JP2725537B2 - Method for producing superior galvannealed steel sheet in impact resistance adhesiveness - Google Patents

Method for producing superior galvannealed steel sheet in impact resistance adhesiveness

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JP2725537B2
JP2725537B2 JP4235942A JP23594292A JP2725537B2 JP 2725537 B2 JP2725537 B2 JP 2725537B2 JP 4235942 A JP4235942 A JP 4235942A JP 23594292 A JP23594292 A JP 23594292A JP 2725537 B2 JP2725537 B2 JP 2725537B2
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steel sheet
steel
temperature
impact resistance
furnace
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保 土岐
一英 大島
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住友金属工業株式会社
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【発明の詳細な説明】 DETAILED DESCRIPTION OF THE INVENTION

【0001】 [0001]

【産業上の利用分野】本発明は、優れためっき密着性を有し、種々の用途、例えば、自動車用鋼板の内板はもとより、外板としても適用可能な、耐衝撃密着性に優れた合金化溶融亜鉛めっき鋼板の製造方法に関する。 BACKGROUND OF THE INVENTION This invention has excellent coating adhesion, various applications, for example, as well the inner plates of steel sheets for automobiles, which can be applied as an outer plate, an excellent impact resistance adhesiveness the method of manufacturing a galvannealed steel sheet.

【0002】 [0002]

【従来の技術】合金化溶融亜鉛めっき鋼板 (以下「GA BACKGROUND OF THE INVENTION galvannealed steel sheet (hereinafter referred to as "GA
鋼板」と称する) は、塗装後の耐食性および塗膜密着性に優れた材料であるため、従来から建材や家電製品などの用途のほかに、自動車車体用の防錆鋼板としても使用されている。 Referred to as steel sheet ") are the material excellent in corrosion resistance and paint adherence after coating, in addition to applications such as building materials and appliances conventionally, it has also been used as a rustproof steel sheet for automobile bodies . 自動車車体に適用する場合、以前は、孔あき腐食対策用として、例えば、フロアー、メンバー、インナーパネルといった内板用材料として使用されてきたが、最近では、GA鋼板製造技術の向上と防錆目標の高度化が相まって、表面欠陥や塗装性などに対して非常に厳しい外板用材料 (例、ドアー、フード、フェンダー、 When applied to an automobile body, previously, for the perforated corrosion protection, for example, floor, members have been used as a plate material among such inner panel, in recent years, improvement and rust goals GA steel manufacturing techniques coupled sophistication of surface defects and paintability very tough outer skin material against such (eg, door, hood, fenders,
シル) としても、既存の電気亜鉛めっき鋼板および電気亜鉛合金めっき鋼板と同様に適用されている。 Even sill), it has been applied similarly to the conventional electro-galvanized steel sheet and electrolytic zinc alloy plated steel sheet.

【0003】ところで、少量のPを添加したP添加鋼は、Pの添加により強度が著しく高まることから、通称P添加ハイテン鋼と呼ばれ、自動車車体用鋼板の高張力化、軽量化の要求に伴って、自動車車体の内外板に25〜 Meanwhile, the P-added steel obtained by adding a small amount of P, since the strength is significantly enhanced by the addition of P, commonly called P added-tensile steel, high tensile of automobile body steel sheet, the demand for weight reduction accompanied by, 25 to the inner and outer plate of an automobile body
45 kg/mm 2のレベルで使用されるようになってきた。 45 has come to be used at a level of kg / mm 2. 従って、GA鋼板の母材鋼板としてもP添加鋼が使用されることがある。 Therefore, there is the P-added steel is used as the base material steel plate of the GA steel sheet.

【0004】自動車車体の外板用材料の外面 (塗装面) [0004] The outer surface of the automobile body of the outer plate for the material (painted surfaces)
側では、その内面側とは異なり、走行時に飛来する石、 On the side, unlike its inner surface side, flying to the time of running stone,
砂などによりいわゆるチッピング衝撃を受ける。 The so-called chipping impacted by such as sand. ところが、GA鋼板のめっき皮膜は、FeとZnの金属間化合物であり、純亜鉛めっきに比べて硬度が高く、かなり脆いため、前記チッピング衝撃によりめっき皮膜が下地鋼板から剥離し易い傾向にある。 However, the plating film of GA steel is an intermetallic compound of Fe and Zn, high hardness as compared with pure zinc plating, since quite fragile, the plated film by the chipping impact tends to easily peel from the substrate steel sheet.

【0005】特に、北米、カナダ等の寒冷地においては、低温(−20〜−40℃)のために塗膜が硬化して、めっき皮膜への拘束力が高くなるとともに、凍結防止のために路面上に散布される岩塩によりチッピングを生じるために、めっき皮膜の剥離が極めて発生し易い。 In particular, North America, in the cold cold locations, such as Canada, and curing the coating film due to low temperatures (-20 to-40 ° C.), with binding to the plating film is high, to prevent freezing in order to produce a chipping by rock salt to be sprayed on the road surface, easy peeling of the plating film is extremely generated.
めっき皮膜の剥離が発生した部分は、その周りに残存するめっき皮膜によるある程度の犠牲防食作用を期待することはできるものの、それには限界があり、最終的には自動車車体の外板にGA鋼板を用いた効果が失われてしまう。 Partial peeling occurs in plating film, although it is possible to expect a certain amount of sacrificial protection action by plating coating remaining around it, it has a limit, eventually a GA steel outer panel of an automobile body effect of the use is lost.

