface layer increases, and the first and third layers with high Al concentration decrease in thickness, and instead, the second, fourth, and fifth layers with low Al concentration. Increases in thickness. In FIG. 1, the thickness of the fifth layer grows to about 15 μm. At this time, the thickness of the first and third layers is reduced to less than half of the whole. As described above, the corrosion resistance after painting of this alloy layer is ensured by Al, and the thickness of the first and third layers having a high Al content greatly contributes to the corrosion resistance after painting. Accordingly, when the bcc layer containing Al, that is, five layers grow to 10 μm or more, the thickness of the first and third layers is reduced, making it difficult to ensure corrosion resistance after coating.
４層は図２でＦｅＡｌに対応する。ＦｅＡｌはｂｃｃ構造のＦｅの一部をＡｌで置換した構造に相当し、ｂｃｃ構造と構造的な親和性が高い。従って第４層の厚みも第５層の厚みと相関が高く、通常第４層の厚みは第５層の１／４〜１／５程度となる。 The four layers correspond to FeAl in FIG. FeAl corresponds to a structure in which part of Fe in the bcc structure is substituted with Al, and has a high structural affinity with the bcc structure. Therefore, the thickness of the fourth layer is also highly correlated with the thickness of the fifth layer, and the thickness of the fourth layer is usually about ¼ to の of that of the fifth layer.
なお、本願発明はＡｌ−Ｆｅ金属間化合物の表面の酸化膜厚みも規定する。ホットプレス工程における鋼板熱負荷により当然表面には酸化膜が生成するが、この厚みも塗料密着性に寄与し、結果として塗装後耐食性に影響するためである。酸化膜厚みは鋼板熱履歴に加え、雰囲気に依存する。加熱時の雰囲気としては、大気、窒素、燃焼ガス等がありえ、酸化濃度が高い方が、熱負荷が高い方が酸化膜は成長する。 The present invention also defines the thickness of the oxide film on the surface of the Al—Fe intermetallic compound. This is because an oxide film is naturally formed on the surface due to the thermal load of the steel sheet in the hot pressing process, but this thickness also contributes to the adhesion of the paint and consequently affects the corrosion resistance after painting. The oxide film thickness depends on the atmosphere in addition to the thermal history of the steel sheet. The atmosphere during heating can be air, nitrogen, combustion gas, etc., and the oxide film grows when the oxidation concentration is higher and the heat load is higher.
酸化膜厚みが０．０５に満たないことは熱負荷が極端に小さいことを意味し、Ａｌ−Ｆｅ合金層が表面まで形成されていない可能性がある。このときには塗装後耐食性、スポット溶接性が低下する。また１μｍを超える酸化膜が生成すると、電着塗装時に塗膜欠陥を形成したり、電着塗装の密着性が低下したりするため、望ましくない。このため酸化皮膜厚はこの範囲とする。 An oxide film thickness of less than 0.05 means that the heat load is extremely small, and there is a possibility that the Al—Fe alloy layer is not formed up to the surface. At this time, corrosion resistance after coating and spot weldability are lowered. If an oxide film exceeding 1 μm is formed, a coating film defect is formed during electrodeposition coating, and adhesion of the electrodeposition coating is lowered, which is not desirable. For this reason, the oxide film thickness is within this range.
Ａｌ−Ｆｅ合金層表面の粗度はＲａとして１〜３μｍを示す。Ａｌめっきの付着量にも依存するが、Ａｌめっき段階よりも粗度は大きくなる傾向にある。本発明は粗度については特に規定はしない。 The roughness of the Al—Fe alloy layer surface is 1 to 3 μm as Ra. Although depending on the adhesion amount of the Al plating, the roughness tends to be larger than that in the Al plating stage. In the present invention, the roughness is not particularly specified.
