JP3735360B2 - Manufacturing method of hot-dip Zn-Mg-Al plated steel sheet with excellent appearance - Google Patents

Manufacturing method of hot-dip Zn-Mg-Al plated steel sheet with excellent appearance Download PDF

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JP3735360B2
JP3735360B2 JP2003430019A JP2003430019A JP3735360B2 JP 3735360 B2 JP3735360 B2 JP 3735360B2 JP 2003430019 A JP2003430019 A JP 2003430019A JP 2003430019 A JP2003430019 A JP 2003430019A JP 3735360 B2 JP3735360 B2 JP 3735360B2
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steel sheet
plated steel
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一実 西村
隆 澤井
栄一 竹内
寛 原田
英俊 新頭
英雄 松岡
敦司 宮崎
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Nippon Steel Corp
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Description

本発明は、めっき外観に優れた溶融Zn−Mg−Al系めっき鋼板の製造方法に関するものである。   The present invention relates to a method for producing a hot-dip Zn—Mg—Al-plated steel sheet having an excellent plating appearance.

耐食性に優れる溶融Zn−Mg−Alめっき鋼板については従来より幾つかの提案がなされており、例えば本発明者らも特許文献1で、Zn−Mg−Alめっき鋼板の製造方法を提案している。
その方法は、還元処理した鋼板、あるいはプレNiめつきした鋼板を460〜550℃の範囲で、Al:0.1〜40%、Mg:0.1〜10%含有するZnめっき浴に浸漬して溶融めっきし、浴より引き上げた溶融めっき鋼板を、慣用のガスワイピングによりめつき付着量調整後、冷却してめつき層を凝固させるものである。尚、めっき層中にMg金属間化合物相を分散させるために、めっき層がまだ溶融状態のうちに冷却速度を5゜C/sec以上程度に制御することなどが望ましいと述べている。
特開2001−64759号号公報
Several proposals have conventionally been made on hot-dip Zn-Mg-Al-plated steel sheets with excellent corrosion resistance. For example, the present inventors have also proposed a method for producing Zn-Mg-Al-plated steel sheets in Patent Document 1. .
The method is to immerse a reduction-treated steel plate or a pre-Ni-plated steel plate in a Zn plating bath containing Al: 0.1 to 40% and Mg: 0.1 to 10% within a range of 460 to 550 ° C. The hot dip galvanized steel sheet that has been hot dip-plated and pulled up from the bath is cooled to adjust the adhesion amount by conventional gas wiping, and then cooled to solidify the adhesion layer. It is stated that it is desirable to control the cooling rate to about 5 ° C./sec or more while the plating layer is still in a molten state in order to disperse the Mg intermetallic compound phase in the plating layer.
JP 2001-64759 A

このような方法で得られた溶融Zn−Mg−Al系めっき鋼板は、建材、土木分野のガードレール、防音壁、家電分野の部品等を中心に寿命延長の観点から高耐食性めっき鋼板として多く使用されており、優れためっき鋼板であるが、めっき層の凝固組織がZn−Mg合金相、Alの含有量に応じてZn初晶、あるいはAl初晶よりなる複雑な構造をしているため、冷却速度をコントロールしないと外観上、斑点〔Zn−Mg−Al3元合金相起因〕あるいは表面の梨地状の微小凹凸(Al初晶起因)、白いざらつき、微小羽根模様等が生じることがあり、その改善が望まれていた。   The hot-dip Zn-Mg-Al-based plated steel sheet obtained by such a method is often used as a highly corrosion-resistant plated steel sheet from the viewpoint of extending the life centering on building materials, guardrails in the civil engineering field, soundproof walls, parts in the home appliance field, etc. It is an excellent plated steel sheet, but the solidification structure of the plating layer has a complex structure consisting of Zn primary crystals or Al primary crystals depending on the Zn-Mg alloy phase and Al content. If the speed is not controlled, the appearance may cause speckles (due to the Zn-Mg-Al ternary alloy phase) or surface textured fine irregularities (due to Al primary crystals), white roughness, fine feather patterns, etc. Was desired.

