JP2005074468A - Heat treatment method of plated steel sheet for hot pressing - Google Patents

Heat treatment method of plated steel sheet for hot pressing Download PDF

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JP2005074468A
JP2005074468A JP2003307874A JP2003307874A JP2005074468A JP 2005074468 A JP2005074468 A JP 2005074468A JP 2003307874 A JP2003307874 A JP 2003307874A JP 2003307874 A JP2003307874 A JP 2003307874A JP 2005074468 A JP2005074468 A JP 2005074468A
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steel sheet
plated steel
hot
heat treatment
heating
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JP4447270B2 (en
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Akira Obayashi
彰 尾林
Masanobu Ichikawa
正信 市川
Shuntaro Sudo
俊太郎 須藤
Kunihiro Fukui
国博 福井
Kazuhito Imai
和仁 今井
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Nippon Steel Corp
Toyoda Iron Works Co Ltd
Toyota Motor Corp
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Toyoda Iron Works Co Ltd
Sumitomo Metal Industries Ltd
Toyota Motor Corp
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Abstract

<P>PROBLEM TO BE SOLVED: To provide a heat treatment method of a plated steel sheet for hot pressing, a method in which a hot-press formed article having sufficient coating adhesion and corrosion resistance can be stably obtained. <P>SOLUTION: According to this heat treatment method of a plated steel sheet for hot pressing, the plated steel sheet is heat treated before hot pressing in which rapid cooling for quenching is performed in a press mold. For this purpose, a slab specimen 10 is heated in the atmosphere in which oxygen concentration is >0 volume % or in which oxygen concentration is ≥0 volume % with dew point ≥0°C. Accordingly, on the surface of the slab specimen 10, there is formed a metallic oxide layer of the plating material, namely, a barrier layer such as zinc oxide or zinc hydroxide, for example. Thus, rapid oxidation is suitably suppressed when the article is taken out from a heating furnace, enabling the hot-pressed article to be stably obtained that has sufficient coating adhesion and corrosion resistance. <P>COPYRIGHT: (C)2005,JPO&NCIPI

Description

本発明は、めっき鋼板をプレス金型内で急冷して焼き入れを施す熱間プレスに先立って、該めっき鋼板を予め加熱するための熱間プレス用めっき鋼板の加熱処理方法に関するものである。   The present invention relates to a heat treatment method for a hot-pressed plated steel plate for preheating the plated steel plate prior to hot pressing in which the plated steel plate is quenched and quenched in a press mold.

特に、自動車の足周りの部材や各種の補強部材などは、高強度化と軽量化とを両立させることが求められる傾向にある。一般に、使用する鋼板の強度が高くなると、成形加工時においてかじりや破断が発生したり、スプリングバック現象が大きいために成形品の形状が不安定となるという問題がある。   In particular, members around the legs of automobiles and various reinforcing members tend to be required to achieve both high strength and light weight. In general, when the strength of a steel sheet to be used increases, there are problems that galling or fracture occurs during the forming process, and that the shape of the molded product becomes unstable due to a large springback phenomenon.

これに対し、特許文献1および2に示されるように、高強度の鋼材部品を製造するための技術の1つとして熱間プレス成形がある。これによれば、焼き入れ可能な鋼種から選択された成形すべき鋼材がたとえばAc3点以上の温度に予め加熱されてオーステナイト領域とされることにより成形し易くされた状態でプレス成形が施されると同時に或いはその直後に、そのプレス成形された鋼材がMs点以下の温度に急冷されてマルテンサイト変態が発生させられることにより焼き入れが施されて高強度化された鋼材部品が得られる。   On the other hand, as shown in Patent Documents 1 and 2, there is hot press forming as one of the techniques for manufacturing high-strength steel parts. According to this, the steel material to be formed selected from the quenchable steel types is preheated to a temperature of, for example, Ac3 or higher and is made into an austenite region, so that press forming is performed in a state that facilitates forming. At the same time or immediately after that, the press-formed steel material is rapidly cooled to a temperature below the Ms point and a martensitic transformation is generated, so that a steel material part having high strength is obtained by quenching.

ところで、上記のような熱間プレス成形に際しては、比較的高温に加熱されることから鋼材の表面に鉄酸化被膜が形成されることが避けられない。たとえ予備加熱炉内において非酸化雰囲気中で加熱したとしても、その後のプレス成形時に大気に触れて鉄酸化物が表面に形成される。このような鉄酸化物は、プレス成形時に金型内に脱落して生産性を阻害したり、プレス成形後に鉄酸化物が残存して外観不良を発生させたりする。また、このようなプレス成形後の鋼材部品の表面に残存する鉄酸化被膜は密着性に劣るので、後工程における化成処理および塗装処理において塗布される塗装膜の密着性が低下する原因となる可能性がある。   By the way, in the hot press molding as described above, since it is heated to a relatively high temperature, it is inevitable that an iron oxide film is formed on the surface of the steel material. Even if heated in a non-oxidizing atmosphere in a preheating furnace, iron oxide is formed on the surface by touching the atmosphere during subsequent press molding. Such iron oxides fall into the mold at the time of press molding and impede productivity, or iron oxide remains after press molding to cause poor appearance. In addition, since the iron oxide film remaining on the surface of such steel parts after press molding is inferior in adhesion, it may cause a decrease in the adhesion of the coating film applied in the chemical conversion treatment and coating treatment in the subsequent process. There is sex.

これに対し、特許文献3に示されるように、サンドブラスト処理、ショットブラスト処理により鉄酸化被膜を除去した後で、上記化成処理および塗装処理により塗装膜を塗着することが行われるようにした技術が提案されている。また、特許文献4乃至6に示されるように、亜鉛系めっき鋼板やアルミめっき鋼板を使用して熱間プレス成形を行い、鉄酸化被膜の生成を抑制し且つ熱間プレス成形後も耐蝕性を有するめっき被膜を鋼材部品の表面に残存させるようにした技術がそれぞれ提案されている。たとえば、上記特許文献4は、熱処理後の耐久性に優れた熱間圧延および冷間圧延被膜鋼板およびその鋼板を用いた成形品の製造方法であって、5℃/秒以上の昇温速度で750℃以上に加熱する方法であるが、加熱炉の炉内雰囲気については何等の言及がない。上記特許文献5は、被覆圧延鋼板の帯材から高機械的特性値を持つ成形部品を製造する製造方法であって、熱間成形前の加熱時には被膜により障壁が形成されるので炉の雰囲気管理が不要となり、管理されていない炉内雰囲気で900℃で加熱するものである。上記特許文献6は、耐酸化性に劣るAlめっきおよびその他のめっきとFeの金属間化合物の酸化抑制や被塗装性を向上させる技術を開示するものであるが、実施例では加熱炉内酸素濃度21容積%と20容積%との比較のみであり、めっき種として開示されているのはAl系めっき、Snめっきのみであり、しかも、炉内雰囲気の露点については何らの言及がない。また、特許文献7は、熱間プレス用亜鉛めっき鋼板として予め酸化亜鉛層を形成しておく技術であって、酸化する雰囲気として露点30℃以上で700℃に加熱して酸化亜鉛層を形成するものである。   On the other hand, as shown in Patent Document 3, after removing the iron oxide film by sand blasting or shot blasting, a technique of applying a coating film by the chemical conversion treatment and coating treatment is performed. Has been proposed. In addition, as shown in Patent Documents 4 to 6, hot press forming is performed using a zinc-based plated steel plate or an aluminum plated steel plate to suppress the formation of an iron oxide film and to provide corrosion resistance even after hot press forming. Techniques have been proposed in which the plated coatings that remain are left on the surface of steel parts. For example, Patent Document 4 is a method of manufacturing a hot-rolled and cold-rolled coated steel sheet having excellent durability after heat treatment and a molded product using the steel sheet, and has a temperature increase rate of 5 ° C./second or more. Although it is the method of heating to 750 degreeC or more, there is no mention about the furnace atmosphere of a heating furnace. The above-mentioned patent document 5 is a manufacturing method for manufacturing a molded part having a high mechanical property value from a strip of a coated rolled steel sheet, and a barrier is formed by a coating during heating before hot forming, so that the furnace atmosphere is controlled. Is no longer necessary, and heating is performed at 900 ° C. in an uncontrolled furnace atmosphere. Although the said patent document 6 discloses the technique which improves the oxidation suppression of the intermetallic compound of Al plating and other plating and Fe which are inferior in oxidation resistance, and a coating property, in an Example, oxygen concentration in a heating furnace It is only a comparison between 21% by volume and 20% by volume, and only Al-based plating and Sn plating are disclosed as plating types, and there is no mention of the dew point in the furnace atmosphere. Patent Document 7 is a technique for forming a zinc oxide layer in advance as a hot-pressed galvanized steel sheet, and the zinc oxide layer is formed by heating to 700 ° C. at a dew point of 30 ° C. or higher as an oxidizing atmosphere. Is.