以下、上述したような被覆層を有するホットプレス用のめっき鋼材の製造に用いられる本発明に係るＡｌめっき鋼材の構成について詳細に説明する。
（鋼材について）
ホットプレスが金型によるプレスと焼入を同時に行うものであることから、本発明に係るホットプレス鋼材としては、焼入されやすい成分である必要がある。具体的には、鋼板中の鋼成分として、質量％で、Ｃ：０．１〜０．４％、Ｓｉ：０．０１〜０．６％、Ｍｎ：０．５〜３％、Ｔｉ：０．０１〜０．１％、Ｂ：０．０００１〜０．０１％であることが好ましい。Ｃ量については、焼入性の向上という観点から０．１％以上であることが好ましく、また、Ｃ量が多過ぎると鋼板の靭性の低下が著しくなるため、０．４質量％以下であることが好ましい。また、Ｓｉを０．６％超添加するとＡｌめっき性が低下し、０．０１％未満とすると疲労特性が劣るため好ましくない。また、Ｍｎは焼入性に寄与する元素で０．５％以上の添加が有効であるが、焼入後の靭性の低下という観点からは３％を超えることは好ましくない。また、Ｔｉはアルミめっき後の耐熱性を向上させる元素で０．０１％以上の添加が有効であるが、過剰に添加するとＣやＮと反応して鋼板強度を低下させてしまうため、０．１％を超えることは好ましくない。また、Ｂは焼入性に寄与する元素で０．０００１％以上の添加が有効であるが、熱間での割れの懸念があるため、０．０１％を超えることは好ましくない。また、鋼板中の成分として、他に、Ｐ、Ｓ、Ａｌ、Ｎ、Ｍｏ、Ｃｒ、Ｎｂ、Ｎｉ、Ｃｕ、Ｖ、Ｓｎ、Ｓｂ等が含有されうる。好ましい範囲は、質量％で、Ｐ：０．０５％以下、Ｓ：０．０２％以下、Ａｌ：０．１％以下、Ｎ：０．０１％以下、Ｍｏ：０．５％以下、Ｃｒ：２％以下、Ｎｂ：０．１％以下、Ｎｉ：１％以下、Ｃｕ：１％以下、Ｖ：０．１％以下、Ｓｎ，Ｓｂ：０．１％以下であり、残部はＦｅ及び不可避的不純物からなる。
（Ａｌめっきについて）
本発明に係るＡｌめっき鋼材のめっきの方法については特に限定するものでなく、溶融めっき法を初めとして電気めっき法、真空蒸着法、クラッド法等が可能である。現在工業的に最も普及しているのは溶融めっき法であり、通常、めっき浴として、Ａｌに３質量％〜１５質量％のＳｉを含有するものを使用することができ、これに不可避的不純物のＦｅ等が混入している。これ以外の添加元素として、Ｍｎ、Ｃｒ、Ｍｇ、Ｔｉ、Ｚｎ、Ｓｂ、Ｓｎ、Ｃｕ、Ｎｉ、Ｃｏ、Ｉｎ、Ｂｉ、ミッシュメタル等があり得るが、めっき層がＡｌを主体とする限り、適用可能である。Ｚｎ、Ｍｇの添加は赤錆を発生し難くするという意味で有効であるが、蒸気圧の高いこれら元素の過剰な添加はＺｎ、Ｍｇのヒューム発生、表面へのＺｎ、Ｍｇ起因の粉体状物質の生成等があり、Ｚｎ：６０質量％以上、Ｍｇ：１０質量％以上の添加は好ましくない。
Hereinafter, the configuration of the Al-plated steel material according to the present invention used for manufacturing a hot-press plated steel material having the above-described coating layer will be described in detail.