本発明者らは、その後種々検討したところ、溶融Zn−Mg−Alめっき鋼板の製造プロセスにおいて、ワイピング後、未凝固状態のめっき鋼鈑表面に固体表面を接触させることでめっき層中に凝固核を生成させることにより、その後どのような冷却速度で冷却しても、斑点〔Zn−Mg−Al3元合金相起因〕あるいは表面の梨地状の微小凹凸(Al初晶起因)、微小羽根模様等が解消し優れた均一外観となることを見出し、下記の本発明を完成したものである。   The inventors of the present invention subsequently studied variously, and in the manufacturing process of the molten Zn-Mg-Al plated steel sheet, after wiping, the solid surface was brought into contact with the surface of the unsolidified plated steel sheet by bringing the solid surface into contact with the solidified nucleus. After forming, no matter what the cooling rate is, spots [because of Zn-Mg-Al ternary alloy phase] or surface-like fine irregularities (because of Al primary crystal), fine feather patterns, etc. The present invention described below has been completed by finding that it has been solved and has an excellent uniform appearance.

即ち本発明は、鋼板をAl:0.1−60%、Mg:0.1−10%含有するZnめつき浴に浸漬し、浴より引き上げた溶融めっき鋼板をガスワイピングによってめつき付着量調整後、冷却してめつき層を凝固させる溶融Zn−Mg−Al系めっき鋼板の製造方法において、めつき付着量調整後、冷却前に未凝固状態のめつき層表面に固体表面を接触させることにより、めっき層中に凝固核を生成させることを特徴とする外観に優れた溶融Zn−Mg−Al系めっき鋼板の製造方法である。   That is, in the present invention, the steel sheet is immersed in a Zn plating bath containing Al: 0.1-60% and Mg: 0.1-10%, and the amount of adhesion is adjusted by gas wiping of a hot-dip plated steel plate pulled up from the bath. Then, in the method of manufacturing a molten Zn—Mg—Al-plated steel sheet that cools and solidifies the adhesion layer, after adjusting the adhesion amount of adhesion, the solid surface is brought into contact with the surface of the unsolidified adhesion layer before cooling. Is a method for producing a hot-dip Zn—Mg—Al-plated steel sheet having an excellent appearance, characterized in that solidification nuclei are generated in the plating layer.

上記未凝固状態のめつき層表面に接触させる固体表面が凹凸を有しており、その平均深さで0.01〜500μm、凹凸間の平均距離が3000μmとなるようにすることができる。   The solid surface brought into contact with the surface of the unsolidified adhesive layer has irregularities, and the average depth can be 0.01 to 500 μm, and the average distance between the irregularities can be 3000 μm.

また、上記Znめつき浴中にSi,Sn,Cr,Ti,B,Ni,Fe,Co,Sb,Pb,Cuの元素を単独あるいは複合で10%以下含有させることができる。   Further, in the Zn plating bath, elements of Si, Sn, Cr, Ti, B, Ni, Fe, Co, Sb, Pb and Cu can be contained alone or in combination of 10% or less.

さらに本発明は、前記した未凝固状態のめつき層中に凝固核を生成させた後、冷却速度5℃/秒以上の空冷あるいは気水冷却をすることができる。   Furthermore, in the present invention, after generating solidified nuclei in the above-mentioned unsolidified adhesive layer, air cooling or air-water cooling at a cooling rate of 5 ° C./second or more can be performed.

さらに本発明は、上記した方法において、鋼板表面にNiを0.2〜10g/m2 プレめつき後、加熱(460〜550℃)し、この鋼板をめっき浴に浸漬する方法も採用できる。 Furthermore, the present invention can employ a method in which Ni is 0.2 to 10 g / m 2 pre-plated on the surface of the steel sheet and then heated (460 to 550 ° C.) and the steel sheet is immersed in a plating bath.

さらには還元処理した(460〜550℃の)鋼板をめっき浴に浸漬することもできる。   Furthermore, a reduction-treated steel plate (from 460 to 550 ° C.) can be immersed in the plating bath.

このように本発明は、上記した各処理を適宜採用することにより、外観に優れた溶融Zn−Mg−Alめっき鋼板を製造することができる。   Thus, this invention can manufacture the hot-dip Zn-Mg-Al plating steel plate excellent in the external appearance by employ | adopting each above-mentioned process suitably.

本発明のめっき製造方法は、Zn−Mg−Al系溶融めっきにおいて、後の冷却方法を選ばず外観が良好になる点で非常に有用である。   The plating production method of the present invention is very useful in terms of improving the appearance of any Zn-Mg-Al-based hot dipping, regardless of the subsequent cooling method.