【0006】GA鋼板のめっき密着性の改善については、従来から、成形時の皮膜剥離 (パウダリングまたはフレーキング) を軽減する目的から、合金化温度やヒートパターンといったGA鋼板の操業条件の影響などに関する研究が行われ (日本鉄鋼協会講演大会: CAMP-ISIJ [0006] For improvement of the coating adhesion of the GA steel sheet, conventionally, for the purpose of reducing the coating exfoliation during molding (powdering or flaking), and the impact of operating conditions GA steel such alloying temperature and heat pattern studies have been made as to (Japan Iron and steel Institute lecture tournament: CAMP-ISIJ
vol. 1 (1988): 655頁) 、また特公平2−39585 号公報に提案されているように、めっき皮膜の構造、生成形態、組成などを限定することも試みられている。 vol 1 (1988):. 655 pp), also as proposed in Japanese Patent Kokoku 2-39585, the structure of the plated film, produced form, attempts have been made to limit the composition and the like.

【0007】 [0007]

【発明が解決しようとする課題】しかし、GA鋼板の衝撃時のめっき皮膜密着性、とりわけ低温での耐衝撃密着性は、前記のような成形時のめっき皮膜剥離とは異なる。 [SUMMARY OF THE INVENTION] However, the plating film adhesion upon impact of GA steel, especially impact resistance adhesiveness at low temperature, different from the plating film peeling at the time of the like of the molding. 本発明者らの調査では、前記方法によっても、GA The study of the present inventors, even by the method, GA
板では、主に北米で自動車車体外板に現在使われている電気亜鉛めっき鋼板のような充分な耐衝撃密着性の性能を得ることができなかった。 The steel plate could not be obtained mainly sufficient impact adhesion performance, such as electro-galvanized steel sheet currently used in the automobile body external panel in North America.

【0008】特に、P添加鋼をめっき母材とするGA鋼板は、一般のAlキルド低炭素鋼や深絞り成形用の極低炭素Ti(Nb)添加鋼を母材とするGA鋼板に比べ、同一めっき組成 (合金化度) において、成形加工時の耐パウダリング (粉状剥離) 性能は同等以上の性能を示すものの、 [0008] In particular, GA steel sheet to plating mother P addition steel material, a general Al-killed ultra low carbon Ti of low carbon steel and deep drawing molding (Nb) added steel compared to GA steel sheet as a base material, in the same plating composition (Fe content), although powdering resistance during molding (powdery peeling) performance indicates a performance equal to or higher than,
耐衝撃密着性は劣り、その改善が要望されている。 Impact resistance adhesiveness is inferior, and improvement is demanded.

【0009】特開平2−97653 号公報には、自動車車体外板で問題となる耐衝撃密着性とは異なるが、鋼板表面の結晶粒界への亜鉛の拡散侵入を利用してFe濃度が8〜 [0009] Japanese Patent Laid-Open No. 2-97653, is different from the impact resistance adhesiveness, which is a problem in automotive body sheet, Fe concentration by utilizing the diffusion and penetration of zinc into the crystal grain boundaries of the steel sheet surface 8 ~
17%(重量%、以下も特に指定しない限り、%は重量% 17% (wt%, unless otherwise specified even less,% weight%
を意味する) のGA鋼板のエナメルヘアー (即ち、塗装後のめっき鋼板の剪断応力を伴う変形過程における各層間の密着性能が最も低い部分での界面剥離現象) の発生を抑制する技術が提案されている。 Enamel hair of GA steel sheet meaning) (i.e. a technique of suppressing the occurrence of interfacial peeling phenomenon) at the lowest part adhesion performance of each layer in the deformation process involving shearing stress of the plated steel sheet after painting have been proposed ing.

【0010】この方法は、素地鋼板に対しZnが粒界に比較的侵入し易い極低炭素Ti(Nb)添加鋼、低炭素鋼などをめっき母材とする場合には、エナメルヘアーの発生がある程度抑制されるが、粒界にPが偏析し、Znの侵入量の少ないP添加鋼を母材とする場合には効果が少なく、ましてや、ここで問題としている厳しい低温耐衝撃密着性に対しては、鋼種を問わずほとんど効果がない。 [0010] This method, Zn respect basis steel sheet is relatively enters the grain boundary easily ultra low carbon Ti (Nb) added steel, when the plating base material such as low carbon steel, the generation of enamel hair Although to some extent suppressed, P segregates at grain boundaries, the effect is small in the case of the Zn from entering a small amount of P-containing steel as a base material, let alone to severe cold impact resistance adhesiveness which is at issue here Te has little effect regardless of the type of steel.

【0011】GA鋼板、特にP添加鋼を母材とするGA [0011] GA steel sheet, GA, especially the P-added steel as a base material
鋼板の低温での耐衝撃密着性を、その他の重要な性能であるプレス成形性 (プレス加工時の耐パウダリング性) The impact resistance adhesiveness at low temperature of the steel sheet, other important performance is that the press formability (powdering resistance at the time of press working)
を損なうことなく改善することは、自動車車体外板として使用する際の防錆力向上のために重要な課題である。 Be improved without impairing is an important issue for the rust prevention improvement in use as automotive body sheet.

【0012】本発明の目的は、密着性に優れ、P添加鋼を母材とした場合であっても耐衝撃密着性、とりわけ低温での耐衝撃密着性に優れた、自動車車体の内板用はもとより、外板用にも適用可能な、GA鋼板の製造方法を提供することである。 An object of the present invention is excellent in adhesion, impact resistance adhesiveness even when the P-containing steel as a base material, especially excellent impact resistance adhesiveness at low temperatures, for inner plates of car bodies as well, even for the outer skin that can be applied, it is to provide a method for producing a GA steel.

【0013】 [0013]

【課題を解決するための手段】本発明者らは、耐衝撃密着性が特に劣化し易いP添加鋼を母材とするGA鋼板について、その原因と改善策について検討し、次のような知見を得た。 The present inventors have SUMMARY OF THE INVENTION may, for GA steel sheet to easily P added steel deteriorates impact resistance adhesiveness is particularly the base material, and examined the causes and remedies, the following knowledge It was obtained. P添加鋼は、一般の低炭素鋼、極低炭素鋼に比べ、合金化処理時のFe、Zn合金化反応速度が遅く、 P addition steel is generally a low-carbon steel, compared with the ultra low carbon steel, during alloying Fe, slow Zn alloying reaction rate,
同一昇温速度、ヒートパターンで合金化した場合には、 Same heating rate, when alloyed by a heat pattern,
マクロ的な合金化度 (Fe%) が同じでも、生成する合金層が異なる。 Macroscopic Fe content (Fe%) is also the same, alloy layer to generate different.