(About steel)
Since hot pressing is performed simultaneously with pressing with a mold and quenching, the hot-pressed steel material according to the present invention needs to be a component that is easily quenched. Specifically, as steel components in the steel sheet, in mass%, C: 0.1 to 0.4%, Si: 0.01 to 0.6%, Mn: 0.5 to 3%, Ti: 0 0.01 to 0.1% and B: 0.0001 to 0.01% are preferable. The amount of C is preferably 0.1% or more from the viewpoint of improving hardenability, and if the amount of C is too much, the toughness of the steel sheet is remarkably lowered, so that it is 0.4% by mass or less. It is preferable. Further, if Si is added in excess of 0.6%, the Al plating property is lowered, and if it is less than 0.01%, the fatigue characteristics are inferior, which is not preferable. Mn is an element that contributes to hardenability, and it is effective to add 0.5% or more, but it is not preferable to exceed 3% from the viewpoint of lowering toughness after quenching. Ti is an element that improves the heat resistance after aluminum plating, and it is effective to add 0.01% or more. However, if it is added excessively, it reacts with C and N to lower the steel sheet strength. It is not preferable to exceed 1%. B is an element that contributes to hardenability, and it is effective to add 0.0001% or more. However, since there is a concern of hot cracking, it is not preferable to exceed 0.01%. In addition, P, S, Al, N, Mo, Cr, Nb, Ni, Cu, V, Sn, Sb and the like can be contained as components in the steel plate. Preferred ranges are% by mass, P: 0.05% or less, S: 0.02% or less, Al: 0.1% or less, N: 0.01% or less, Mo: 0.5% or less, Cr: 2% or less, Nb: 0.1% or less, Ni: 1% or less, Cu: 1% or less, V: 0.1% or less, Sn, Sb: 0.1% or less, the balance being Fe and inevitable Consists of impurities.
(About Al plating)
The method for plating the Al-plated steel material according to the present invention is not particularly limited, and electroplating, vacuum deposition, cladding, and the like including hot dipping are possible. Currently, the most widely used industrially is the hot dipping method. Usually, a plating bath containing 3% by mass to 15% by mass of Si can be used as an inevitable impurity. Fe and the like are mixed. Other additive elements may be Mn, Cr, Mg, Ti, Zn, Sb, Sn, Cu, Ni, Co, In, Bi, Misch metal, etc., but as long as the plating layer is mainly Al. Is possible. Addition of Zn and Mg is effective in terms of making red rust unlikely to occur, but excessive addition of these elements having a high vapor pressure causes generation of fumes of Zn and Mg, Zn on the surface, and powdery substances derived from Mg The addition of Zn: 60% by mass or more and Mg: 10% by mass or more is not preferable.
また、本発明において、Ａｌめっきのめっき前処理、後処理等については特に限定するものではない。めっき前処理としてＮｉ、Ｃｕ、Ｃｒ、Ｆｅプレめっき等もありうるが、これも適用可能である。また、めっき後処理としては一次防錆、潤滑性を目的としてクロメート処理、樹脂被覆処理等を施してもよい。ただし、クロメート処理については、近年の６価クロム規制を考慮すると、電解クロメート等の３価の処理皮膜が好ましい。その他、無機系のクロメート以外の後処理も適用可能である。潤滑性を付与するため、アルミナ、シリカ、ＭｏＳ２等を用いて予め表面処理することも可能である。 Moreover, in this invention, it does not specifically limit about the plating pre-processing and post-processing of Al plating. Ni, Cu, Cr, Fe pre-plating and the like may be used as the plating pretreatment, but this is also applicable. Further, as a post-plating treatment, chromate treatment, resin coating treatment, or the like may be performed for the purpose of primary rust prevention and lubricity. However, with regard to the chromate treatment, a trivalent treatment film such as electrolytic chromate is preferable in consideration of recent hexavalent chromium regulations. In addition, post-treatment other than inorganic chromate is also applicable. In order to impart lubricity, it is also possible to perform surface treatment in advance using alumina, silica, MoS 2 or the like.