特開平7−116900号公報JP-A-7-116900 特開2002−102980号公報JP 2002-102980 A 特開2003−002058号公報JP 2003-002058 A 特開2000−038640号公報JP 2000-038640 A 特開2001−353548号公報JP 2001-353548 A 特開2003−105445号公報JP 2003-105445 A 特開2003−129209号公報JP 2003-129209 A

また、アルミめっき鋼板を熱間プレスした場合、表面にアルミの酸化被膜が生成されることから、鉄酸化被膜の生成ほどでないにしても、塗装密着性に問題があるので、自動車の外板、足周り用部材などに要求されるように厳しい塗装密着性について満足できるものが得られない。   In addition, when an aluminum-plated steel sheet is hot-pressed, an aluminum oxide film is generated on the surface. As required for members around the foot, etc., it is not possible to obtain satisfactory paint adhesion.

また、亜鉛系めっきを鋼板に使用した場合、亜鉛系めっき鋼板を熱間プレス前の予備加熱において酸素濃度0容積%とすると最上層に酸化亜鉛層が形成されないので、加熱炉から大気中に取り出したとき、鋼板が急速に酸化してしまう問題が発生する。また、加熱条件によっては、その酸化亜鉛層が厚くなり過ぎて塗装密着性に問題が発生するおそれもある。   In addition, when zinc-based plating is used for the steel sheet, if the zinc-based plated steel sheet is preheated before hot pressing and the oxygen concentration is 0% by volume, a zinc oxide layer is not formed on the uppermost layer. When this happens, there is a problem that the steel sheet is rapidly oxidized. Further, depending on the heating conditions, the zinc oxide layer may become too thick, which may cause a problem in paint adhesion.

また、酸化亜鉛層が形成される加熱雰囲気条件下であっても、炉内における鋼板の支持方法によっては、支持部材と接触する鋼板部分でそれら2層の形成が不十分となって外観上も不均一が生じるので、その部分の塗装密着性、耐蝕性が低下する場合もあり、予め支持部材との接触部分を除去し、残りの部分を加熱処理後めっき鋼板として用いられるようにしておく必要があった。   Moreover, even under the heating atmosphere conditions in which the zinc oxide layer is formed, depending on the method of supporting the steel plate in the furnace, the formation of these two layers is insufficient at the steel plate portion in contact with the support member, so that the appearance is also improved. Since non-uniformity occurs, the paint adhesion and corrosion resistance of the part may decrease, so it is necessary to remove the contact part with the support member in advance and use the remaining part as a plated steel sheet after heat treatment was there.

本発明は以上の事情を背景として為されたもので、その目的とするところは、十分な塗装密着性および耐蝕性を有する熱間プレス成形品を安定して得ることができる熱間プレス用めっき鋼板の加熱処理方法を提供することにある。   The present invention has been made against the background of the above circumstances, and its object is to provide hot press plating that can stably obtain a hot press-formed product having sufficient paint adhesion and corrosion resistance. It is providing the heat processing method of a steel plate.

本発明者等は、以上の事情を背景として種々検討を重ねた結果、熱間プレス成形に先立つめっき鋼板の加熱のための加熱炉内の酸素濃度を0容積%より高い酸素濃度としたときに、加熱炉から取り出したときに鋼板の表面が急速酸化されることがなくなって均一な外観が得られることを見い出した。本発明者等の分析によれば、その加熱炉内においてそのめっき鋼板の表面に酸化物層或いは水酸化物層が予め形成され、それが急速酸化を抑制するバリア層として機能すること、また、上記加熱炉内においては、めっき鋼板を支持する支持部材との接触面が小さいほど、酸化物層或いは水酸化物層がより一層均一に形成されることなどが判明した。本発明は、このような知見に基づいて為されたものである。なお、上記めっき鋼板が亜鉛めっき鋼板である場合には、その亜鉛めっき鋼板の表面に酸化亜鉛層或いは水酸化亜鉛層が予め形成される。   As a result of repeating various studies on the background of the above circumstances, the present inventors have made the oxygen concentration in the heating furnace for heating the plated steel sheet prior to hot press forming an oxygen concentration higher than 0% by volume. It has been found that the surface of the steel sheet is not rapidly oxidized when taken out from the heating furnace, and a uniform appearance can be obtained. According to the analysis of the present inventors, an oxide layer or a hydroxide layer is formed in advance on the surface of the plated steel plate in the heating furnace, and it functions as a barrier layer for suppressing rapid oxidation. It has been found that in the heating furnace, the smaller the contact surface with the support member that supports the plated steel sheet, the more uniformly the oxide layer or hydroxide layer is formed. The present invention has been made based on such knowledge. In addition, when the said plated steel plate is a galvanized steel plate, the zinc oxide layer or the zinc hydroxide layer is previously formed in the surface of the galvanized steel plate.

すなわち、請求項1に係る発明の要旨とするところは、めっき鋼板をプレス金型内で急冷して焼き入れを施す熱間プレスに先立ってそのめっき鋼板を予め加熱するための熱間プレス用めっき鋼板の加熱処理方法であって、そのめっき鋼板を、酸素濃度が0容積%よりも高い雰囲気で加熱することにある。   That is, the gist of the invention according to claim 1 is that hot-plated plating for pre-heating the plated steel sheet prior to hot pressing in which the plated steel sheet is quenched and quenched in a press die. It is a heat treatment method for a steel sheet, and the plated steel sheet is heated in an atmosphere having an oxygen concentration higher than 0% by volume.

また、請求項2に係る発明の要旨とするところは、めっき鋼板をプレス金型内で急冷して焼き入れを施す熱間プレスに先立ってそのめっき鋼板を予め加熱するための熱間プレス用めっき鋼板の加熱処理方法であって、そのめっき鋼板を、酸素濃度が0容積%以上且つ露点が0℃以上の雰囲気で加熱することにある。   Further, the subject matter of the invention according to claim 2 is a hot press plating for preheating a plated steel sheet prior to a hot press in which the plated steel sheet is quenched in a press die and quenched. It is a heat treatment method for a steel sheet, and the plated steel sheet is heated in an atmosphere having an oxygen concentration of 0% by volume or more and a dew point of 0 ° C. or more.

また、請求項3に係る発明の要旨とするところは、前記雰囲気は、酸素濃度が1〜5容積%の範囲内の低酸素雰囲気であることにある。   The gist of the invention according to claim 3 is that the atmosphere is a low oxygen atmosphere having an oxygen concentration in the range of 1 to 5% by volume.

また、請求項4に係る発明の要旨とするところは、前記めっき鋼板は、亜鉛系めっき鋼板であることにある。   The gist of the invention according to claim 4 is that the plated steel sheet is a zinc-based plated steel sheet.

また、請求項5に係る発明の要旨とするところは、前記加熱処理は、ガス炉内の燃焼ガス雰囲気で行われるものであることにある。   Further, the gist of the invention according to claim 5 is that the heat treatment is performed in a combustion gas atmosphere in a gas furnace.

また、請求項6に係る発明の要旨とするところは、前記加熱処理は、前記めっき鋼板が支持部材により線接触または点接触にて支持された状態で行われるものである。   The gist of the invention according to claim 6 is that the heat treatment is performed in a state where the plated steel sheet is supported by a support member in a line contact or a point contact.

請求項1に係る熱間プレス用めっき鋼板の加熱処理方法によれば、プレス金型内で急冷して焼き入れを施す熱間プレスに先立ってめっき鋼板を加熱処理するために、酸素濃度が0容積%よりも高い雰囲気でめっき鋼板が加熱されることから、そのめっき鋼板の表面にそのめっき材料の金属酸化物層などのバリヤ層が形成されて加熱炉から取り出したときの急速酸化が好適に抑制されるので、十分な塗装密着性および耐蝕性を有する熱間プレス成形品が安定して得られる。   According to the heat treatment method of a hot-pressed plated steel sheet according to claim 1, the oxygen concentration is 0 in order to heat-treat the plated steel sheet prior to the hot press in which the steel sheet is quenched and quenched in the press die. Since the plated steel sheet is heated in an atmosphere higher than the volume%, a rapid oxidation is preferably performed when a barrier layer such as a metal oxide layer of the plating material is formed on the surface of the plated steel sheet and taken out from the heating furnace. Therefore, a hot press-formed product having sufficient paint adhesion and corrosion resistance can be stably obtained.

また、前記請求項2に係る熱間プレス用めっき鋼板の加熱処理方法によれば、酸素濃度が0容積%以上且つ露点が0℃以上の雰囲気でめっき鋼板が加熱されることから、たとえ加熱炉の酸素濃度が0容積%であっても露点が0℃以上のある程度の気中の水分の存在下で、めっき材料を構成する金属の水酸化物層がバリヤ層を構成することから、加熱炉から取り出したときの急速酸化が好適に抑制されるので、十分な塗装密着性および耐蝕性を有する熱間プレス成形品が安定して得られる。   Further, according to the heat treatment method for a hot-pressed plated steel sheet according to claim 2, the plated steel sheet is heated in an atmosphere having an oxygen concentration of 0% by volume or more and a dew point of 0 ° C or more. Since the metal hydroxide layer constituting the plating material constitutes a barrier layer in the presence of a certain amount of moisture in the air with a dew point of 0 ° C. or higher even when the oxygen concentration in the furnace is 0% by volume, the heating furnace Since the rapid oxidation when taken out from is suitably suppressed, a hot press-formed product having sufficient paint adhesion and corrosion resistance can be stably obtained.