【0014】例えば、一般の低炭素鋼をAl濃度0.10%の溶融亜鉛めっき浴中で溶融めっき後、Fe 8〜11%に合金化した場合、鋼板/めっき界面には表層よりFe濃度の高いΓ相 (Fe 3 Zn 10 )、或いはΓ 1相 (Fe 5 Zn 21 )が形成されるが、P添加鋼では、同じ合金化度でもΓ相やΓ 1相はあまり生成しない。 [0014] For example, after a general low-carbon steel hot dipping of Al concentration 0.10% of molten zinc plating bath, when alloyed Fe 8 to 11%, higher Fe concentration than the surface layer of the steel sheet / plating interface Γ phase (Fe 3 Zn 10), or is gamma 1-phase (Fe 5 Zn 21) is formed in the P-added steel, it does not generate much even gamma phase or gamma 1-phase with the same alloyed. Γ相は脆性が高く、プレス加工時の圧縮−引張り変形による耐パウダリング性を劣化させるので、P添加鋼はこの点において有利であり、実際、良好な耐パウダリング性を示す。 Γ phase has high brittleness, compressive during press working - so degrades the powdering resistance by tensile deformation, P-added steel is advantageous in this respect, in fact, show a good powdering resistance.

【0015】しかし、本発明者らの調査によれば、P添加鋼をめっき母材とするGA鋼板の鋼板/めっき界面は、Γ相、Γ 1相が形成されにくい反面、非常に平滑な構造を有し、そのために耐衝撃密着性に劣ることが判明した。 [0015] However, according to the investigation of the present inventors, the steel sheet / plating interface GA steel sheet a plating base material of P addition steel, gamma phase, contrary less likely to be gamma 1-phase is formed and very smooth structure the a, poor in impact resistance adhesiveness has been found for it. この界面付近の構造は、めっき浴への侵入時の鋼板温度、めっき浴中Al濃度、めっき浴温度などの操業因子によっても変化する。 The structure near the interface, the steel sheet temperature at the time of intrusion of the plating bath, Al concentration in the plating bath, also vary according to operating factors such as the plating bath temperature. しかし、一般的な操業範囲 (浴中Al濃度0.08〜0.15%、侵入時の鋼板温度 450〜550 However, typical operating range (bath Al concentration 0.08 to 0.15%, the steel sheet temperature at the time of intrusion 450-550
℃) ではその影響は小さく、めっき操業因子によるGA ° C.) in the effect is small, GA by plating operations factor
鋼板、特にP添加鋼を母材とするGA鋼板の耐衝撃密着性の改善は困難である。 Steel, in particular improved impact resistance adhesiveness of GA steel sheet as a base material for P-containing steel is difficult.

【0016】さらに検討した結果、鋼板を溶融めっき前に、無酸化炉内である程度前酸化させ、次いで還元した後、所定のめっきを施し、急速加熱にて合金化処理すると、耐パウダリング性を損なうことなく、GA鋼板の耐衝撃密着性が著しく向上することを見出した。 Furthermore considering a result, the steel sheet before hot dipping, non-oxidizing furnace in to some extent pre-oxidation, then after reduction, subjected to a predetermined plating, when an alloying treatment at rapid heating, the powdering resistance without compromising found that impact resistance adhesiveness of GA steel is remarkably improved. この方法による耐衝撃密着性の向上は、耐衝撃密着性が劣化し易いP添加鋼板を母材とする場合に特に顕著であるが、低炭素鋼板や極低炭素鋼板を母材とするGA鋼板についても有効であることも判明した。 This method improves the impact resistance adhesiveness by is particularly noticeable when the easy P added steel impact resistance adhesiveness is deteriorated as the base material, GA steel sheet of low carbon steel plate or ultra low carbon steel as a base material for also found it is effective.

【0017】本発明は上記知見に基づき完成したもので、「鋼板に合金化溶融亜鉛めっきを連続的に施すにあたり、前焼鈍炉内の予熱工程において鋼板表面の酸化皮膜量が0.1〜5g/m 2となるように前酸化を行った後、還元工程で還元処理した鋼板に所定量の溶融亜鉛めっきを付着させた後、30℃/sec以上の昇温速度で鋼板温度 420 [0017] The present invention has been completed based on the above findings, the galvannealed Upon continuously subjected to "steel, oxide film of the steel sheet surface in a preheating step prior to the annealing furnace 0.1-5 g / m after pre-oxidation to be 2, after depositing a predetermined amount of molten zinc plating reduction treated steel sheet in the reduction step, the steel sheet temperature at 30 ° C. / sec or more Atsushi Nobori rate 420
〜700 ℃の温度領域内に加熱し、この温度領域内で熱処理して合金化を行うことを特徴とする、耐衝撃密着性に優れたGA鋼板の製造方法」を要旨とする。 Was heated to to 700 ° C. in a temperature region, this was heat-treated at a temperature region and performing alloying, the manufacturing method "subject matter excellent GA steel impact adhesion.