以下に本発明の実施の形態を詳細に説明する。
本発明は、溶融Zn−Mg−Alめっき鋼板の製造プロセスにおいて、ワイピング後、未凝固状態のめっき鋼板表面に固体表面を接触させるにより、めっき層中に凝固核を生成させ、これにより溶融Zn−Mg−Al系めっき鋼板の外観が非常に良好となるところに最大の技術上のポイントがある。
Hereinafter, embodiments of the present invention will be described in detail.
In the manufacturing process of the molten Zn-Mg-Al plated steel sheet, the present invention generates solidified nuclei in the plated layer by bringing a solid surface into contact with the surface of the unsolidified plated steel sheet after wiping. The biggest technical point is that the appearance of the Mg—Al-based plated steel sheet is very good.

以下に本発明における各条件の限定理由について述べる。
まず、Al:0.1〜60%、Mg:0.1〜10%、残りZn及び不可避成分よりなる溶融Zn−Mg−Alめっき鋼板の製造プロセスとしたのは、本組成範囲において本発明のポイントとなるプロセスである未凝固状態のめっき鋼板表面に固体表面を接触させることにより、めっき層中に凝固核を生成させめっき外観が良好となる効果が最も出やすいためである。
The reasons for limiting each condition in the present invention will be described below.
First, the manufacturing process of the hot-dip Zn—Mg—Al-plated steel sheet composed of Al: 0.1 to 60%, Mg: 0.1 to 10%, the remaining Zn and inevitable components was used in the present composition range. This is because by bringing the solid surface into contact with the surface of the unsolidified plated steel sheet, which is a key process, the effect of generating solidified nuclei in the plating layer and improving the plating appearance is most likely to occur.

また、ワイピング後、未凝固状態のめっき鋼板表面に固体表面を接触させこととしたのは、未凝固状態の時でないとめっき層中に凝固核が生成しないためである。
さらには、未凝固状態のめっき鋼板表面に接触させる固体表面が凹凸を有していると、めっき表面外観が良好となったためである。
In addition, the reason why the solid surface is brought into contact with the surface of the unsolidified plated steel sheet after wiping is that solidification nuclei are not generated in the plating layer unless the solid surface is in an unsolidified state.
Furthermore, when the solid surface brought into contact with the surface of the unsolidified plated steel sheet has irregularities, the appearance of the plated surface is improved.

そのメカニズムは未だ明確ではないが、固体表面の凹凸により、Zn−Mg−Al系めっき層中に発生する初期凝固核の数、核の距離などが影響を受け、Al初晶あるいはZn初晶及び3元Zn−Mg−Al合金相、さらにはZn−Mg−AlめっきにSiあるいはSnを含有する場合には、Mg2 Si、Mg2 Sn金属間化合物などの生成状態が変化し、上述の斑点、表面の梨地状の微小凹凸(Al初晶起因)、白いざらつき、微小羽根模様等が解消し、外観向上につながっているものと思われる。 Although the mechanism is not yet clear, the number of initial solidification nuclei generated in the Zn—Mg—Al-based plating layer, the distance of the nuclei, etc. are affected by the unevenness of the solid surface. When Si or Sn is contained in the ternary Zn—Mg—Al alloy phase and further Zn—Mg—Al plating, the production state of Mg 2 Si, Mg 2 Sn intermetallic compound, etc. changes, and the above-mentioned spots It seems that the textured surface irregularities (because of Al primary crystal), white roughness, fine feather pattern, etc. have been eliminated, leading to improved appearance.

接触させる装置については特に限定しないが、水冷銅ロール、ベルトキャスター、ウオーキングバーなどが使用でき、接触させる固体の種類についても銅そのもの、あるいはその表面に金属めっき、セラミックコーティングを施したものなどいろいろ使用できる。   There are no particular restrictions on the device to be contacted, but water-cooled copper rolls, belt casters, walking bars, etc. can be used, and various types of solids to be contacted, such as copper itself or metal plating or ceramic coating on its surface, can be used. it can.

