JP6569618B2 - Method for producing zinc phosphate treated steel sheet - Google Patents
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本発明は、自動車、家電、建材等の用途に用いられるリン酸亜鉛処理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 zinc phosphate-treated steel sheet used for applications such as automobiles, home appliances, and building materials.
リン酸亜鉛系被膜を有する鋼板（以下、リン酸亜鉛処理鋼板と称す）は、プレス成形時の摺動抵抗が小さく、鋼板をプレス金型へ流入させやすいため、自動車車体用途を中心に用いられている。 Steel sheets with zinc phosphate coating (hereinafter referred to as zinc phosphate-treated steel sheets) have low sliding resistance during press forming and are easy to flow into the press mold, so they are mainly used for automobile bodies. ing.
リン酸亜鉛処理鋼板は、例えば、冷延鋼板上に亜鉛めっきを施した後、表面調整液を鋼板表面に吹き掛けリン酸亜鉛結晶の核となる物質を鋼板表面に散布した後、リン酸亜鉛処理を施してリン酸亜鉛被膜を形成させ製造される。リン酸亜鉛処理法としては、スプレー方式やコーター方式が挙げられる。 Zinc phosphate-treated steel sheet, for example, after galvanizing on a cold-rolled steel sheet, spraying a surface conditioning liquid on the steel sheet surface and spraying a substance that becomes the core of zinc phosphate crystals on the steel sheet surface, then zinc phosphate It is manufactured by applying a treatment to form a zinc phosphate coating. Examples of the zinc phosphate treatment method include a spray method and a coater method.
しかしながら、鋼板表面において反応ムラが発生する問題がある。特に鋼板のリン酸亜鉛処理法としてスプレー方式やコーター方式等はいずれも反応型の化成処理被膜（リン酸亜鉛被膜）形成であるため、鋼板表面において反応ムラが発生しやすい。 However, there is a problem that uneven reaction occurs on the surface of the steel plate. In particular, as a zinc phosphate treatment method for a steel plate, any of a spray method, a coater method, and the like is a reactive chemical conversion coating (zinc phosphate coating) formation, so that reaction unevenness is likely to occur on the steel plate surface.
本発明は、かかる事情に鑑みてなされたものであって、反応ムラが軽減された表面性状に優れたリン酸亜鉛処理鋼板の製造方法を提供することを目的とする。 This invention is made | formed in view of this situation, Comprising: It aims at providing the manufacturing method of the zinc phosphate treatment steel plate excellent in the surface property from which the reaction nonuniformity was reduced.
発明者らは、上記課題を解決するために、表面調整処理直後の鋼板表面の状態に着目した。そして、表面調整処理直後に鋼板表面に気体を吹き付けることにより表面調整液が鋼板表面に均一にレベリング（平滑化）され、その後のリン酸亜鉛被膜形成時において反応ムラが抑えられることを見出し、本発明を完成させた。 In order to solve the above-mentioned problems, the inventors focused on the state of the steel sheet surface immediately after the surface adjustment treatment. Then, immediately after the surface adjustment treatment, the surface adjustment liquid is uniformly leveled (smoothed) on the surface of the steel sheet by blowing gas on the surface of the steel sheet, and it is found that the reaction unevenness can be suppressed during the subsequent formation of the zinc phosphate coating. Completed the invention.
本発明は、以上の知見に基づきなされたものであり、その要旨は以下の通りである。
[1] 亜鉛めっき鋼板または亜鉛系めっき鋼板の表面上に表面調整液を塗布し表面調整処理を行った後、鋼板表面に吹きつけ圧力：0.20MPa以上で気体を吹きつけ、次いで、リン酸亜鉛系処理液を鋼板表面に塗布することによりリン酸亜鉛被膜を形成することを特徴とするリン酸亜鉛処理鋼板の製造方法。
［２］前記吹きつけ圧力は、0.30MPa以上0.40MPa以下であることを特徴とする上記［１］に記載のリン酸亜鉛処理鋼板の製造方法。
［３］スリット状のノズルを用いて鋼板表面に気体を吹きつけることを特徴とする上記［１］または［２］に記載のリン酸亜鉛処理鋼板の製造方法。
［４］前記表面調整液中には、Ｔｉコロイドを含有することを特徴とする上記［１］〜［３］のいずれかに記載のリン酸亜鉛処理鋼板の製造方法。
The present invention has been made based on the above findings, and the gist thereof is as follows.