また、前記請求項3に係る発明によれば、上記加熱雰囲気は、酸素濃度が1〜5容積%の範囲内の低酸素雰囲気とされることから、そのめっき鋼板の表面にそのめっき材料を構成する金属の金属酸化物層などのバリヤ層が適切な厚みに形成されるので、加熱炉から取り出したときの急速酸化が好適に抑制されると同時に、その金属酸化物層などが厚くなり過ぎて塗装密着性に問題が生じることも好適に解消される。   According to the invention of claim 3, since the heating atmosphere is a low oxygen atmosphere having an oxygen concentration in the range of 1 to 5% by volume, the plating material is formed on the surface of the plated steel sheet. Since the barrier layer such as the metal oxide layer of the metal is formed with an appropriate thickness, rapid oxidation when taken out from the heating furnace is suitably suppressed, and at the same time the metal oxide layer becomes too thick. It is also preferable to eliminate the problem of paint adhesion.

また、前記請求項4に係る発明によれば、前記めっき鋼板は、亜鉛系めっき鋼板であることから、バリヤ層として、酸化亜鉛層或いは水酸化亜鉛層が形成されるので、加熱炉から取り出したときの急速酸化が好適に抑制される。   Further, according to the invention according to claim 4, since the plated steel sheet is a zinc-based plated steel sheet, a zinc oxide layer or a zinc hydroxide layer is formed as a barrier layer. When the rapid oxidation is suitably suppressed.

また、前記請求項5に係る発明によれば、前記加熱処理はガス炉内の燃焼ガス雰囲気で行われることから、そのガス炉における可燃性(燃料)ガスと空気の割合を変化させることにより、酸素濃度を簡単且つ容易に制御できる利点がある。   According to the invention of claim 5, since the heat treatment is performed in a combustion gas atmosphere in a gas furnace, by changing the ratio of combustible (fuel) gas and air in the gas furnace, There is an advantage that the oxygen concentration can be controlled easily and easily.

また、請求項6に係る発明によれば、前記加熱処理において、前記めっき鋼板が支持部材により線接触または点接触にて支持された状態で行われるものであるので、鋼板の表面に酸化亜鉛層或いは水酸化亜鉛層などのバリヤ層が一層均一に形成される。また、めっき鋼板とそれを支持する支持部材とが面接触する場合のように、その面接触した部分を除去し、残りの部分を加熱処理後めっき鋼板として用いる必要がない。   Moreover, according to the invention which concerns on Claim 6, in the said heat processing, since the said plated steel plate is performed in the state supported by the support member by the line contact or the point contact, a zinc oxide layer is formed on the surface of a steel plate. Alternatively, a barrier layer such as a zinc hydroxide layer is formed more uniformly. Further, as in the case where the plated steel plate and the supporting member supporting it are in surface contact, it is not necessary to remove the surface-contacted portion and use the remaining portion as the plated steel plate after the heat treatment.

ここで、熱間プレスは、鋼板をAc3点以上の温度に加熱処理してオーステナイト領域とした低強度状態でプレス加工した後、直ちにそのプレス金型内で或いはプレス金型外でMs点以下の温度に急冷し、マルテンサイト変態を発生させることにより焼き入れを施して高強度の鋼材部品を製造する加工技術である。したがって、この熱間プレスに先立ってめっき鋼板をオーステナイト相とする温度まで加熱炉で加熱する必要がある。亜鉛めっき鋼板である場合、上記加熱処理および熱間プレス後にはその鋼板の表面に鉄亜鉛層および酸化亜鉛層の2層が生成されている。   Here, in the hot press, the steel sheet is heat-treated at a temperature of Ac3 point or higher and pressed into austenite region in a low-strength state, and then immediately within the press die or outside the press die, the Ms point or less. It is a processing technique for quenching to temperature and quenching by generating martensitic transformation to produce high strength steel parts. Therefore, prior to this hot pressing, it is necessary to heat in a heating furnace to a temperature at which the plated steel sheet becomes an austenitic phase. In the case of a galvanized steel sheet, two layers of an iron zinc layer and a zinc oxide layer are formed on the surface of the steel sheet after the heat treatment and hot pressing.

純粋な亜鉛の融点は420℃、沸点は907℃であることから、上記加熱炉内における900℃の加熱処理において亜鉛は蒸発或いは溶融するものと一般的に推定されるかも知れないが、実際の電気炉内における大気雰囲気中で加熱した鋼材の断面を観察すると、最表層に酸化亜鉛および/または水酸化亜鉛のバリア層が形成され、その内層に鉄亜鉛層が形成されていた。この酸化亜鉛層や水酸化亜鉛層が、加熱炉から取り出したときの急速酸化反応を抑制していると考えられる。このため、その酸化亜鉛層や水酸化亜鉛層の形成には、酸素および/または水蒸気の寄与が必要であり、上記加熱処理において窒素雰囲気や、完全燃焼に理論上必要な酸素量以下の空気を供給して酸素欠乏状態(低酸素状態)とした場合には亜鉛の酸化被膜である酸化亜鉛層が形成されない。   Since pure zinc has a melting point of 420 ° C. and a boiling point of 907 ° C., it may be generally estimated that zinc will evaporate or melt in the heat treatment at 900 ° C. in the heating furnace. When the cross section of the steel material heated in the air atmosphere in an electric furnace was observed, the barrier layer of zinc oxide and / or zinc hydroxide was formed in the outermost layer, and the iron zinc layer was formed in the inner layer. This zinc oxide layer or zinc hydroxide layer is considered to suppress the rapid oxidation reaction when taken out from the heating furnace. For this reason, the formation of the zinc oxide layer and the zinc hydroxide layer requires the contribution of oxygen and / or water vapor. In the above heat treatment, a nitrogen atmosphere or air below the oxygen amount theoretically required for complete combustion is used. When supplied to be in an oxygen-deficient state (low oxygen state), a zinc oxide layer that is an oxide film of zinc is not formed.

上記加熱処理後或いは熱間プレス後の鋼材の表面において上記鉄亜鉛層の上に生成される酸化亜鉛層は平均膜厚として5μm以下の範囲であることが望ましい。酸化亜鉛層の平均膜厚が5μmを超えると、酸化亜鉛層自体の鋼材に対する密着性が劣化して塗装の密着性が不十分となる。なお、酸化亜鉛層には、酸化亜鉛の他に、亜鉛の水酸化物などを含む場合やめっき中の成分であるAl(アルミニウム)などの酸化物が含まれる場合がある。本発明の酸化亜鉛層とは、このような場合のものが含まれる。   The zinc oxide layer formed on the iron zinc layer on the surface of the steel material after the heat treatment or after hot pressing is desirably in the range of 5 μm or less as an average film thickness. When the average thickness of the zinc oxide layer exceeds 5 μm, the adhesion of the zinc oxide layer itself to the steel material is deteriorated and the adhesion of the coating becomes insufficient. In addition to the zinc oxide, the zinc oxide layer may contain a hydroxide of zinc or the like, or an oxide such as Al (aluminum) which is a component during plating. The zinc oxide layer of the present invention includes such a case.

上記加熱処理後或いは熱間プレス後の鋼材の表面に生成される鉄亜鉛層の平均厚みは、1μm乃至50μmの範囲内のものが望ましい。鉄亜鉛層の平均厚みが1μmを下まわると耐蝕性が十分でなくなり、50μmを超えるとスポット溶接などの溶接性が不十分となるからである。   The average thickness of the iron-zinc layer generated on the surface of the steel material after the heat treatment or after hot pressing is preferably in the range of 1 μm to 50 μm. This is because when the average thickness of the iron-zinc layer is less than 1 μm, the corrosion resistance becomes insufficient, and when it exceeds 50 μm, the weldability such as spot welding becomes insufficient.

熱間プレス加工された鋼材部品の素地である鋼材は、特に成分が限定されるものではない。たとえば、前述のように、熱間プレス工程で焼き入れすることを想定した場合、鋼板の焼き入れ後の強度は主にそれに含有される炭素、マンガン、クロム、ボロンの含有量から算出される炭素当量により決定される。高強度の成形品が必要である場合にはたとえばCの含有量が0.1重量%以上且つ3.0重量%以下の範囲内とすることが望ましい。0.1重量%を下まわると強度が低下し、3.0重量%を超えると靱性が低下するおそれがある。   The component of the steel material that is the base of the hot-pressed steel material component is not particularly limited. For example, as described above, when it is assumed that the steel sheet is quenched in the hot pressing process, the strength after quenching of the steel sheet is mainly calculated from the contents of carbon, manganese, chromium, and boron contained therein. Determined by equivalent weight. When a high-strength molded product is required, for example, the C content is desirably in the range of 0.1 wt% or more and 3.0 wt% or less. If the amount is less than 0.1% by weight, the strength is lowered, and if it exceeds 3.0% by weight, the toughness may be lowered.