本発明に係るＡｌめっき鋼材の、Ａｌめっきの付着量について説明する。通常のＡｌめっき鋼材の付着量は両面で６０〜２００ｇ／m2程度とされており、本発明においてもこの程度の付着量が適している。但し、塗装後耐食性がＡｌに依存する以上、付着量が多い方が耐食性優位であることは自明であり、炉加熱を使用する場合には望ましくは１２０〜１８０ｇ／m2である。しかし加熱方法によってはこれ以下の付着量でも塗装後耐食性を確保しうる場合もあり、２０℃／秒以上の急速加熱を適用する前提においては、６０ｇ／m2以上で塗装後耐食性を確保しうる。 The amount of Al plating adhesion of the Al plated steel material according to the present invention will be described. The amount of adhesion of a normal Al-plated steel material is about 60 to 200 g / m 2 on both sides, and this amount of adhesion is also suitable in the present invention. However, since the corrosion resistance after coating depends on Al, it is obvious that the larger the amount of adhesion, the better the corrosion resistance, and preferably 120 to 180 g / m 2 when furnace heating is used. However, depending on the heating method, there may be cases where corrosion resistance after coating can be ensured even with an adhesion amount less than this, and on the premise that rapid heating at 20 ° C./second or more is applied, corrosion resistance after painting can be secured at 60 g / m 2 or more. .
溶融めっき法でめっきする場合には極端な薄目付けは困難で、一方めっき付着量が多いと、外観不良を惹起したり、エッジ部の過剰な付着量に起因するコイルの形状不良を起こしたりする。両面６０〜２００ｇ／m2を膜厚に換算すると、片面１０〜３３μｍに相当する。Ａｌめっきをホットプレス工程で加熱する際にＡｌめっきがＡｌ−Ｆｅ金属間化合物に変化する。熱負荷が大きいと、当初の膜厚よりも厚くなる傾向にあるが、本発明は比較的熱負荷が小さい場合を規定しており、１０〜４２μｍとなる。
（ホットプレス前の加熱工程について）
なお、上述したようにして得られたＡｌめっき鋼材は、その後のホットプレス工程においてオーステナイト領域まで加熱され、しかる後に金型で急冷されてマルテンサイト組織となる。このときの加熱条件、冷却条件については特に限定するものではないが、本発明の趣旨は拡散によって生成するＡｌを含有するｂｃｃ層の厚みを規定するもので、加熱条件もある範囲に制約される。また先述したように加熱速度が大きいと塗装後耐食性上は有利となる。通常の電気炉あるいはガス加熱炉を用いた輻射加熱、近赤外線を使用したような加熱法、通電加熱、高周波誘導加熱を用いるような電気的な加熱法のいずれを使用することも可能である。通常は８５０〜１０００℃程度に加熱され、６００〜７００℃付近で急冷されることが多い。加熱雰囲気についても先述したような雰囲気を使用可能である。
（ホットプレス後の酸化膜およびホットプレス前の塗油量）
次に、Ａｌ含有ｂｃｃ層と酸化膜の関係について述べる。Ａｌを含有するｂｃｃ層も、酸化膜も加熱により生じるものであるため、一般には両者は加熱条件に依存してある相関を持つ筈である。ところが加熱条件を適正に保っても塗装後耐食性が劣位となる場合があり、この原因を検討したところ塗油に起因した酸化皮膜が成長し、この酸化皮膜が塗料密着性を弱めることで塗装後耐食性を低下させていた。通常電着塗装前に化成処理と呼ばれるリン酸塩処理が施され、塗料との適合性を確保するが、この材料は化成処理液に対して極めて不活性で、リン酸塩が付着しないことが分かっている。それでも電着塗装との適合性には優れるが、塗油によって成長する酸化皮膜は電着塗装との馴染みが悪いものと推察している。従って塗油の管理は重要であり、０．１〜１ｇ／m2とする。塗油はＡｌめっき鋼板を鉄鋼会社から出荷した後、プレス会社にて熱間プレスを行うまでの一次防錆の役割を担っている。０．１ｇ／m2より少ないとその所定の役割を果たすことができず、１ｇ／m2を超えるような塗油を施すと、先述した理由により塗装後耐食性が低下する。このため上記の量に制限する。
When plating by hot dipping, extreme thinning is difficult. On the other hand, if the amount of plating is large, poor appearance may occur or the shape of the coil may be poor due to excessive amount of adhesion on the edge. . When the thickness on both sides of 60 to 200 g / m 2 is converted into the film thickness, it corresponds to 10 to 33 μm on one side. When the Al plating is heated in a hot press process, the Al plating changes to an Al—Fe intermetallic compound. When the heat load is large, the film thickness tends to be thicker than the initial film thickness. However, the present invention defines a case where the heat load is relatively small, and is 10 to 42 μm.