[1] After applying the surface conditioning liquid on the surface of the galvanized steel sheet or zinc-based plated steel sheet and performing surface conditioning treatment, the gas was sprayed onto the steel sheet surface at a pressure of 0.20 MPa or more, and then zinc phosphate A method for producing a zinc phosphate-treated steel sheet, comprising forming a zinc phosphate coating by applying a system treatment liquid to a steel sheet surface.
[2] The method for producing a zinc phosphate-treated steel sheet according to the above [1], wherein the spraying pressure is 0.30 MPa or more and 0.40 MPa or less.
[3] The method for producing a zinc phosphate-treated steel sheet according to the above [1] or [2], wherein a gas is blown onto the steel sheet surface using a slit-shaped nozzle.
[4] The method for producing a zinc phosphate-treated steel sheet according to any one of [1] to [3], wherein the surface conditioning liquid contains a Ti colloid.
本発明によれば、表面調整液やリン酸亜鉛系処理液の組成や製造条件を変更することなく、反応ムラを軽減することができる。その結果、表面性状に優れたリン酸亜鉛処理鋼板が製造できる。
表面性状性が大きく改善することが可能となるので、本発明のリン酸亜鉛処理鋼板は、自動車、家電、建材等に好適に用いることができる。
According to the present invention, reaction unevenness can be reduced without changing the composition and manufacturing conditions of the surface conditioning solution and the zinc phosphate-based treatment solution. As a result, a zinc phosphate-treated steel sheet with excellent surface properties can be produced.
Since surface properties can be greatly improved, the zinc phosphate-treated steel sheet of the present invention can be suitably used for automobiles, home appliances, building materials and the like.
本発明の詳細を以下に説明する。 Details of the present invention will be described below.
本発明のリン酸亜鉛処理鋼板は、亜鉛めっき鋼板または亜鉛系めっき鋼板の表面上に表面調整液を塗布し表面調整処理を行った後、鋼板表面に吹きつけ圧力：0.20MPa以上で気体を吹きつけ、次いで、リン酸亜鉛系処理液を鋼板表面に塗布することによりリン酸亜鉛被膜を形成し、製造される。さらに、吹きつけ圧力は、0.30MPa以上0.40MPa以下であることが好ましい。 The zinc phosphate-treated steel sheet of the present invention is applied with a surface conditioning solution on the surface of a galvanized steel sheet or a zinc-based steel sheet, and then subjected to a surface conditioning treatment, and then sprayed onto the steel sheet surface with a pressure of 0.20 MPa or more. Then, a zinc phosphate coating solution is applied to the surface of the steel sheet to form a zinc phosphate coating. Furthermore, the spraying pressure is preferably 0.30 MPa or more and 0.40 MPa or less.
本発明では、表面調整処理を行った後に鋼板表面に吹きつけ圧力：0.20MPa以上で気体を吹き付けることを特徴とする。鋼板表面に吹きつけ圧力：0.20MPa以上で気体を吹き付けることで、鋼板上に付着した表面調整液を均一にレベリングし、リン酸亜鉛処理の反応ムラを抑制することが可能となる。吹きつけ圧力が0.20MPa未満では、表面調整液を均一にレベリングするのが不十分である。吹きつけ圧力が高いほどレベリングには有効である。この点から、吹きつけ圧力は0.30MPa以上が好ましい。一方、0.40MPaを超えると表面調整液が跳ねることでスプラッシュ状のムラが発生する場合がある。最適な外観が得る点から、吹きつけ圧力は0.40MPa以下が好ましい。 The present invention is characterized in that gas is blown at a pressure of 0.20 MPa or more on the surface of the steel sheet after the surface adjustment treatment. By spraying the gas on the surface of the steel sheet at a pressure of 0.20 MPa or more, it is possible to uniformly level the surface conditioning liquid adhering to the steel sheet and suppress reaction unevenness of the zinc phosphate treatment. When the spraying pressure is less than 0.20 MPa, it is insufficient to level the surface conditioning liquid uniformly. Higher spray pressure is more effective for leveling. From this point, the spraying pressure is preferably 0.30 MPa or more. On the other hand, if it exceeds 0.40 MPa, splashing unevenness may occur due to the surface adjustment liquid splashing. From the viewpoint of obtaining an optimal appearance, the spraying pressure is preferably 0.40 MPa or less.