ワイピング後、未凝固状態のめっき鋼板表面に固体表面を接触させることによりめっき層中に凝固核を生成させた後に、冷却速度5℃/s以上の空冷あるいは気水冷却することとしたのは、本未凝固状態のめっき鋼板表面に固体表面を接触させる工程により、その後の冷却が空冷であっても気水冷却であっても平滑な美しい表面外観が確保でき、特に冷却速度を5℃/s以上でその効果が顕著なためである。また固体表面接触後、気水冷却を行うと冷却速度が早いために、平滑な外観に加えてめっき結晶粒の微細化及びめっき層中のMg2 Si等の析出物の均一分散化も可能なためである。 After wiping, solidified nuclei were generated in the plated layer by bringing the solid surface into contact with the surface of the unsolidified plated steel sheet, and then air cooling or air-water cooling at a cooling rate of 5 ° C./s or more was performed. The step of bringing the solid surface into contact with the surface of the unsolidified plated steel sheet can ensure a smooth and beautiful surface appearance regardless of whether the subsequent cooling is air cooling or air-water cooling. This is because the effect is remarkable. In addition, since the cooling rate is fast when air-water cooling is performed after contact with the solid surface, it is possible to refine the plating crystal grains and uniformly disperse precipitates such as Mg 2 Si in the plating layer in addition to a smooth appearance. Because.

これらのメカニズムも未だ明確ではないが、未凝固状態のめっき鋼板表面に固体表面を接触させるによりめっき層中に凝固核を生成させた場合、この凝固核が後に空冷あるいは気水凝固してもそのまま保持され、表面の外観を保つ効果があるものと思われる。   These mechanisms are still unclear, but when solidified nuclei are generated in the plating layer by bringing the solid surface into contact with the surface of the unsolidified plated steel sheet, the solidified nuclei will remain as they are even after solidification by air cooling or air-water solidification. It seems that it is retained and has the effect of maintaining the appearance of the surface.

さらに、めっき浴の組成としてAl:0.1〜40%、Mg:0.1〜10%含有するZn−Al―Mg合金浴、もくは本溶融Zn−Mg−Alめっき浴中にSi,Sn,Cr,Ti,B,Ni,Fe,Co,Sb,Pb,Cuの元素を単独あるいは複合で10以下含有するめっき浴としたのは、本範囲においてめっき層の耐食性が極めて良好となるためである。   Further, the composition of the plating bath is Al: 0.1 to 40%, Mg: 0.1 to 10% of Zn-Al-Mg alloy bath, or in the present molten Zn-Mg-Al plating bath, Si, The reason why the plating bath containing the elements of Sn, Cr, Ti, B, Ni, Fe, Co, Sb, Pb, and Cu alone or in combination is 10 or less is that the corrosion resistance of the plating layer is extremely good in this range. It is.

次にNiプレめっき量を0.2〜10g/m2 としたのは、この範囲でめっき性が良好となるためである。プレNi量が0.2g/m2 未満では、溶融めっき時に微小不めっきが生じ、10g/m2 を超えるとめっき密着性がやや劣化するからである。
さらに、還元処理した460〜550℃の鋼板を浴浸することとしたのは、プレNiめっきなしの場合のめっきにも本方法が効果があったためである。
Next, the reason why the Ni pre-plating amount is set to 0.2 to 10 g / m 2 is that the plating property is good in this range. This is because if the amount of pre-Ni is less than 0.2 g / m 2 , minute non-plating occurs at the time of hot dipping, and if it exceeds 10 g / m 2 , the plating adhesion is slightly deteriorated.
Furthermore, the reason why the reduced-treated 460 to 550 ° C. steel sheet is bath-immersed is that the present method was effective in plating without pre-Ni plating.

溶融めっきの付着量については特に制約は設けないが、耐食性の観点から10g/m2 以上、加工性の観点からすると350g/m2 以下であることが望ましい。
なお、本発明の下地鋼板としては、熱延鋼板、冷延鋼板共に使用でき、鋼種もAlキルド鋼、Ti,Nb等を添加した極低炭素鋼板、およびこれらにP,Si,Mn等の強化元素を添加した高強度鋼、ステンレス鋼板など種々のものが適用できる。
Although there is no particular restriction on the adhesion amount of the hot dipping, it is preferably 10 g / m 2 or more from the viewpoint of corrosion resistance and 350 g / m 2 or less from the viewpoint of workability.
In addition, as a base steel plate of the present invention, both hot-rolled steel plates and cold-rolled steel plates can be used, and steel grades are ultra-low carbon steel plates to which Al killed steel, Ti, Nb, etc. are added, and reinforced with P, Si, Mn, etc. Various materials such as high-strength steel added with elements and stainless steel plate can be applied.