(About the heating process before hot pressing)
Note that the Al-plated steel material obtained as described above is heated to the austenite region in the subsequent hot pressing step, and then quenched with a mold to become a martensite structure. The heating conditions and cooling conditions at this time are not particularly limited, but the gist of the present invention is to define the thickness of the bcc layer containing Al generated by diffusion, and the heating conditions are also limited to a certain range. . Further, as described above, when the heating rate is high, the corrosion resistance after coating is advantageous. Any of a radiant heating using a normal electric furnace or a gas heating furnace, a heating method using near infrared rays, an electric heating method, or an electric heating method using high-frequency induction heating can be used. Usually, it is heated to about 850 to 1000 ° C. and often rapidly cooled at about 600 to 700 ° C. As the heating atmosphere, the atmosphere as described above can be used.
(Oxide film after hot pressing and amount of oil before hot pressing)
Next, the relationship between the Al-containing bcc layer and the oxide film will be described. Since both the bcc layer containing Al and the oxide film are produced by heating, both should generally have a correlation depending on the heating conditions. However, even if the heating conditions are kept properly, the corrosion resistance after painting may be inferior. After examining the cause, an oxide film grows due to the oil coating, and this oxide film weakens the adhesion of the paint. Corrosion resistance was reduced. A phosphate treatment called a chemical conversion treatment is usually applied before electrodeposition coating, ensuring compatibility with the paint, but this material is extremely inert to the chemical conversion treatment solution and phosphate does not adhere to it. I know it. Even so, it is excellent in compatibility with electrodeposition coating, but it is assumed that the oxide film that grows by oil coating is not familiar with electrodeposition coating. Therefore, the management of oil coating is important, and is set to 0.1 to 1 g / m 2 . Lubricating plays the role of primary rust prevention until it hot-presses in a press company after shipping an Al plating steel plate from a steel company. If the amount is less than 0.1 g / m 2 , the predetermined role cannot be achieved, and if the oil is applied in excess of 1 g / m 2 , the corrosion resistance after coating decreases for the reason described above. For this reason, the above amount is limited.
ホットプレス後の鋼材は、溶接、化成処理、電着塗装等を経て最終製品となる。板厚は通常１〜２．５ｍｍ程度、５９０〜９８０ＭＰａ程度の高強度鋼と溶接で組み合わされて部品となることが多いが、ホットプレス材同士で接合されることもある。また３枚の板組み合せとなることもある。塗装については、通常カチオン電着塗装が用いられることが多く、その膜厚は１〜３０μｍ程度である。電着塗装の後に中塗り、上塗り等の塗装が施されることもある。 The steel material after hot pressing becomes a final product through welding, chemical conversion treatment, electrodeposition coating, and the like. The plate thickness is usually about 1 to 2.5 mm and is combined with high strength steel of about 590 to 980 MPa by welding and often becomes a part, but may be joined by hot press materials. Moreover, it may be a combination of three plates. For coating, cationic electrodeposition coating is usually used, and the film thickness is about 1 to 30 μm. After electrodeposition coating, coating such as intermediate coating and top coating may be applied.