上記熱間プレス加工される素地鋼材は、亜鉛めっきを行うために亜鉛との濡れ性や密着性が十分であることが必要である。高Si鋼など濡れ性に問題がある場合には、表面研削やプレめっき(予備めっき)などの密着性向上工程が適宜用いられ得る。   The base steel material to be hot-pressed needs to have sufficient wettability and adhesion with zinc in order to perform galvanization. When there is a problem with wettability such as high Si steel, an adhesion improving process such as surface grinding or pre-plating (pre-plating) can be used as appropriate.

本発明においては、めっき鋼板として合金化溶融亜鉛めっき鋼板が好適に用いられるため、めっき後の鉄亜鉛の合金化が短時間で行われるように、Pの含有量の少ない鋼材が好ましい。連続ラインでのめっき合金化処理を前提とすると、Pの含有量は0.2重量%以下が好ましい。   In the present invention, an alloyed hot-dip galvanized steel sheet is suitably used as the plated steel sheet. Therefore, a steel material having a low P content is preferable so that the alloying of iron zinc after plating is performed in a short time. Assuming a plating alloying treatment in a continuous line, the P content is preferably 0.2% by weight or less.

素地鋼材の表面に固着されるめっき種は、Al系めっきや亜鉛系めっきなどがあるが、好ましくは亜鉛系めっきである。そのめっき種は、最終的に熱間プレス成形品の品質が得られるのであれば、特にその種類は限定されない。即ち、純亜鉛めっきであってもMn、Ni、Cr、Co、Mg、Sn、Pbなどの合金元素をその目的に応じて適宜添加した亜鉛合金めっきであってもよい。その原料から不可避的にBe、B、Si、P、Ti、V、W、Mo、Sb、Cd、Nb、Cu、Srなどが含有されることがある。望ましい組成は、亜鉛−鉄合金、亜鉛−ニッケル合金、亜鉛−コバルト合金、亜鉛−クロム合金、亜鉛−マンガン合金のめっきなどである。これは、めっき被膜の融点が純亜鉛めっきと比較して高く、めっき被膜中の亜鉛が蒸発しにくいためである。めっき方法は、電気めっき法、溶融めっき法により鋼板にめっき処理が施されるが、この方法に限定されない。   The plating type fixed to the surface of the base steel material includes Al-based plating and zinc-based plating, and zinc-based plating is preferable. The plating type is not particularly limited as long as the quality of the hot press-formed product can be finally obtained. That is, even pure zinc plating may be zinc alloy plating in which alloy elements such as Mn, Ni, Cr, Co, Mg, Sn, and Pb are appropriately added according to the purpose. The raw material inevitably contains Be, B, Si, P, Ti, V, W, Mo, Sb, Cd, Nb, Cu, Sr and the like. Desirable compositions include zinc-iron alloy, zinc-nickel alloy, zinc-cobalt alloy, zinc-chromium alloy, zinc-manganese alloy plating, and the like. This is because the melting point of the plating film is higher than that of pure zinc plating, and the zinc in the plating film is difficult to evaporate. The plating method is not limited to this method, although the steel sheet is plated by electroplating or hot dipping.

製造コストおよび性能面からは、合金化溶融亜鉛めっき鋼板が最も好ましい。このとき、めっき被膜中の鉄含有量を比較的高めの10%以上としておけば、実用上比較的短時間で鉄亜鉛層が形成されるので、さらに好ましい。めっき被膜中の鉄含有量は20重量%以下であることが望ましい。これは、現在のめっき製造ラインにおいては、これを超えた鉄含有率を達成しようとすると、ラインスピードを極端に低下させる必要があり、非現実的であるからである。   From the viewpoint of production cost and performance, an alloyed hot-dip galvanized steel sheet is most preferable. At this time, if the iron content in the plating film is set to a relatively high value of 10% or more, the iron-zinc layer is formed in a relatively short time for practical use. The iron content in the plating film is desirably 20% by weight or less. This is because in the current plating production line, if it is attempted to achieve an iron content exceeding this, it is necessary to extremely reduce the line speed, which is unrealistic.

めっき付着量は、後述する加熱工程での亜鉛の蒸発および酸化被膜形成工程での減少をも考慮して、最終的に熱間プレス成形品の表層部に亜鉛として10g/m2 以上残存する程度に十分なものとする。具体的には成形品が使用される部位が必要とする耐蝕性のレベルによって選択されるべきであるが、40g/m2 以上は必要である。厳しい耐蝕性が要求される自動車部品では、めっき付着量が亜鉛として50g/m2 以上の付着量が望ましい。めっきの生産性を考慮すると、50〜70g/m2 の範囲内の付着量が最適である。 The amount of plating adhesion is such that zinc will remain at 10 g / m 2 or more as zinc in the surface layer portion of the hot press-molded product in consideration of the evaporation of zinc in the heating step described later and the decrease in the oxide film forming step. Be sufficient. Specifically, it should be selected depending on the level of corrosion resistance required by the site where the molded product is used, but 40 g / m 2 or more is necessary. For automotive parts that require strict corrosion resistance, an adhesion amount of 50 g / m 2 or more as the zinc adhesion amount is desirable. Considering the productivity of plating, the adhesion amount in the range of 50 to 70 g / m 2 is optimal.

熱間プレスに先立つ加熱方法或いは加熱装置は特に限定されないが、通常、ガス炉または窒素などによる不活性ガス雰囲気の電気炉により加熱が行われる。この加熱によりめっき被膜中の亜鉛の一部は蒸発したり酸化亜鉛層となって上部に存在し、また残りの一部または全部が素地鋼材中に拡散させられることにより、鉄亜鉛層を含むめっき層が形成される。   The heating method or heating device prior to hot pressing is not particularly limited, but heating is usually performed in a gas furnace or an electric furnace in an inert gas atmosphere such as nitrogen. By this heating, part of the zinc in the plating film evaporates or becomes a zinc oxide layer and exists in the upper part, and the remaining part or the whole is diffused into the base steel material, thereby plating including the iron zinc layer A layer is formed.

熱間プレス時の鋼板材料の加熱温度は、通常、700〜1000℃程度である。このときの鋼板を加熱する加熱炉は、700〜1000℃の温度に設定される。鋼板材料の温度が高すぎると、酸化亜鉛層の膜厚が大きくなりすぎて、溶接性が低下したり酸化亜鉛層の密着性が劣化して塗装密着性に劣るものとなる。反対に、加熱温度が低すぎると、鋼板材料の軟化が不十分となって熱間プレス加工時に過大なプレス圧(負荷)が必要となり、鋼板材料の表面にクラックなどの欠陥を発生させたり、鋼板材料が破断する原因となる。また、焼き入れ鋼の場合、冷却勾配がその焼き入れ性と関連しているので、材料温度を一定値以上に加熱保持し、一定値以上の冷却勾配で冷却することが必要となる。したがって、材料の加熱温度も一定温度以上でなければ、十分にその冷却勾配を確保できなくなる。このような観点から、好ましい加熱条件は、材料温度が800〜900℃となるように加熱炉の温度を設定することである。   The heating temperature of the steel plate material during hot pressing is usually about 700 to 1000 ° C. The heating furnace which heats the steel plate at this time is set to a temperature of 700 to 1000 ° C. If the temperature of the steel plate material is too high, the film thickness of the zinc oxide layer becomes too large, resulting in poor weldability, poor adhesion of the zinc oxide layer, and poor paint adhesion. On the other hand, if the heating temperature is too low, the softening of the steel plate material is insufficient and an excessive press pressure (load) is required during hot press processing, causing defects such as cracks on the surface of the steel plate material, It causes the steel sheet material to break. In the case of hardened steel, since the cooling gradient is related to the hardenability, it is necessary to heat and hold the material temperature at a certain value or higher and to cool with a cooling gradient at a certain value or more. Therefore, if the heating temperature of the material is not higher than a certain temperature, the cooling gradient cannot be sufficiently secured. From such a viewpoint, a preferable heating condition is to set the temperature of the heating furnace so that the material temperature becomes 800 to 900 ° C.

熱間プレス前の鋼板材料の加熱時間すなわち前記加熱温度の保持時間は特に限定はない。しかし、鉄亜鉛層およびその上の酸化亜鉛層の厚みを目的の条件に制御するためには、最適値が存在する。加熱時間が極端に短い場合、たとえば数秒程度であるとすると、亜鉛系めっき被膜と母材の鋼材の相互拡散により形成される鉄亜鉛層を十分に形成することが難しい。また、逆に加熱時間が10分を超えるような長時間となると、炉内雰囲気にもよるが、酸化亜鉛層の厚さが過剰となる場合がある。当然、エネルギー損失を考えても、長時間加熱は好ましくない。従って、好ましい加熱時間は数分である。   The heating time of the steel plate material before hot pressing, that is, the holding time of the heating temperature is not particularly limited. However, there is an optimum value for controlling the thickness of the iron-zinc layer and the zinc oxide layer thereon to a desired condition. When the heating time is extremely short, for example, about several seconds, it is difficult to sufficiently form an iron-zinc layer formed by mutual diffusion of the zinc-based plating film and the base steel material. On the other hand, if the heating time is longer than 10 minutes, the thickness of the zinc oxide layer may become excessive depending on the atmosphere in the furnace. Of course, even if energy loss is considered, heating for a long time is not preferable. Therefore, the preferred heating time is a few minutes.