吹きつけ圧力は吹きつけ用ヘッダーの圧力であり、吹きつけノズル先端と鋼板との距離は10〜200mmとすることが望ましい。 The spray pressure is the pressure of the header for spraying, and the distance between the tip of the spray nozzle and the steel plate is preferably 10 to 200 mm.
吹きつけに用いる気体としては、使用する表面調整液の表面調整機能に実用上の影響を及ぼさない気体であれば適用可能である。窒素、ヘリウム、アルゴン等が使用可能である。コストと周囲環境への影響を考慮すると空気（エアー）が最も好適に使用可能である。 As the gas used for spraying, any gas that does not have a practical effect on the surface adjustment function of the surface adjustment liquid to be used is applicable. Nitrogen, helium, argon, etc. can be used. Considering the cost and the influence on the surrounding environment, air (air) can be most suitably used.
また、鋼板表面への気体の吹きつけのノズルの形状はどのようなものでも適用される。中でも、スリット状のノズルを用いることが好ましい。スリット状のノズルを用いることで、スプレー式のノズルと比較し、巾方向の気体吹付けが均一となる。 Further, any shape of nozzle for blowing gas onto the surface of the steel plate is applicable. Among these, it is preferable to use a slit-shaped nozzle. By using the slit-shaped nozzle, the gas blowing in the width direction becomes uniform as compared with the spray type nozzle.
本発明に用いる亜鉛めっき鋼板または亜鉛系めっき鋼板は特に限定がなく、純亜鉛めっき鋼板、Ｚｎ−Ａｌめっき鋼板やＺｎ−Ｎｉめっき鋼板等の合金めっき鋼板のいずれについても用いることができる。また、めっき処理方法についても特に限定がなく、電気めっき、溶融めっき、蒸着めっき等いずれも用いることができる。 The galvanized steel sheet or zinc-based plated steel sheet used in the present invention is not particularly limited, and any galvanized steel sheet, alloy-plated steel sheet such as Zn-Al plated steel sheet or Zn-Ni plated steel sheet can be used. Further, the plating method is not particularly limited, and any of electroplating, hot dipping, vapor deposition plating and the like can be used.
また、上述したように、本発明は、リン酸亜鉛処理鋼板の製造時に表面調整液を使用し表面調整処理を施しているものに対し適用される。 In addition, as described above, the present invention is applied to the case where the surface conditioning treatment is performed using the surface conditioning liquid during the manufacture of the zinc phosphate treated steel sheet.
リン酸亜鉛系処理を行う前に表面調整処理を行うことで、リン酸亜鉛系処理時にリン酸亜鉛系処理液とめっきとの反応性を増大させることができる。 By performing the surface adjustment treatment before the zinc phosphate treatment, the reactivity between the zinc phosphate treatment solution and the plating can be increased during the zinc phosphate treatment.