【0018】 [0018]

【作用】本発明のGA鋼板の製造方法における母材鋼板の鋼種は特に限定されない。 [Action] steels of the base material steel plate in the manufacturing method of the GA steel sheet of the present invention is not particularly limited. 即ち、GA鋼板の製造に利用されている任意の種類の鋼種でよく、P添加鋼、低炭素鋼 (例、アルミキルド低炭素鋼) 、極低炭素鋼 (例、 That can be any kind of steels that are used in the manufacture of GA steel, P-added steel, low carbon steel (e.g., aluminum killed low carbon steel), ultra-low carbon steel (e.g.,
深絞り用の極低炭素TiまたはNb添加鋼) などが例示される。 Such as deep ultra low carbon Ti or Nb added steel for stop) is illustrated. P添加鋼とは、Pを意図的に添加した鋼であって、 The P-added steel, a steel that is intentionally added to P,
通常はP含有量が0.03%以上、0.2 %以下である。 Normally P content of 0.03% or more, 0.2% or less. P添加高張力鋼板は、一般にP添加鋼を熱間圧延、酸洗および冷間圧延することにより製造される。 P added high-strength steel sheet, generally P-added steel hot-rolled, is produced by pickling and cold rolling.

【0019】本発明の方法は、GA鋼板の製造に従来より使用されている連続溶融亜鉛めっきラインを利用して実施することができる。 The process of the present invention may be implemented using a continuous galvanizing line, which is conventionally used in the manufacture of GA steel. GA鋼板の連続製造は、一般に前焼鈍工程→溶融亜鉛めっき工程→合金化工程を経て製造される。 Continuous production of GA steel sheet is generally produced through a pre-annealing step → hot-dip galvanizing process → alloying step. 使用する鋼板は、前焼鈍工程の前に、常法により表面を洗浄する。 Steel sheet to be used, prior to the pre-annealing step, cleaning the surface by a conventional method. 洗浄は、アルカリ脱脂、或いはアルカリ脱脂と酸洗(塩酸または硫酸など)により行うのが普通である。 Washing, alkaline degreasing, or is generally performed by alkaline degreasing and pickling (such as hydrochloric acid or sulfuric acid).

【0020】前焼鈍工程は、前酸化炉と還元炉とからなる前焼鈍炉内で行われる。 [0020] before the annealing step is carried out in front before consisting of oxidation furnace and the reduction furnace annealing furnace. 前酸化炉では、鋼板の表面浄化を兼ねて鋼板を弱酸化性雰囲気で加熱し、鋼板表面に薄い酸化皮膜を形成する。 The pre-oxidation furnace, the steel sheet also serves as a surface cleaning of the steel sheet is heated in a weak oxidizing atmosphere to form a thin oxide film on the steel sheet surface. 代表的な前酸化炉は無酸化炉と呼ばれているものであり、無酸化炉の前に鋼板を予熱する予熱炉を設けることもある。 Typical prior to oxidation reactor are those which are called non-oxidizing furnace, there also be provided a preheating furnace for preheating the steel sheet before the non-oxidizing furnace. 本発明においては、還元炉の前の無酸化炉や予熱炉で行われる加熱をすべて含めて予熱工程と称する。 In the present invention, it referred to as preheating step including all heating performed in a non-oxidizing furnace and the preheating furnace prior to the reduction furnace. 次いで、還元炉で鋼板表面の酸化鉄の還元を行い、表面を活性化するとともに、焼鈍または焼ならしを行う (還元工程) 。 Next, by reduction of the iron oxide of the steel sheet surface in the reduction furnace, as well as activate the surface, performing the normalizing annealing or tempering (reduction step).

【0021】本発明によれば、アルカリ脱脂などにより表面を洗浄した鋼板を、前焼鈍炉内の予熱工程において弱酸化性雰囲気中にて予熱し、鋼板表面の酸化皮膜量が According to the present invention, the steel sheet surface was washed by alkali degreasing, prior to preheating in a weak oxidizing atmosphere in the preheating step of the annealing furnace, the oxide film of the steel sheet surface
0.1〜5g/m 2 、好ましくは 0.3〜3g/m 2となるように前酸化を行う。 0.1-5 g / m 2, preferably performs pre-oxidation so that 0.3 to 3 g / m 2. 酸化皮膜量は、重量法、X線回折法などにより測定できる。 Amount oxide film, a weight method, measured by X-ray diffraction method. 従来の溶融亜鉛めっきラインにおける無酸化炉でも、鋼板にごく薄い酸化皮膜は形成されるが、酸化皮膜量は0.1 g/m 2未満である。 In a non-oxidizing furnace in the conventional galvanizing line, the very thin oxide film on the steel sheet are formed, the amount of oxide film is less than 0.1 g / m 2. 予熱工程で酸化皮膜量が 0.1〜5g/m 2となるように前酸化を行うには、 In performing a pre-oxidized as anodized coating in the preheating step is 0.1-5 g / m 2, the
予熱工程の加熱炉内の雰囲気 (空燃比) と加熱温度を制御すればよい。 Atmosphere in the heating furnace of the preheating step may be controlled (the air-fuel ratio) and the heating temperature. 例えば、上記範囲内の皮膜量の酸化皮膜を形成するには、空燃比は 1.0〜1.3 の範囲内、加熱温度は鋼板温度で 500〜650 ℃の範囲内とすることが好ましい。 For example, to form an oxide film of the coating amount in the above range, the air-fuel ratio is in the range of 1.0 to 1.3, the heating temperature is preferably in the range of 500 to 650 ° C. at a steel sheet temperature.

【0022】予熱工程での加熱炉の種類は、上記酸化が可能な炉であればよく特に限定されないが、例えば、ガス燃焼炉、直火加熱炉などが例示される。 The type of furnace in the preheating step is not particularly limited as long a furnace capable of the oxidation, for example, a gas combustion furnace, and direct flame heating furnace is exemplified. この加熱炉としては、従来の溶融亜鉛めっきラインに設置されている無酸化炉または予熱炉と無酸化炉をそのまま使用してもよく、或いは別に専用の加熱炉を還元炉の前に設置してもよい。 As the heating furnace installed may a conventional molten zinc-free oxidizing furnace is installed in the plating line or a preheating furnace and a non-oxidizing furnace used as it, or a furnace dedicated to another prior to the reduction furnace it may be.