熱間プレス前に鋼板材料を加熱するための加熱炉内においては、酸素濃度が0容積%よりも高い雰囲気、好ましくは1〜5容積%の範囲内の低酸素雰囲気、さらに好ましくは1〜3容積%の範囲内の低酸素雰囲気であることが望まれる。酸素量が多すぎると温度条件によっては酸化亜鉛層が厚くなり過ぎて塗装密着性に問題が生じる可能性がある。0容積%よりも高い酸素濃度であれば酸化亜鉛層が一応形成されるが、1容積%以上の酸素濃度であれば酸化亜鉛層が能率よく形成される。   In a heating furnace for heating a steel plate material before hot pressing, an atmosphere having an oxygen concentration higher than 0% by volume, preferably a low oxygen atmosphere in the range of 1 to 5% by volume, more preferably 1 to 3%. A low oxygen atmosphere within the volume percent range is desired. If the amount of oxygen is too large, the zinc oxide layer becomes too thick depending on the temperature condition, which may cause a problem in coating adhesion. If the oxygen concentration is higher than 0% by volume, the zinc oxide layer is temporarily formed. If the oxygen concentration is 1% by volume or more, the zinc oxide layer is efficiently formed.

加熱炉として電気抵抗の高い発熱体によって加熱される電気炉が用いられる場合は、任意に酸素濃度、水蒸気濃度を調節したり制御したりすることが可能であるが、上記酸素濃度の範囲内とするために大気の酸素濃度約21容積%よりも低酸素とするためには、窒素ガスなどの不活性ガスを炉内に注入して酸素濃度を低下させることができる。また、酸化し易い別の金属を予め炉内において酸化させることにより酸素濃度を低下させることも行われ得る。   When an electric furnace heated by a heating element having a high electric resistance is used as the heating furnace, the oxygen concentration and the water vapor concentration can be arbitrarily adjusted or controlled. Therefore, in order to make the oxygen concentration lower than the atmospheric oxygen concentration of about 21% by volume, an inert gas such as nitrogen gas can be injected into the furnace to lower the oxygen concentration. It is also possible to reduce the oxygen concentration by previously oxidizing another metal that is easily oxidized in the furnace.

ガス炉が用いられる場合は、燃焼ガス雰囲気で加熱される。この場合、ガス炉内の可燃性ガスと空気との流量比を変化させることで、燃焼状態や炉内雰囲気が制御される。計算上で完全燃焼するのに必要な酸素を含む空気量と同等かそれより少なくすると、炉内は酸素欠乏状態となる。また、酸素濃度を0容積%よりも高い値、たとえば1〜5容積%の範囲内或いは1〜3容積%の範囲内とするためには、上記の空気量が調節される。上記燃焼ガスを生成する可燃性ガスとしては天然ガス、プロパンガス等の炭化水素系ガスが好適に用いられるが、鋼材を腐食させないガスであればよい。   When a gas furnace is used, it is heated in a combustion gas atmosphere. In this case, the combustion state and the furnace atmosphere are controlled by changing the flow rate ratio between the combustible gas and the air in the gas furnace. If the amount of air containing oxygen necessary for complete combustion in the calculation is equal to or less than the amount of air, the inside of the furnace becomes deficient in oxygen. In order to set the oxygen concentration to a value higher than 0% by volume, for example, in the range of 1 to 5% by volume or in the range of 1 to 3% by volume, the air amount is adjusted. As the combustible gas for generating the combustion gas, a hydrocarbon-based gas such as natural gas or propane gas is preferably used, but any gas that does not corrode steel materials may be used.

上記加熱炉には、火炎を直接鋼材に当てる直火加熱方法や、輻射熱で加熱する方法もあるが、被加熱材の昇温勾配の均一性、到達温度制御の容易性の観点から、一定温度に加熱された雰囲気中で加熱する雰囲気加熱が望ましい。   The heating furnace includes a direct flame heating method in which a flame is directly applied to a steel material, and a method of heating with radiant heat. However, from the viewpoint of uniformity of a temperature rising gradient of a material to be heated and ease of achieving ultimate temperature control, a constant temperature It is desirable to perform atmospheric heating in which the heating is performed in a heated atmosphere.

熱間プレス前に鋼板材料を加熱するための加熱炉内の水蒸気量は露点で管理されるのが一般的である。各温度で飽和する水蒸気量が予め求められているので、その露点を測定することにより炉内雰囲気中の水蒸気量が測定される。一般に、低水蒸気量とするには、冷凍法にて除去する方法があるが、温度が低くなるに伴って高コストとなる。逆に、高くするのは特に難しくなく、水蒸気を炉内に加えることで簡単に実現できる。露点は、0℃以上であればよいが、効率的な水酸化亜鉛の生成のために、好ましくは20℃以上、さらに好ましくは30℃以上が望まれる。   The amount of water vapor in the heating furnace for heating the steel plate material before hot pressing is generally managed by the dew point. Since the amount of water vapor saturated at each temperature is determined in advance, the amount of water vapor in the furnace atmosphere is measured by measuring the dew point. In general, there is a method of removing by a refrigeration method to reduce the amount of water vapor, but the cost increases as the temperature decreases. On the other hand, it is not particularly difficult to make it high, and it can be easily realized by adding steam into the furnace. Although a dew point should just be 0 degreeC or more, in order to produce | generate efficient zinc hydroxide, Preferably it is 20 degreeC or more, More preferably, 30 degreeC or more is desired.

前記熱間プレス成形は、通常のプレス方法と同様にプレス型を用いて鋼板を成形するものであるが、成形時の温度は鋼材を軟化させる一定値以上でなければならない。鋼材の厚み、強度、成形形状によって鋼材の温度は調整されるが、一般的には熱間プレス時において700℃以上であることが好ましい。このため、加熱炉から出された鋼板は速やかにプレス機に搬送され且つプレス型にセットされることが望ましい。   In the hot press forming, a steel plate is formed using a press die in the same manner as in a normal pressing method, but the temperature at the time of forming must be not less than a certain value that softens the steel material. The temperature of the steel material is adjusted depending on the thickness, strength, and shape of the steel material, but generally it is preferably 700 ° C. or higher during hot pressing. For this reason, it is desirable that the steel sheet taken out of the heating furnace is promptly transported to a press machine and set in a press die.

上記熱間プレス成形に際して鋼材を急速冷却する方法は、特に限定されるものではないが、焼き入れを行うという観点からは、冷却勾配が十分にとれるように調整されることが必要であり、プレス金型内に水冷機構を組み込むことが、設備的或いは能率的な面で有効である。この場合、熱間の鋼板材料に直接水がかかる直接水冷方式、プレス金型内部に冷却水路を設ける間接冷却方式があるがいずれでもよい。熱間の鋼板材料に直接水がかかるか否かによって表面の酸化亜鉛層の厚みや構造に若干の差異は生じるが、5μmという被膜厚み以下に設定することはいずれの方法でも可能である。   The method of rapidly cooling the steel material during the hot press forming is not particularly limited, but from the viewpoint of quenching, it is necessary to adjust the cooling gradient sufficiently. Incorporation of a water cooling mechanism in the mold is effective in terms of equipment or efficiency. In this case, there are a direct water cooling method in which water is directly applied to the hot steel plate material and an indirect cooling method in which a cooling water channel is provided inside the press die. A slight difference occurs in the thickness and structure of the zinc oxide layer on the surface depending on whether or not water is directly applied to the hot steel sheet material, but any method can be used to set the coating thickness to 5 μm or less.

前記熱間プレス前に鋼板材料を加熱するための加熱炉内において、鋼板材料が700〜1000℃で加熱処理されるが、そのような温度域において鋼板材料は支持部材によって点接触或いは線接触で支持されることが望ましい。具体的には、円柱或いは円筒状支持部材による線接触支持、円錐状支持部材による曲面支持、角柱状或いは角錐状支持部材による稜線支持、板材状支持部材による端面支持、円錐或いは角錐状支持部材による頂点支持、半球状支持部材による球面支持などである。これら支持部材は、700〜1000℃で鉄、亜鉛又はアルミニウムと反応し難い材料で且つ酸素および水蒸気とも反応し難い材料であればよく、セラミックス材料、耐熱合金鋼などが好適に用いられる。この支持部材は、中空或いは中実であってもよい。炉内における鋼板に対するその他の支持方法として、エアー圧で浮遊させる支持方法であってもよい。   In the heating furnace for heating the steel plate material before the hot pressing, the steel plate material is heat-treated at 700 to 1000 ° C., but in such a temperature range, the steel plate material is point contact or line contact by the support member. It is desirable to be supported. Specifically, line contact support using a columnar or cylindrical support member, curved surface support using a conical support member, ridge line support using a prismatic or pyramid support member, end surface support using a plate-like support member, cone or pyramid support member For example, apex support and spherical support by a hemispherical support member. These supporting members may be any material that does not easily react with iron, zinc, or aluminum at 700 to 1000 ° C. and does not easily react with oxygen and water vapor, and ceramic materials, heat-resistant alloy steel, and the like are preferably used. This support member may be hollow or solid. As another support method for the steel plate in the furnace, a support method in which the steel plate is floated by air pressure may be used.