以下、実施例によって本発明をさらに詳細に説明する。
(実施例1)
表面粗度(3,10,100μm)の変化した水冷Cu板で溶融状態のZn−3%Mg−11%Al−0.2%Si(一部Zn−0.5%Mg−0.2%Al、Zn−0.5%Mg−0.2%Al−0.2%Si、一部Zn−0.5%Mg−0.2%Al−5%Sn)めっき表面をワイピング後に400℃で1secタッチを行った後、自然放冷、空冷(ガスジェット:AJC)及び気水冷却、水冷で冷却した場合の外観の変化、ミクロ構造を表1に示す。
比較には、空冷のみ、気水冷却のみの場合を示した。
溶融めっき条件は、熱延酸洗鋼板1.6mmにプレNiめっきを1g/m2 施した後、板温度450℃まで加熱し、450℃のめっき浴中で溶融めっきした。めっき付着量は、片面135g/m2 とした。
Hereinafter, the present invention will be described in more detail with reference to examples.
Example 1
Zn-3% Mg-11% Al-0.2% Si (partially Zn-0.5% Mg-0.2%) in a molten state with a water-cooled Cu plate having a changed surface roughness (3, 10, 100 μm) Al, Zn-0.5% Mg-0.2% Al-0.2% Si, partially Zn-0.5% Mg-0.2% Al-5% Sn) After wiping the plating surface at 400 ° C Table 1 shows changes in appearance and microstructure when cooled by natural cooling, air cooling (gas jet: AJC), air-water cooling, and water cooling after touching for 1 sec.
For comparison, only air cooling and air / water cooling were shown.
The hot-dip pickled steel sheet 1.6 mm was subjected to pre-Ni plating 1 g / m 2 and then heated to a plate temperature of 450 ° C. and hot-dip plated in a 450 ° C. plating bath. The plating adhesion amount was set to 135 g / m 2 on one side.

Figure 0003735360
Figure 0003735360

表1から明らかなように、本発明の溶融Zn−Mg−Al系めっき鋼板の製造方法(No.1〜8,11〜13)は、比較の方法(No.9,10)に比べて、めっき外観が良好である。   As apparent from Table 1, the production method (Nos. 1 to 8, 11 to 13) of the hot-dip Zn—Mg—Al-plated steel sheet of the present invention is compared to the comparative method (Nos. 9 and 10). The plating appearance is good.

(実施例2)
鏡面仕上げした水冷Cuロール(表面凹凸の平均深さ0.05μm、表面凹凸の平均距離2500μm)およびその上にCrめっきを20μm施した水冷Cuロール(表面凹凸の平均深さ0.1μm、表面凹凸の平均距離2000μm)あるいはNi−Wめっきを5μm施した水冷Cuロール(表面凹凸の平均深さ0.1μm、表面凹凸の平均距離1800μm)で溶融状態のZn−3%Mg−11%Al−0.2%Si(一部Zn−0.5%Mg−0.2%Al、Zn−0.5%Mg−0.2%Al−0.2%Si、一部Zn−0.5%Mg−0.2%Al−5%Sn)めっき表面をワイピング後に400℃で1secタッチを行った後、自然放冷、空冷(ガスジェット:AJC)及び気水冷却、水冷で冷却した場合の外観の変化、ミクロ構造を表2に示す。
比較には、空冷のみ、気水冷却のみの場合を示した。
溶融めっき条件は、熱延酸洗鋼板1.6mmにプレNiめっきを1g/m2 施した後、板温度450℃まで加熱し、430℃のめっき浴中で溶融めっきした。めっき付着量は、片面90g/m2 とした。
(Example 2)
Mirror-finished water-cooled Cu roll (average depth of surface irregularities 0.05 μm, average distance of surface irregularities 2500 μm) and water-cooled Cu roll with 20 μm of Cr plating thereon (average depth of surface irregularities 0.1 μm, surface irregularities) Zn-3% Mg-11% Al-0 in a molten state with a water-cooled Cu roll (average depth of surface irregularities 0.1 μm, average distance of surface irregularities 1800 μm) subjected to Ni-W plating 5 μm .2% Si (partially Zn-0.5% Mg-0.2% Al, Zn-0.5% Mg-0.2% Al-0.2% Si, part Zn-0.5% Mg -0.2% Al-5% Sn) After wiping the plating surface for 1 second at 400 ° C., the appearance of natural cooling, air cooling (gas jet: AJC), air / water cooling, and water cooling Change, microstructure It shows in Table 2.
For comparison, only air cooling and air / water cooling were shown.
The hot-dip pickled steel sheet 1.6 mm was subjected to pre-Ni plating 1 g / m 2, then heated to a plate temperature of 450 ° C. and hot-dip plated in a 430 ° C. plating bath. The amount of plating was 90 g / m 2 on one side.