【0023】前酸化での酸化皮膜量が0.1 g/m 2未満では、後述のように急速加熱により合金化処理した場合であっても、得られたGA鋼板の耐衝撃密着性の向上が認められない。 [0023] In the previous amount oxide film is less than 0.1 g / m 2 in the oxidation, even when the alloying treatment by rapid heating as described later, observed improvements in impact resistance adhesiveness of the resulting GA steel It is not. 一方、酸化皮膜量が5g/m 2を超えると、その後の還元工程で酸化皮膜が充分に還元されないためか、耐衝撃密着性がかえって劣化し、耐パウダリング性やめっき外観も不良となる。 On the other hand, the amount of oxide film is more than 5 g / m 2, probably because the subsequent oxide film in the reduction step are not sufficiently reduced, impact resistance adhesiveness is deteriorated rather, it is poor powdering resistance and plating appearance.

【0024】この前酸化の後、前焼鈍炉内の還元炉において鋼板を高温の還元雰囲気に保持し、前酸化で生じた酸化層を還元して表面を活性化すると共に、焼なましまたは焼ならしを行う。 [0024] After this pre-oxidation, with prior steel sheet in reduction furnace annealing furnace maintained at a high temperature reducing atmosphere to activate the surface by reducing the oxidized layer generated by pre-oxidation, annealing or tempering break-in carried out. この還元工程の操業条件 (炉内雰囲気、温度、処理時間) は特に限定されず、従来と同様でもよいが、前酸化での酸化量が従来より多いため、25 Operating conditions of this reduction step (furnace atmosphere, temperature, treatment time) is not particularly limited, and may be the same as the conventional, but because the oxidation amount of the previous oxidation is greater than conventional, 25
〜30% H 2 +N 2雰囲気で、温度750 〜850 ℃、時間60〜12 In ~30% H 2 + N 2 atmosphere at a temperature 750 to 850 ° C., time 60 to 12
0 秒とすることが好ましい。 It is preferable that the 0 seconds. その後、鋼板は冷却帯を経て大気に触れることなく、溶融亜鉛めっき浴に導かれる。 Thereafter, the steel sheet is not exposed to the air through the cooling zone, it is led to the hot-dip galvanizing bath.

【0025】溶融亜鉛めっきも通常の条件下で実施すればよい。 [0025] may be carried out hot-dip galvanizing even under normal conditions. 例えば、浴中Al濃度は0.08〜0.15%程度、侵入時の鋼板温度は 450〜550 ℃程度が好ましい。 For example, bath Al concentration of about .08 to .15%, the steel sheet temperature at the time of intrusion is preferably about 450 to 550 ° C.. めっき付着量の制御はガスワイピングなどの慣用手段により実施でき、それにより所定量の亜鉛が付着した溶融亜鉛めっき鋼板が得られる。 Control of coating weight can be carried out by conventional means such as gas wiping and thereby hot-dip galvanized steel sheet a predetermined amount of zinc is attached, it is obtained.

【0026】溶融亜鉛めっきを施した鋼板を、次いで、 [0026] The steel sheet was subjected to hot-dip galvanized, then,
合金化炉において、30℃/sec以上の昇温速度で鋼板温度 In the alloying furnace, the steel sheet temperature at 30 ° C. / sec or more Atsushi Nobori rate
420〜700 ℃の温度領域内に急速加熱し、この温度領域内で熱処理して合金化を行い、GA鋼板を得る。 Rapidly heated to four hundred twenty to seven hundred ° C. temperature region, it performs alloying by heat treatment at this temperature region, obtain the GA steel sheet. この急速加熱は、鋼板がめっき付着量制御手段 (通常はガスワイピング装置) を経た後の初期加熱 (昇温時) に行われ、この状態ではめっきの上層にはZnのη相のみが残存している。 This rapid heating is (usually gas wiping apparatus) steel sheet coating weight control unit made to initial heating (in heating) after undergoing only η phase Zn is left on the upper layer of plating in this state ing. この状態で上記の急速加熱をすることにより、耐衝撃密着性の改善効果が現れる。 By rapid heating of the in this state, the effect of improving impact resistance adhesiveness appears.

【0027】この時の昇温速度が30℃/sec未満では、前酸化量がどの程度であっても、耐衝撃密着性の改善効果は全く認められない。 The heating rate at this time is less than 30 ° C. / sec, even how the previous oxidation amount, the effect of improving the impact resistance adhesiveness is not observed at all. また、たとえ30℃/sec以上の昇温速度で急速加熱しても、合金化温度が鋼板温度で420 ℃ Further, even if rapid heating at even 30 ° C. / sec or higher heating rate, 420 ° C. alloying temperature at a steel sheet temperature
より低いと、耐衝撃密着性の改善効果は認められない。 If lower, the effect of improving the impact resistance adhesiveness is not observed.
一方、この温度が700 ℃を超えると、合金化が進みすぎ、耐パウダリング性などの性能が劣化する。 On the other hand, if the temperature exceeds 700 ° C., too proceeds alloying, the performance of such powdering resistance deteriorates.

【0028】合金化炉の加熱手段としては、ガス燃焼加熱、輻射加熱、直火加熱バーナー、通電加熱、高周波誘導加熱など従来より利用されてきたいずれの方式でもよい。 Examples of the heating means of the alloying furnace, gas fired heating, radiant heating, direct flame heating burners, electrical heating may be any method that has been used conventionally, such as high frequency induction heating. また、合金化熱処理時のヒートパターンは、その初期過程での昇温速度が上記条件を満たす限り、その後のヒートパターンは特に制限されない。 Further, heat pattern during alloying heat treatment, as long as heating rate at the initial process satisfies the above conditions, then the heat pattern is not particularly limited. 鋼板温度 420〜70 Steel plate temperature 420-70
0 ℃の温度領域内で、合金化炉の滞留時間 (熱処理時間) やめっき付着量に応じて所望の合金化度が得られるように合金化温度やヒートパターンを選択すればよい。 At 0 ℃ temperature region may be selected alloying temperature and heat pattern as desired alloying degree depending on the residence time of the alloying furnace (heat treatment time) and coating weight is obtained.
合金化度は特に限定されないが、通常はFe含有量8〜12 Alloyed is not particularly limited, usually Fe content 8-12
%の範囲内に管理する。 To manage within the scope percent.