前記の加熱炉により加熱されるとともに熱間プレスにより所定形状に成形され且つ焼き入れされた亜鉛めっき鋼板は、耐蝕性があり且つ軽量で高剛性或いは高強度であるため、単独で或いはスポット溶接されて一体化された複数で、たとえば、自動車の車体、或いはその構成部品の一部であるフレーム、パネル、サイドメンバ、ドア、リンフォースメント、ドアインパクトビーム、センターピラーやフロントピラーなどのピラー類などの鋼材部品を構成する。   The galvanized steel sheet, which is heated by the heating furnace and formed into a predetermined shape by hot pressing and quenched, is corrosion-resistant and lightweight, high-rigidity or high-strength. For example, a frame, a panel, a side member, a door, a reinforcement, a door impact beam, a pillar such as a center pillar or a front pillar, etc. Of steel material parts.

以下、本発明の熱間プレス用めっき鋼板の加熱処理方法について、本発明者等が行った実験例およびその評価結果を以下に説明する。   Hereinafter, the experiment example and the evaluation result which the present inventors performed about the heat processing method of the plated steel plate for hot press of this invention are demonstrated below.

試料の製造
・試験素材
実験に用いるために、Cを0.2重量%、Siを0.3重量%、Mnを1.3重量%、Pを0.01重量%、を含有する板厚2mm×縦300mm×横100mmの冷間圧延鋼板を素地鋼板とし、それに対して溶融めっき法により合金化溶融亜鉛めっき付着量が片面で56g/m2 でめっき被膜中の鉄含有量が13重量%である合金化溶融亜鉛めっき鋼板GAと、同様の冷間圧延鋼板を素地鋼板とし、それに対して電気めっき法により亜鉛めっき付着量が片面で55g/m2 の電気亜鉛めっき鋼板EGとをそれぞれ複数個用意し、鋼片試料とした。
・加熱処理工程
次いで、上記の各鋼片試料をAc3点以上の温度に加熱するためにそれらに対して、加熱炉を用いて炉内温度920℃−5分保持にて熱処理を施した。この熱処理では、それに用いた加熱炉方式、炉内雰囲気ガス種、可燃性ガス種、加熱炉内の酸素濃度と露点の組み合わせについては、鋼片試料毎に図1および図2に示すものをそれぞれ適用して熱処理を施した。炉内雰囲気の露点DP(℃)と水蒸気量(vol %)とは、図3のグラフ或いは図4の表に示すように1対1の関係にあり、露点DP(℃)が上昇すると水蒸気量(vol %)も上昇する。この加熱処理工程では、図5乃至図8に示すように、加熱炉内における試料10の支持方法の影響を調べるために、4種類の異なる支持部材、すなわち20mmφの円柱状の支持部材12、断面6cm2 の三角柱状の支持部材14、円錐先端径が1mmの円錐状の支持部材16、断面8cm2 の四角柱状の支持部材18を用いて同じ加熱条件が適用された鋼片試料10をそれぞれ下から支持した。円柱状の支持部材12および三角柱状の支持部材14を用いた場合は、鋼片試料10との間で線接触となり、円錐状の支持部材16を用いた場合は、鋼片試料10との間で点接触となり、四角柱状の支持部材18を用いた場合は、鋼片試料10との間で面接触となる。ここで、上記図4に示す表は、「鋼の熱処理改訂5版」(日本鉄鋼協会編、昭和60年3月15日丸善株式会社発行)の第30頁表1・11に記載されたものであり、上記図3は図4の数値からグラフ化したものである。
・熱間プレス成形工程(急冷工程含む)
そして、上記各鋼片試料は、上記加熱炉で加熱しその加熱炉から取り出した後に直ちに、プレス成形を模擬するために用意された水冷機構を有する平板プレスの平坦な金型間において30秒間挟圧し急冷した。
Sample production / test material Thickness 2 mm containing 0.2 wt% C, 0.3 wt% Si, 1.3 wt% Mn, 0.01 wt% P for use in experiments X Cold rolled steel sheet of length 300mm x width 100mm is used as a base steel sheet. On the other hand, the amount of galvanized alloyed galvanized coating is 56g / m 2 on one side and the iron content in the plating film is 13% by weight. A certain alloyed hot-dip galvanized steel sheet GA and a similar cold-rolled steel sheet are used as a base steel sheet, and a plurality of electrogalvanized steel sheets EG each having a galvanized coating amount of 55 g / m 2 by electroplating. Prepared and used as a steel slab sample.
-Heat-treatment process Next, in order to heat each said steel piece sample to the temperature of Ac3 point or more, it heat-processed by holding | maintaining in-furnace temperature 920 degreeC-5 minutes using a heating furnace. In this heat treatment, the heating furnace system, the atmospheric gas type in the furnace, the flammable gas type, and the combination of the oxygen concentration and the dew point in the heating furnace are those shown in FIG. 1 and FIG. Applied and heat treated. The dew point DP (° C.) and the amount of water vapor (vol%) in the furnace atmosphere have a one-to-one relationship as shown in the graph of FIG. 3 or the table of FIG. 4, and when the dew point DP (° C.) increases, the amount of water vapor (Vol%) also increases. In this heat treatment step, as shown in FIGS. 5 to 8, in order to investigate the influence of the method of supporting the sample 10 in the heating furnace, four different support members, that is, a cylindrical support member 12 having a diameter of 20 mm, a cross section A steel piece sample 10 to which the same heating conditions were applied was respectively applied using a 6 cm 2 triangular columnar support member 14, a conical support member 16 having a cone tip diameter of 1 mm, and a square columnar support member 18 having a cross section of 8 cm 2. Supported from. When the columnar support member 12 and the triangular columnar support member 14 are used, line contact is made with the steel piece sample 10, and when the conical support member 16 is used, between the steel piece sample 10 and the steel piece sample 10. When the square pillar-shaped support member 18 is used, surface contact is made with the steel piece sample 10. Here, the table shown in FIG. 4 is the one described in Tables 1 and 11 on page 30 of "Steel Heat Treatment Revision 5th Edition" (edited by the Japan Iron and Steel Institute, published by Maruzen Co., Ltd. on March 15, 1985). FIG. 3 is a graph from the numerical values of FIG.
・ Hot press forming process (including rapid cooling process)
Each steel slab sample is sandwiched for 30 seconds between flat molds of a flat plate press having a water cooling mechanism prepared for simulating press forming immediately after being heated in the heating furnace and taken out from the heating furnace. Pressurized and cooled rapidly.

評価方法
・外観評価
上記平板プレスが施された各鋼片試料の表面状態を目視で観察し、表面状態の異常な酸化や、不均一の有無を評価した。図1および図2の加熱プレス後外観の欄に記入された◎印は鋼片試料10の表面である鉄亜鉛層および酸化亜鉛層または水酸化亜鉛層が非常に良好な表面状態、○印は良好、×印は不芳を示す。
・塗装密着性評価
上記平板プレスが施された各鋼片試料について化成処理(処理液:日本パーカライジング社製PBL−3080、処理条件:その処理液での標準条件)を施した後、さらに電着塗装(塗料:関西ペイント社製GT10、塗装膜厚:20μm、電圧および通電パターン:200Vのスロープ通電(0V〜200Vまで30秒間)、焼付:160℃×20分)を施し40℃イオン交換水に500時間浸漬した。次いで、塗装面に碁盤目試験(JISG3312 12.2.5)に記載の方法で碁盤目を入れた後でテープ剥離試験を行った。剥離面積が1%以下のものを合格とし、図1および図2の塗装密着性の欄に記入された◎印は非常に良好、○印はその合格(良好)を示すが、×印は不合格(不芳)を示す。
Evaluation Method / Appearance Evaluation The surface state of each steel slab sample subjected to the flat plate press was visually observed to evaluate whether the surface state was abnormally oxidized or non-uniform. 1 and FIG. 2 are marked in the column of the appearance after heating press are marked with a very good surface state of the iron zinc layer and the zinc oxide layer or the zinc hydroxide layer, which are the surface of the steel slab sample 10, Good, x indicates unsatisfactory.
-Coating adhesion evaluation Each steel slab sample subjected to the above flat plate press was subjected to chemical conversion treatment (treatment liquid: PBL-3080 manufactured by Nihon Parkerizing Co., Ltd., treatment conditions: standard conditions in the treatment liquid), and then electrodeposition Coating (paint: GT10 manufactured by Kansai Paint Co., Ltd., coating film thickness: 20 μm, voltage and energization pattern: 200 V slope energization (30 seconds from 0 V to 200 V), baking: 160 ° C. × 20 minutes), applied to 40 ° C. ion exchange water It was immersed for 500 hours. Next, a tape peeling test was performed after placing a grid pattern on the painted surface by the method described in the grid pattern test (JISG3312 12.2.5). Those with a peel area of 1% or less are accepted, and the mark ◎ marked in the paint adhesion column of FIGS. 1 and 2 is very good, the mark ○ indicates the pass (good), but the mark x is not. Indicates pass (bad).