以下、実施例を用いて本発明をさらに具体的に説明する。
実施例
（実施例１）
通常の熱延、冷延工程を経た、表１に示すような鋼成分の冷延鋼板（板厚１．２ｍｍ）を材料として、溶融Ａｌめっきを行った。溶融Ａｌめっきは無酸化炉−還元炉タイプのラインを使用し、めっき後ガスワイピング法でめっき付着量を両面８０〜１６０g/m2まで調節し、その後冷却した。この際のめっき浴組成としてはＡｌ−９％Ｓｉ−２％Ｆｅであった。浴中のＦｅは浴中のめっき機器やストリップから供給される不可避のものである。めっき外観は不めっき等なく良好であった。
Hereinafter, the present invention will be described more specifically with reference to examples.
Example (Example 1)
Using a cold-rolled steel sheet (thickness: 1.2 mm) having a steel component as shown in Table 1 that has undergone normal hot rolling and cold rolling processes, hot-dip Al plating was performed. For the hot-dip Al plating, a non-oxidation furnace-reduction furnace type line was used, and after plating, the amount of plating adhered was adjusted to 80 to 160 g / m 2 on both sides by a gas wiping method, followed by cooling. The plating bath composition at this time was Al-9% Si-2% Fe. Fe in the bath is inevitable supplied from plating equipment or strips in the bath. The plating appearance was good with no plating.
次にこの鋼板を大気中で８５０℃以上に加熱し、約７００℃の温度まで大気中で冷却して、その後厚さ５０ｍｍの金型間で圧着することで急冷した。このときの金型間での冷却速度は約１５０℃/秒であった。加熱方法は電気炉での輻射加熱と近赤外線加熱（ＮＩＲ）の２種類を使用した。このときの加熱速度は炉加熱で約５℃／秒、ＮＩＲで約２０℃／秒であった。加熱条件を種々変化させたときの組織並びに特性を評価した。なお加熱前に脱脂して、油を除去して評価した。 Next, the steel sheet was heated to 850 ° C. or higher in the air, cooled in the air to a temperature of about 700 ° C., and then rapidly cooled by pressure bonding between molds having a thickness of 50 mm. The cooling rate between the molds at this time was about 150 ° C./second. Two types of heating were used: radiation heating in an electric furnace and near infrared heating (NIR). The heating rate at this time was about 5 ° C./second for furnace heating and about 20 ° C./second for NIR. The structure and characteristics when the heating conditions were changed were evaluated. In addition, it degreased before heating and removed and evaluated oil.
Ａｌ含有ｂｃｃ層厚みに関しては、断面研磨、3％ナイタールエッチング後、光学顕微鏡撮影して測定した。酸化膜厚は高周波ＧＤＳを用いて酸素のピークが低下するまでの時間とその間のスパッタリング深さより厚みに換算した。 The thickness of the Al-containing bcc layer was measured by optical microscope photography after cross-sectional polishing and 3% nital etching. The oxide film thickness was converted into thickness using the high frequency GDS from the time until the oxygen peak decreased and the sputtering depth in between.
表２に加熱条件と組織並びに特性評価結果をまとめた。 Table 2 summarizes the heating conditions, structure, and property evaluation results.
（ 実施例２ ）
表１に示した鋼成分を持つ冷延鋼板（厚１．６ｍｍ）に実施例１と同じ要領で溶融Ａｌめっきを施した。めっき付着量は両面１６０g/m2とした。これらのＡｌめっき鋼板に防錆油を塗布した。油は出光興産(株)製のダフニーオイルコートＺ−３とし、付着量を変動させた。大気炉輻射加熱により到達温度９００〜９５０℃、保定時間１〜５分で加熱し、その後金型焼入した。この試料の酸化膜厚及び塗装後耐食性を評価した結果を表３にまとめた。
(Example 2)
A cold-rolled steel plate (thickness 1.6 mm) having the steel components shown in Table 1 was subjected to hot-dip Al plating in the same manner as in Example 1. The plating adhesion amount was 160 g / m 2 on both sides. A rust preventive oil was applied to these Al plated steel sheets. The oil was Daphne Oil Coat Z-3 manufactured by Idemitsu Kosan Co., Ltd., and the adhesion amount was varied. Heating was performed by atmospheric furnace radiant heating at an ultimate temperature of 900 to 950 ° C. and a holding time of 1 to 5 minutes, and then the mold was quenched. Table 3 summarizes the results of evaluating the oxide film thickness and post-coating corrosion resistance of this sample.