【0029】こうして製造されたGA鋼板は、その後溶融亜鉛めっきライン内で化成処理を施してから製品化してもよい。 [0029] Thus GA steel produced may be commercialized after subjected to chemical conversion treatment in the subsequent galvanizing line. 化成処理としては、塗膜密着性を高めるリン酸塩処理、或いは耐食性を高めるクロメート処理が代表的であり、これらを併用してもよい。 The chemical conversion treatment, a phosphate treatment for improving coating adhesion, or chromate treatment for increasing the corrosion resistance is typically these may be used in combination.

【0030】図1に、P含有量0.06%のP添加鋼板をめっき母材とするGA鋼板の前酸化における酸化皮膜量と低温での耐衝撃密着性との関係について実験結果で示す。 [0030] FIG. 1 shows the experimental results for the relation between the impact resistance adhesiveness with the oxide film amount and the low temperature before oxidation of GA steel sheet of the P content 0.06% P addition steel and the plating base material. 酸化皮膜量は、予熱工程で使用した無酸化炉内の雰囲気 (空燃比) および予熱温度を変化させることにより変動させた。 Amount oxide film was varied by changing the atmosphere (air) and the preheating temperature of the non-oxidizing furnace used in the preheating step. めっき後の合金化処理は520 ℃で行い、その際の昇温速度は20℃/sec (破線) および80℃/sec (実線) とした。 Alloying treatment after plating was carried out at 520 ° C., heating rate at that time was 20 ° C. / sec (broken line) and 80 ° C. / sec (solid line). 耐低温衝撃密着性は、実施例1に記載したのと同じ方法で評価した。 Low-temperature impact adhesion was evaluated in the same manner as described in Example 1.

【0031】図1に示した結果からわかるように、合金化初期段階での昇温速度が20℃/secと遅い場合には、前酸化を皮膜量 0.1〜5g/m 2の範囲内の量で行っても、耐衝撃密着性の改善はほとんど得られない。 [0031] As can be seen from the results shown in FIG. 1, an amount in the case where the heating rate of the alloying initial stage 20 ° C. / sec and slow, the pre-oxidation of the coating amount 0.1-5 g / m 2 range be carried out in an improvement in impact resistance adhesiveness is hardly obtained. これに対し、 On the other hand,
この昇温速度が80℃/secと急速加熱により合金化処理を行った場合には、前酸化の皮膜量が0.1 g/m 2以上になると耐衝撃密着性が無酸化の場合に比べて著しく改善される。 When performing alloying treatment by the heating rate is 80 ° C. / sec and rapid heating, the coating amount of the pre-oxidation is 0.1 g / m 2 or more impact resistance adhesiveness is remarkably as compared with the non-oxidizing It is improved. ただし、酸化皮膜量が5g/m 2を超えると、耐衝撃密着性の改善効果が失われる。 However, the amount of oxide film is more than 5 g / m 2, the effect of improving the impact resistance adhesiveness is lost.

【0032】本発明の方法により製造されたGA鋼板が非常に良好な耐衝撃密着性を示す理由は明らかではないが、適正な皮膜量での前酸化と急速加熱による合金化処理との複合効果により、密着性を支配するめっき/鋼板界面にFe含有量がかなり高くミクロな凹凸の多い特異な合金層が形成されるためではないかと考えられる。 The GA steel sheet is not clear why a very good impact resistance adhesiveness prepared by the method of the present invention, the combined effect of the alloying treatment by rapid heating and pre-oxidation in an appropriate amount of the coating film the thought that it is the order often peculiar alloy layer of Fe content in the plating / steel sheet interface governing adhesion much higher microscopic unevenness is formed.

【0033】本発明の方法により、耐パウダリング性などのプレス成形性の劣化を伴わずに低温での耐衝撃密着性が改善されたGA鋼板を製造することができる。 [0033] By the method of the present invention, it is possible to manufacture a GA steel sheet impact resistance adhesiveness is improved at low temperatures without the press formability deterioration such as powdering resistance. 従って、得られたGA鋼板は、塗装後に低温でチッピング衝撃を受けても塗膜やめっき皮膜が剥離しにくいので、自動車車体の内板はもとより、外板用にも充分に適用可能である。 Thus, the resulting GA steel sheet, since the low-temperature coating or a plating film even when subjected to chipping impact is hardly peeled after painting, the inner plates of car bodies, as well as a sufficiently applicable for the outer skin. もちろん、建材や家電製品といった用途にも使用できる。 Of course, it can also be used in applications such as building materials and home appliances.

【0034】 [0034]

【実施例】板厚0.8 mmの各種P添加鋼板 (フルハード冷延鋼板) またはP無添加鋼板をめっき母材とし、前洗浄として、通常のアルカリ脱脂 (NaOH水溶液中にてブラシ洗浄) 、水洗、乾燥を行った。 EXAMPLES Various P addition steel sheet having a thickness of 0.8 mm and (full hard cold rolled steel plate) or P additive-free steel sheet plated base metal, as precleaning, (brush washing with aqueous NaOH) ordinary alkali degreasing, washing with water , it was dried. その後、ガス燃焼式加熱炉において炉内の空燃比を0.9〜1.3 の範囲内、加熱温度を鋼板温度で 400〜650 ℃の範囲内で変化させて前酸化を行った。 This was followed by oxidation before by changing the air-fuel ratio in the furnace in the gas-combustion heating furnace in the range of 0.9 to 1.3, in the range of 400 to 650 ° C. The heating temperature of a steel plate temperature. 炉内の滞留時間は60秒であった。 The residence time in the furnace was 60 seconds. この前酸化で生成した酸化皮膜量をX線回折法により測定した。 The anodized coating produced in this pre-oxidation was measured by X-ray diffraction method.