評価結果
図1には、円柱状の支持部材12により鋼片試料10が支持されるという共通の支持条件が適用されるがそれ以外は異なる加熱条件で加熱された場合の、加熱状態とそれに対応する評価結果が示されている。この図1に示すように、合金化溶融亜鉛めっき鋼板GAと電気亜鉛めっき鋼板EGとの間においては、評価結果に差が認められない。次いで、電気炉で炉内雰囲気ガス種として窒素が用いられた場合と燃焼ガス炉で可燃性ガス種として天然ガス或いはプロパンガスが用いられた場合との間においても、評価結果に差が認められない。そして、加熱炉内において、酸素濃度が0容積%より高い加熱雰囲気、或いは酸素濃度が0容積%以上且つ露点DPが0℃以上の加熱雰囲気では、鋼片試料10の表面状態および塗装密着性において○印以上の一応の評価が得られる。又、酸素濃度が1容積%乃至5容積%の範囲の低酸素加熱雰囲気、或いは酸素濃度が1容積%より低くても露点DPが4℃以上の水蒸気が存在する雰囲気では、鋼片試料10の表面状態および塗装密着性において、◎印の非常に高い評価が得られる。
Evaluation results FIG. 1 shows a common support condition in which the steel piece sample 10 is supported by the columnar support member 12, but otherwise the heating state and the corresponding case when heated under different heating conditions. The evaluation results are shown. As shown in FIG. 1, there is no difference in the evaluation results between the galvannealed steel sheet GA and the electrogalvanized steel sheet EG. Next, there is a difference in the evaluation results between the case where nitrogen is used as the atmospheric gas type in the electric furnace and the case where natural gas or propane gas is used as the flammable gas type in the combustion gas furnace. Absent. In the heating furnace, in a heating atmosphere in which the oxygen concentration is higher than 0% by volume, or in a heating atmosphere in which the oxygen concentration is 0% by volume or more and the dew point DP is 0 ° C. or more, the surface condition and coating adhesion of the steel slab sample 10 A temporary evaluation above the ○ mark is obtained. Further, in a low oxygen heating atmosphere in which the oxygen concentration is in a range of 1% to 5% by volume, or in an atmosphere in which water vapor having a dew point DP of 4 ° C. or higher exists even if the oxygen concentration is lower than 1% by volume, A very high evaluation of ◎ is obtained in the surface condition and paint adhesion.

図2には、加熱炉、炉内雰囲気ガス種、可燃性ガス種、酸素濃度、水蒸気について共通の条件が適用されるが支持方法について異なる条件で加熱された場合の、支持状態とそれに対応する評価結果が示されている。すなわち、この図2には、可燃性ガス種がプロパンガスである燃焼ガス炉を用いて、酸素濃度が3容積%且つ水蒸気量が6容積%の燃焼ガス雰囲気で合金化溶融亜鉛めっき鋼板GAから成る鋼片試料を加熱処理する点は共通であるが、4種の異なる支持部材、すなわち線接触で鋼片試料10を支持する円柱状の支持部材12、同様に線接触で鋼片試料10を支持する三角柱状の支持部材14、点接触で鋼片試料10を支持する円錐状の支持部材16、面接触で鋼片試料10を支持する四角柱状の支持部材18を用いて熱処理した場合の、支持状態とそれに対応する評価結果が示されている。図2に示すように、加熱炉中で鋼片試料10が線接触或いは点接触にて円柱状の支持部材12、三角柱状の支持部材14、円錐状の支持部材16により支持される場合はそれぞれ場合は、鋼片試料10の表面状態および塗装密着性において◎印の非常に高い評価が得られる。しかし、加熱炉中で鋼片試料10が面接触にて四角柱状の支持部材18により支持される場合は、鋼片試料10の表面状態および塗装密着性において×印の不合格或いは不芳の低い評価しか得られない。   In FIG. 2, common conditions are applied to the heating furnace, the atmospheric gas species in the furnace, the combustible gas species, the oxygen concentration, and the water vapor. The evaluation results are shown. That is, in this FIG. 2, from a galvannealed steel sheet GA using a combustion gas furnace in which the combustible gas species is propane gas, in a combustion gas atmosphere having an oxygen concentration of 3% by volume and a water vapor amount of 6% by volume. Although the point which heat-processes the billet sample which consists of is common, four types of different support members, ie, the column-shaped support member 12 which supports the billet sample 10 by line contact, similarly, the billet sample 10 by line contact is carried out. When heat treatment is performed using a triangular prism-shaped support member 14 that supports, a conical support member 16 that supports the billet sample 10 by point contact, and a square columnar support member 18 that supports the billet sample 10 by surface contact, The support state and the corresponding evaluation results are shown. As shown in FIG. 2, when the billet sample 10 is supported by a columnar support member 12, a triangular columnar support member 14, and a conical support member 16 in a heating furnace by line contact or point contact, respectively. In this case, a very high evaluation of “◎” is obtained in the surface condition and paint adhesion of the steel slab sample 10. However, when the steel slab sample 10 is supported by the quadrangular columnar support member 18 in surface contact in the heating furnace, the surface state of the steel slab sample 10 and the coating adhesion are unacceptable or poor. Only an evaluation can be obtained.

上述のように、本実施例の熱間プレス用めっき鋼板の加熱処理方法によれば、プレス金型内で急冷して焼き入れを施す熱間プレスに先立ってめっき鋼板を加熱処理するために、酸素濃度が0容積%よりも高い雰囲気で鋼片試料10が加熱されることから、その鋼片試料10の表面にそのめっき材料の金属酸化物層すなわち酸化亜鉛層などのバリヤ層が形成されて加熱炉から取り出したときの急速酸化が好適に抑制されるので、十分な塗装密着性および耐蝕性を有する熱間プレス成形品が安定して得られる。   As described above, according to the heat treatment method of the hot-pressed plated steel sheet of the present embodiment, in order to heat-treat the plated steel sheet prior to the hot press that quenches and quenches in the press mold, Since the billet sample 10 is heated in an atmosphere in which the oxygen concentration is higher than 0% by volume, a barrier layer such as a metal oxide layer of the plating material, that is, a zinc oxide layer, is formed on the surface of the billet sample 10. Since rapid oxidation when taken out from the heating furnace is suitably suppressed, a hot press-formed product having sufficient coating adhesion and corrosion resistance can be stably obtained.

また、本実施例の熱間プレス用めっき鋼板の加熱処理方法によれば、酸素濃度が0容積%以上且つ露点が0℃以上の雰囲気で鋼片試料10が加熱されることから、たとえ加熱炉の酸素濃度が0容積%であっても露点が0℃以上のある程度の気中の水分の存在下で、鋼片試料10の表面にめっき材料を構成する金属の水酸化金属被膜である水酸化亜鉛層などがバリヤ層を構成することから、加熱炉から取り出したときの急速酸化が好適に抑制されるので、十分な塗装密着性および耐蝕性を有する熱間プレス成形品が安定して得られる。   In addition, according to the heat treatment method for a hot-pressed plated steel sheet of this example, the billet sample 10 is heated in an atmosphere having an oxygen concentration of 0% by volume or more and a dew point of 0 ° C. or more. In the presence of a certain amount of moisture in the air with a dew point of 0 ° C. or higher even if the oxygen concentration of the steel is 0% by volume, the hydroxylation is a metal hydroxide metallized film that forms the plating material on the surface of the steel piece sample 10 Since the zinc layer and the like constitute the barrier layer, rapid oxidation when taken out from the heating furnace is suitably suppressed, so that a hot press-formed product having sufficient coating adhesion and corrosion resistance can be stably obtained. .

また、本実施例の熱間プレス用めっき鋼板の加熱処理方法によれば、加熱雰囲気は、酸素濃度が1〜5容積%の範囲内の低酸素雰囲気とされると、鋼片試料10の表面にそのめっき材料を構成する金属の金属酸化物層すなわち酸化亜鉛層のバリヤ層が適切な厚みに形成されるので、加熱炉から取り出したときの急速酸化が好適に抑制されると同時に、その金属酸化物層などが厚くなり過ぎて塗装密着性に問題が生じることも好適に解消される。   Moreover, according to the heat processing method of the hot-pressed plated steel sheet of the present embodiment, when the heating atmosphere is a low oxygen atmosphere having an oxygen concentration in the range of 1 to 5% by volume, the surface of the slab sample 10 In addition, since the metal oxide layer of the metal constituting the plating material, that is, the barrier layer of the zinc oxide layer, is formed in an appropriate thickness, rapid oxidation when taken out from the heating furnace is preferably suppressed, and at the same time, the metal It is also preferable to eliminate the problem of coating adhesion due to the oxide layer becoming too thick.