Figure 0003735360
Figure 0003735360

表2から明らかなように、本発明の溶融Zn−Mg−Al系めっき鋼板の製造方法(No.1〜9,12−14)は、比較の方法(No.10,11)に比べてめっき外観が良好である。   As apparent from Table 2, the production method (Nos. 1-9, 12-14) of the hot-dip Zn—Mg—Al-based plated steel sheet of the present invention is plated compared to the comparative method (Nos. 10, 11). Appearance is good.

Claims (5)

鋼板を、Al:0.1〜60質量%、Mg:0.1〜10質量%含有するZnめつき浴に浸漬し、浴より引き上げた溶融めっき鋼板をワイピングによってめつき付着量調整後、冷却してめつき層を凝固させる溶融Zn−Mg−Al系めっき鋼板の製造方法において、めつき付着量調整後、冷却前に未凝固状態の初期凝固核生成前のめつき層表面に固体表面を接触させることにより、めっき層中に凝固核を生成させることを特徴とする外観に優れた溶融Zn−Mg−Al系めっき鋼板の製造方法。 The steel sheet was immersed in a Zn plating bath containing Al: 0.1 to 60% by mass and Mg: 0.1 to 10% by mass. In the method of manufacturing a molten Zn-Mg-Al plated steel sheet that solidifies the adhesion layer, after adjusting the adhesion amount of the adhesion, the solid surface is applied to the surface of the adhesion layer before the formation of initial solidified nuclei before cooling. A method for producing a hot-dip Zn—Mg—Al-based plated steel sheet having an excellent appearance, wherein solidified nuclei are generated in a plating layer by contacting. 未凝固状態の初期凝固核生成前のめつき層表面に接触させる固体表面が凹凸を有することを特徴とする請求項1に記載の外観に優れた溶融Zn−Mg−Al系めっき鋼板の製造方法。 Method for producing a molten Zn-Mg-Al-based plated steel sheet excellent in appearance according to claim 1, a solid surface is brought into contact with the initial solidification nucleation before plated layer surface of the non-coagulated state is characterized by having irregularities . Znめつき浴中にSi,Sn,Cr,Ti,B,Ni,Fe,Co,Sb,Pb,Cuの元素を単独あるいは複合で10質量%以下含有することを特徴とする請求項1または2に記載の外観に優れた溶融Zn−Mg−Al系めっき鋼板の製造方法。   3. The Zn plating bath contains elements of Si, Sn, Cr, Ti, B, Ni, Fe, Co, Sb, Pb, Cu alone or in combination of 10% by mass or less. The manufacturing method of the hot-dip Zn-Mg-Al system plated steel plate excellent in the external appearance described in 2. 表面にNiを0.2〜10g/m0.2-10 g / m of Ni on the surface 2 プレめつき後、加熱した460〜550℃の鋼板を浴浸漬することを特徴とする請求項1〜3のいずれかに記載の外観に優れた溶融Zn−Mg−Al系めっき鋼板の製造方法。The method for producing a hot-dip Zn-Mg-Al-based plated steel sheet having excellent appearance according to any one of claims 1 to 3, wherein a heated 460-550 ° C steel sheet is immersed in a bath after pre-plating. 還元処理した460〜550℃の鋼板を浴に浸漬することを特徴とする請求項1〜3のいずれかに記載の外観に優れた溶融Zn−Mg−Al系めっき鋼板の製造方法。The method for producing a hot-dip Zn-Mg-Al-plated steel sheet having excellent appearance according to any one of claims 1 to 3, wherein a reduction-treated steel sheet at 460 to 550 ° C is immersed in a bath.
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