【0035】前酸化を受けた鋼板を還元炉内で25%H 2 [0035] before received steel sheet oxide in the reduction furnace 25% H 2 +
N 2の雰囲気にて850 ℃×100 秒間の還元焼鈍を行った後、外気に触れさせずに直ちに溶融亜鉛めっき浴中に導入した。 After the reduction annealing of 850 ℃ × 100 seconds in an atmosphere of N 2, it was introduced immediately in the molten zinc plating bath to not exposed to the outside air. めっき浴は、温度460 ℃、Al添加量0.10%であり、ガスワイピング装置によりめっき付着量を片面当たり60 g/m 2に調整した。 Plating bath temperature 460 ° C., it is Al addition amount 0.10%, was adjusted coating weight on one side per 60 g / m 2 by gas wiping apparatus.

【0036】その後、加熱手段として高周波誘導加熱装置を用いて、周波数100 kHz で加熱することにより合金化のための熱処理を行った。 [0036] Then, using a high frequency induction heating device as the heating means, a heat treatment was performed for the alloy by heating at a frequency 100 kHz. この熱処理初期過程での昇温速度を変化させ、ゾーン選択により所定温度に到達した時点で加熱を止めるか、或いはさらに合金化を進める場合にはその到達温度に温度保持するヒートパターンとした。 This changing the heating rate of the heat treatment the initial stage, either stop heating when it reaches the predetermined temperature by the zone selection, or even if advancing the alloying was heat pattern that temperature maintained at that temperature reached. このようにして、Fe8〜12%の範囲内の合金化度のGA鋼板を得た。 There was thus obtained the GA steel alloying size in the range of Fe8~12%.

【0037】得られたGA鋼板の耐パウダリング性、耐フレーキング性および耐低温衝撃密着性を、次のようにして測定した、試験結果を母材鋼板の鋼種、P添加量、 The powdering resistance of the resulting GA steel sheets, the anti-flaking resistance and low-temperature impact adhesion was measured as follows, steels of the base material steel plate of the test results, P addition amount,
前酸化量 (酸化皮膜量) 、合金化初期の昇温速度、合金化温度範囲、めっき皮膜の合金化度とともに、表1に示す。 Before oxidation amount (amount oxide film), an alloy of the initial rate of temperature increase, the alloying temperature range, the alloying of the plating film are shown in Table 1.

【0038】1) 耐パウダリング性 GA鋼板を直径60 mm の円板状に打ち抜き、ポンチ直径 [0038] 1) powdering resistance punching a ring of GA steel sheet 60 mm diameter disc-shaped punch diameter
30 mm 、ダイス肩半径3Rの円筒絞り試験を行った後、 30 mm, after the cylindrical drawing test of die shoulder radius 3R,
外側円筒部のテープ剥離を行い、剥離程度を目視により4段階 (◎、○、△、×) の4段階で評価した。 Perform tape peeling of the outer cylindrical portion, four stages visually about peeling (◎, ○, △, ×) was evaluated in four stages. ◎が優秀、×が不良である。 ◎ is excellent, × is bad.

【0039】2) 耐フレーキング性 250 ×50 mm の寸法に切り出したGA鋼板の試験片を用い、図2に示す装置によりビード付ハット成形試験を行った。 [0039] 2) using a test piece of GA steel sheet was cut into dimensions of anti-flaking resistance 250 × 50 mm, it was beaded hat forming test by the apparatus shown in FIG. ビード高さは7mm、成形高さは50 mm 、成形速度は80 mm/sec であった。 Bead height is 7 mm, forming height is 50 mm, the molding speed was 80 mm / sec. 得られた成形体のビード接触部内壁側についてテープ剥離を行い、その黒化度からフレーキング性を次の基準で判断した。 For bead contact part inner wall of the resulting molded body subjected to a tape peeling it was determined flaking resistance from the blackening degree in the following criteria. ○:使用上問題なし、 △:剥離がやや多い、 ×: ○: Nashi use on the problem, △: peeling slightly more, ×:
使用不可。 Usage prohibited.

【0040】3) 耐低温衝撃密着性 (耐低温チッピング性) 150 ×70 mm の寸法に切り出したGA鋼板の試験片に、 [0040] 3) low-temperature impact adhesion (the test piece GA steel sheet was cut into sizes of low temperature chipping resistance) 0.99 × 70 mm,
市販の浸漬式リン酸塩処理液を使用してリン酸塩処理した後、カチオン型電着塗料による下塗り→中塗り→上塗りの3コート塗装 (合計膜厚:100 μm) を施した。 After phosphating using a commercially available immersion phosphating solution, 3-coat paint undercoating → intermediate → topcoat by cationic electrodeposition paint (total thickness: 100 [mu] m) were subjected to. 得られた塗装鋼板を−20℃に冷却保持し、グラベロ試験機において直径4〜6mmの砂利石10個を空気圧2.0 kg/c The resulting coated steel sheet was cooled held at -20 ° C., pneumatic ten gravel stones with a diameter of 4~6mm in Gurabero tester 2.0 kg / c
m 2 、衝突速度 100〜150 km/hr の条件で衝突させ、各衝突点での塗膜の剥離径を測定した。 m 2, to collide with the conditions of impact speed 100 to 150 miles / hr, to measure the peel diameter of the coating at each point of impact. この剥離径の平均値 The average value of this peel diameter
(平均剥離径) により耐低温衝撃密着性を評価した。 It was evaluated low-temperature impact adhesion by (average peel diameter).