また、本実施例の熱間プレス用めっき鋼板の加熱処理方法によれば、鋼片試料10は、合金化溶融亜鉛めっき鋼板GAや電気亜鉛めっき鋼板EGである亜鉛系めっき鋼板であることから、バリヤ層として、酸化亜鉛層或いは水酸化亜鉛層が形成されるので、加熱炉から取り出したときの急速酸化が好適に抑制される。   Moreover, according to the heat treatment method of the hot-pressed plated steel sheet of this example, the billet sample 10 is a zinc-based plated steel sheet that is an alloyed hot-dip galvanized steel sheet GA or an electrogalvanized steel sheet EG. Since the zinc oxide layer or the zinc hydroxide layer is formed as the barrier layer, rapid oxidation when taken out from the heating furnace is suitably suppressed.

また、本実施例の熱間プレス用めっき鋼板の加熱処理のために、ガス炉内の雰囲気ガス種として燃焼ガスが用いられる場合は、そのガス炉における可燃性ガスと空気との割合を変化させることにより、酸素濃度を簡単且つ容易に制御できる利点がある。   In addition, when the combustion gas is used as the atmospheric gas species in the gas furnace for the heat treatment of the hot-press plated steel sheet of the present embodiment, the ratio of the combustible gas and air in the gas furnace is changed. Thus, there is an advantage that the oxygen concentration can be controlled easily and easily.

また、本実施例の熱間プレス用めっき鋼板の加熱処理方法おいて、加熱炉の炉内において、鋼片試料(めっき鋼板)10は、それを支持する支持部材、すなわち、図5、図6、図7に示すように、円柱状の支持部材12、三角柱状の支持部材14、円錐状の支持部材16により線接触または点接触にて支持されるので、鋼片試料10の表面に酸化亜鉛層或いは水酸化亜鉛層などのバリヤ層が一層均一に形成される。また、図8に示すように、四角柱状の支持部材18により鋼片試料10が面接触にて支持される場合のように、その面接触部分を取り除いた残りの部分を加熱処理された鋼片試料10として用いる必要がない。   Further, in the heat treatment method for a hot-pressed plated steel sheet according to the present embodiment, a billet sample (plated steel sheet) 10 is a supporting member that supports it in the furnace of the heating furnace, that is, FIGS. As shown in FIG. 7, since it is supported by a cylindrical support member 12, a triangular prism-shaped support member 14, and a conical support member 16 in a line contact or a point contact, zinc oxide is applied to the surface of the steel slab sample 10. A barrier layer such as a layer or a zinc hydroxide layer is formed more uniformly. Further, as shown in FIG. 8, a steel piece in which the remaining part from which the surface contact portion is removed is heat-treated, as in the case where the steel piece sample 10 is supported by surface contact by a square columnar support member 18. It is not necessary to use as the sample 10.

また、本実施例の熱間プレス用めっき鋼板の加熱処理方法により加熱され、熱間プレスによりプレス成形および焼き入れされ、且つ必要に応じてスポット溶接された鋼板部材は、溶接品質が安定し、高強度が得られ、且つ高耐蝕性が得られるので、自動車の車体或いはその構成部品の一部を構成する鋼板部材の製造に適用されることにより、溶接品質が安定し且つ高剛性或いは高耐蝕性の自動車の車体或いはその構成部品が得られる。   Moreover, the steel plate member heated by the heat treatment method of the hot-pressed plated steel plate of this example, press-formed and quenched by hot press, and spot-welded as necessary, has a stable welding quality, High strength and high corrosion resistance can be obtained, so that it can be applied to the manufacture of steel plate members that make up part of the body of automobiles or its components, resulting in stable welding quality and high rigidity or high corrosion resistance. A car body or its components can be obtained.

以上、本発明の実施例を図面に基づいて詳細に説明したが、これ等はあくまでも一実施形態であり、本発明は当業者の知識に基づいて種々の変更、改良を加えた態様で実施することができる。   As mentioned above, although the Example of this invention was described in detail based on drawing, these are one Embodiment to the last, This invention is implemented in the aspect which added the various change and improvement based on the knowledge of those skilled in the art. be able to.

本発明の加熱方法に従って種々の条件で熱処理された鋼板の評価結果を、従来の加熱方法に従って加熱処理された鋼板の評価結果と対比させて示す図表である。It is a graph which compares the evaluation result of the steel plate heat-processed on various conditions according to the heating method of this invention with the evaluation result of the steel plate heat-processed according to the conventional heating method. 本発明の加熱方法に従って熱処理されるときの鋼板の異なる支持方法が採られたときの鋼板の評価結果を示す図表である。It is a graph which shows the evaluation result of the steel plate when the different support method of the steel plate when heat-processed according to the heating method of this invention is taken. 図1および図2において用いられる加熱雰囲気内の水蒸気量と加熱雰囲気の露点との関係を示す図ある。It is a figure which shows the relationship between the amount of water vapor | steam in the heating atmosphere used in FIG. 1 and FIG. 2, and the dew point of a heating atmosphere. 図1および図2において用いられる加熱雰囲気内の水蒸気量と加熱雰囲気の露点との関係を示す対応表である。3 is a correspondence table showing the relationship between the amount of water vapor in the heating atmosphere used in FIGS. 1 and 2 and the dew point of the heating atmosphere. 図2の実験において加熱処理のために円柱状の支持部材が鋼片試料を支持する状態を示す斜視図である。It is a perspective view which shows the state in which the column-shaped support member supports a steel piece sample for heat processing in the experiment of FIG. 図2の実験において加熱処理のために三角柱状の支持部材が鋼片試料を支持する状態を示す斜視図である。It is a perspective view which shows the state in which the triangular prism-shaped support member supports a steel piece sample for heat processing in the experiment of FIG. 図2の実験において加熱処理のために円錐状の支持部材が鋼片試料を支持する状態を示す斜視図である。It is a perspective view which shows the state in which a cone-shaped support member supports a steel piece sample for heat processing in the experiment of FIG. 図2の実験において加熱処理のために四角柱状の支持部材が鋼片試料を支持する状態を示す斜視図である。It is a perspective view which shows the state in which the square-column-shaped support member supports a steel piece sample for heat processing in the experiment of FIG.

符号の説明Explanation of symbols

10:鋼板試料
12:円柱状の支持部材
14:三角柱状の支持部材
16:円錐状の支持部材
18:四角柱状の支持部材
10: Steel plate sample 12: Columnar support member 14: Triangular columnar support member 16: Conical support member 18: Square columnar support member

Claims (6)

めっき鋼板をプレス金型内で急冷して焼き入れを施す熱間プレスに先立って該めっき鋼板を予め加熱するための熱間プレス用めっき鋼板の加熱処理方法であって、
該めっき鋼板を、酸素濃度が0容積%よりも高い雰囲気で加熱することを特徴とする熱間プレス用めっき鋼板の加熱処理方法。
A heat treatment method for a hot-pressed plated steel sheet for pre-heating the plated steel sheet prior to hot pressing in which the plated steel sheet is quenched and quenched in a press die,
A method of heat-treating a plated steel sheet for hot pressing, wherein the plated steel sheet is heated in an atmosphere having an oxygen concentration higher than 0% by volume.
めっき鋼板をプレス金型内で急冷して焼き入れを施す熱間プレスに先立って該めっき鋼板を予め加熱するための熱間プレス用めっき鋼板の加熱処理方法であって、
該めっき鋼板を、酸素濃度が0容積%以上且つ露点が0℃以上の雰囲気で加熱することを特徴とする熱間プレス用めっき鋼板の加熱処理方法。
A heat treatment method for a hot-pressed plated steel sheet for pre-heating the plated steel sheet prior to hot pressing in which the plated steel sheet is quenched and quenched in a press die,
A method of heat-treating a plated steel sheet for hot pressing, comprising heating the plated steel sheet in an atmosphere having an oxygen concentration of 0% by volume or more and a dew point of 0 ° C or more.
また、前記酸素濃度は1〜5容積%の範囲内の低酸素雰囲気である請求項1または2の熱間プレス用めっき鋼板の加熱処理方法。   The heat treatment method for a hot-pressed plated steel sheet according to claim 1 or 2, wherein the oxygen concentration is a low oxygen atmosphere within a range of 1 to 5% by volume. 前記めっき鋼板は、亜鉛系めっき鋼板である請求項1乃至3のいずれかの熱間プレス用めっき鋼板の加熱処理方法。 The heat treatment method for a hot-pressed plated steel sheet according to any one of claims 1 to 3, wherein the plated steel sheet is a zinc-based plated steel sheet. 前記加熱処理は、ガス炉内の燃焼ガス雰囲気で行われるものである請求項1乃至4のいずれかの熱間プレス用めっき鋼板の加熱処理方法。 The heat treatment method for a hot-pressed plated steel sheet according to any one of claims 1 to 4, wherein the heat treatment is performed in a combustion gas atmosphere in a gas furnace. 前記加熱処理は、前記めっき鋼板が支持部材により線接触または点接触にて支持された状態で行われるものである請求項1乃至5のいずれかの熱間プレス用めっき鋼板の加熱処理方法。
The said heat processing is a heat processing method of the plated steel plate for hot press in any one of the Claims 1 thru | or 5 which are performed in the state by which the said plated steel plate was supported by the contact member by the line contact or the point contact.
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