（ 実施例３ ）
表４に示した様々な鋼成分を持つ冷延鋼板（厚１．２ｍｍ）に実施例１と同じ要領で溶融Ａｌめっきを施した。めっき付着量は両面１６０g/m2とした。これらのＡｌめっき鋼板を、大気炉輻射加熱により到達温度900℃、保定時間１．５分で加熱し、その後金型焼入した。焼入後の硬度（ビッカース硬度、荷重１0ｋｇ）を測定した結果も表４に示しているが，鋼中C量が低いと焼入後の硬度が低下するため，C量として0.1%以上あることが好ましい。
(Example 3)
The cold-rolled steel sheet (thickness: 1.2 mm) having various steel components shown in Table 4 was subjected to hot Al plating in the same manner as in Example 1. The plating adhesion amount was 160 g / m 2 on both sides. These Al-plated steel sheets were heated by an atmospheric furnace radiant heating at an ultimate temperature of 900 ° C. and a holding time of 1.5 minutes, and then quenched by die. The results of measuring the hardness after quenching (Vickers hardness, load 10 kg) are also shown in Table 4, but since the hardness after quenching decreases when the C content in steel is low, the C content must be 0.1% or more. Is preferred.
Claims (2)
Ｃ：０．１〜０．４％、
Ｓｉ：０．０１〜０．６％、
Ｍｎ：０．５〜３％、
Ｔｉ：０．０１〜０．１％、
Ｂ：０．０００１〜０．０１％を含有し、体積％で９０％以上がマルテンサイトである鋼材の表面に、複数の相からなるＡｌ−Ｆｅ金属間化合物層を有し、
更にその表面に厚みが０．０５〜１μｍの酸化膜を有し、Ａｌ−Ｆｅ金属間化合物層と鋼材の界面にＡｌを含有し厚みが２．５〜１０μｍのｂｃｃ層を有することを特徴とする、塗装後耐食性に優れた自動車部材。 As a steel component in mass%,
C: 0.1-0.4%
Si: 0.01 to 0.6%,
Mn: 0.5-3%,
Ti: 0.01 to 0.1%,
B: having an Al-Fe intermetallic compound layer composed of a plurality of phases on the surface of a steel material containing 0.0001 to 0.01% and having a volume% of 90% or more of martensite;
Furthermore, it has an oxide film having a thickness of 0.05 to 1 μm on its surface, has an bcc layer having a thickness of 2.5 to 10 μm, containing Al at the interface between the Al—Fe intermetallic compound layer and the steel material. Automotive parts with excellent corrosion resistance after painting.
Ｃ：０．１〜０．４％、
Ｓｉ：０．０１〜０．６％、
Ｍｎ：０．５〜３％、
Ｔｉ：０．０１〜０．１％、
Ｂ：０．０００１〜０．０１％を含有し、残部がＦｅ及び不可避的不純物からなる鋼板の表面に片面当たり２０〜１００ｇ／m2のＡｌめっき層を有し、
更にその表面に０．１〜１ｇ／m2の油が付着していることを特徴とする、熱間プレス用Ａｌめっき鋼板。 As a steel component in mass%,
C: 0.1-0.4%
Si: 0.01 to 0.6%,
Mn: 0.5-3%,
Ti: 0.01 to 0.1%,
B: It has 0.0001 to 0.01% of Al and has an Al plating layer of 20 to 100 g / m 2 per side on the surface of the steel plate, the balance being Fe and inevitable impurities,
Further, an Al-plated steel sheet for hot pressing, wherein 0.1 to 1 g / m 2 of oil adheres to the surface.
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