【0041】 [0041]

【表1】 [Table 1]

【0042】表1に示した結果からわかるように、本発明方法により適量の前酸化を行った後、還元、溶融亜鉛めっきを施し、次いで急速加熱により合金化処理したG [0042] As can be seen from the results shown in Table 1, after an appropriate amount of the pre-oxidized by the method of the present invention, reduction, galvanized and then treated alloy by rapid heating G
A鋼板は、耐パウダリング性および耐フレーキング性を良好に保持したまま、低温での耐衝撃密着性が著しく向上した。 A steel sheet, while satisfactorily retaining the resistance to powdering resistance and flaking resistance, impact resistance adhesiveness at low temperatures is significantly improved. この効果は、P添加鋼に限らず、P無添加鋼においても得られた。 This effect is not limited to the P-added steel, it was obtained in P-free steels. これに対して、合金化処理時の昇温速度が30℃/secより低いと、耐衝撃密着性はほとんど改善されなかった。 In contrast, when the heating rate during the alloying treatment is lower than 30 ° C. / sec, impact resistance adhesiveness was hardly improved. また、前酸化での酸化皮膜量が 0.1〜 Further, 0.1 oxidation film of prior oxidation
5 g/m 2の範囲を外れるか、或いは合金化処理の熱処理温度領域が 420〜700 ℃の温度領域を外れると、耐衝撃密着性のみならず、耐パウダリング性か耐フレーキング性も劣化した。 5 or out of the range of g / m 2, or when the heat treatment temperature region of the alloying process is out of the temperature range of four hundred and twenty to seven hundred ° C., not impact resistance adhesiveness only, powdering resistance or anti-flaking property deterioration did.

【0043】 [0043]

【発明の効果】以上に説明したように、本発明の方法により、耐パウダリング性や耐フレーキング性といった必要な他の性能を劣化させずに、耐衝撃密着性、特に衝撃に弱い低温での耐衝撃密着性が著しく改善されたGA鋼板を製造することができる。 As described above, according to the present invention, the method of the present invention, without degrading other performance required such powdering resistance and flaking resistance, impact resistance adhesiveness, especially a weak low temperature impact it can impact resistance adhesiveness of producing GA steel sheet was markedly improved. 本発明の方法は、耐衝撃密着性が劣化し易いP添加鋼を母材鋼板とするGA鋼板の製造において特に大きな耐衝撃密着性の改善が得られるが、低炭素鋼、極低炭素鋼といった他の鋼種を使用したGA鋼板の衝撃密着性の向上にも有効である。 The method of the present invention, a likely P-added steel impact resistance adhesiveness is deteriorated but improvement in particular of large impact resistance adhesiveness in the production of GA steel sheet as a base material steel plate is obtained, low-carbon steel, such as ultra-low carbon steel it is also effective in improving the impact adhesion GA steel using other grades. 本発明の方法により製造されたGA鋼板は、自動車車体の外板に適しているほか、自動車車体の内板、建材、家電製品といった各種用途に有用である。 GA steel sheet produced by the method of the present invention, in addition to being suitable for outer panel of automobile body, useful automobile body of the inner plate, building materials, in various applications such as home appliances.

【図面の簡単な説明】 BRIEF DESCRIPTION OF THE DRAWINGS

【図1】合金化溶融亜鉛めっき鋼板の前酸化における酸化皮膜量と低温での耐衝撃密着性 (−20℃でのチッピング試験における平均剥離径) との関係を示すグラフである。 1 is a graph showing the relationship between the (average peel diameter in chipping test at -20 ° C.) impact resistance adhesiveness of the previous oxide film amount and the low temperature in the oxidation of the galvannealed steel sheet.

【図2】耐フレーキング性の評価に用いたビード付ハット成形試験の概要を示す説明図である。 FIG. 2 is an explanatory diagram showing an outline of a beaded hat molded test used for evaluation of flaking resistance.

Claims (1)

    (57)【特許請求の範囲】 (57) [the claims]
  1. 【請求項1】 鋼板に合金化溶融亜鉛めっきを連続的に施すにあたり、前焼鈍炉内の予熱工程において鋼板表面の酸化皮膜量が 0.1〜5g/m 2となるように前酸化を行った後、還元工程で還元処理した鋼板に所定量の溶融亜鉛めっきを付着させた後、30℃/sec以上の昇温速度で鋼板温度 420〜700 ℃の温度領域内に加熱し、この温度領域内で熱処理して合金化を行うことを特徴とする、耐衝撃密着性に優れた合金化溶融亜鉛めっき鋼板の製造方法。 1. A galvannealed Upon continuously applied to the steel sheet, before after an oxide film of the steel sheet surface in the preheating step of the annealing furnace is subjected to pre-oxidation so that 0.1-5 g / m 2 , after depositing a predetermined amount of molten zinc plating reduction treated steel sheet in the reduction step, it is heated to a temperature in the region of the steel plate temperature 420-700 ° C. at 30 ° C. / sec or higher heating rate, at this temperature region and performing alloying and heat treatment method for producing a superior galvannealed steel sheet in impact resistance adhesiveness.
JP4235942A 1992-09-03 1992-09-03 Method for producing superior galvannealed steel sheet in impact resistance adhesiveness Expired - Lifetime JP2725537B2 (en)

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KR100892815B1 (en) * 2004-12-21 2009-04-10 가부시키가이샤 고베 세이코쇼 Method and facility for hot dip zinc plating
US8025982B2 (en) 2005-12-06 2011-09-27 Kobe Steel, Ltd. High-strength hot dip galvannealed steel sheet having high powdering resistance and method for producing the same
JP4718381B2 (en) * 2006-06-21 2011-07-06 株式会社神戸製鋼所 Hot dip galvanizing equipment
JP6137002B2 (en) * 2014-03-17 2017-05-31 Jfeスチール株式会社 Method for producing hot-dip galvanized steel sheet and alloyed hot-dip galvanized steel sheet, hot-dip galvanized steel sheet and alloyed hot-dip galvanized steel sheet

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JPH03134147A (en) * 1989-10-17 1991-06-07 Sumitomo Metal Ind Ltd Production of alloying hot dip galvanized steel sheet
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