表面調整液中には、Ｔｉコロイドを含有することが好ましい。表面調整液中にＴｉコロイドを含有させることで、Ｔｉコロイドは分散性が高いためその後のリン酸亜鉛処理時の反応核となりリン酸亜鉛被膜を形成することができる。しかしながら、表面調整液中にＴｉコロイドを含有する場合、表面調整液が不均一な散布状態となれば、リン酸亜鉛結晶の付着量が局部的に不均一となり、リン酸亜鉛結晶の形に差異が生まれ易くなる。これに対して、本発明では、表面調整液が不均一な散布状態になったとしても、その直後に気体を吹き付けることで、表面調整液が均一にレベリングされ、その後のリン酸亜鉛処理時も反応ムラが抑えられた均一な反応状態になると考えられる（図１参照）。 The surface conditioning liquid preferably contains Ti colloid. By containing the Ti colloid in the surface conditioning liquid, the Ti colloid has high dispersibility, so that it becomes a reaction nucleus during the subsequent zinc phosphate treatment and can form a zinc phosphate coating. However, when Ti colloid is contained in the surface conditioning liquid, if the surface conditioning liquid is in a non-uniform spraying state, the amount of zinc phosphate crystals deposited becomes locally non-uniform, resulting in differences in the shape of the zinc phosphate crystals. Becomes easier to be born. On the other hand, in the present invention, even when the surface conditioning liquid is in a non-uniform sprayed state, the surface conditioning liquid is uniformly leveled by spraying the gas immediately after that, even during the subsequent zinc phosphate treatment. It is considered that a uniform reaction state in which uneven reaction is suppressed is obtained (see FIG. 1).
表面調整処理の方法としては、めっき鋼板を表面調整液中に浸漬する方法、めっき鋼板に表面調整液をスプレーする方法等が挙げられる。 Examples of the method of surface adjustment treatment include a method of immersing a plated steel sheet in a surface adjustment liquid, a method of spraying a surface adjustment liquid on the plated steel sheet, and the like.
リン酸亜鉛系処理液としては、特に限定はしない。通常用いられるリン酸亜鉛系処理液を用いることができる。Ｚｎイオン、リン酸イオンの他に硝酸イオン、Ｆ化合物等を含有するものを用いることができる。Ｎｉ、Ｍｎ、Ｍｇ、Ｃｏ、Ｆｅ、Ｃｕを含有させることもできる。 There is no particular limitation on the zinc phosphate processing solution. A commonly used zinc phosphate-based treatment solution can be used. What contains nitrate ion, F compound, etc. in addition to Zn ion and phosphate ion can be used. Ni, Mn, Mg, Co, Fe, Cu can also be contained.
鋼板のリン酸亜鉛処理法としては、特に限定しない。スプレー方式やコーター方式等、従来から用いられている方法を好適に用いることができる。スプレーを用いてリン酸亜鉛被膜を形成することが好ましい。本発明は、実施例としてスプレー方式のリン酸亜鉛処理を行なっているが、原理上、コーター方式のリン酸亜鉛処理にも適用される。 It does not specifically limit as a zinc phosphate processing method of a steel plate. Conventionally used methods such as a spray method and a coater method can be suitably used. It is preferable to form a zinc phosphate coating using a spray. In the present invention, spray zinc phosphate treatment is performed as an example, but in principle, the present invention is also applicable to coater zinc phosphate treatment.
本発明を実施例により更に詳細に説明する。
冷間圧延後焼鈍を施した板厚0.7〜0.8ｍｍの鋼板上に、付着量36ｇ/ｍ2となるように電気亜鉛めっきを施した。次いで、鋼板の表面上に表面調整液（チタンコロイド系処理液、日本パーカライジング（株）製ＰＬ−ＺＮ3.0g/L）を塗布し40℃に3秒浸漬させることで表面調整処理を行った。次いで、表２に示す吹きつけ圧力で鋼板表面に気体を吹きつけた。気体としては空気（エアー）を用いた。次いで、表１に示す浴組成からなるリン酸亜鉛系処理液を鋼板表面に吹き付けることで、リン酸亜鉛系被膜を1.5g/ｍ2形成しリン酸亜鉛処理鋼板を製造した。鋼板表面への気体吹きつけはスリット状のノズルを用いて、リン酸亜鉛系処理液の鋼板表面への吹き付けはスプレーを用いた。
The present invention will be described in more detail with reference to examples.
Electrogalvanizing was performed on a steel sheet having a thickness of 0.7 to 0.8 mm that had been annealed after cold rolling so that the adhesion amount was 36 g / m 2 . Next, a surface conditioning treatment was performed by applying a surface conditioning solution (titanium colloid processing solution, PL-ZN 3.0 g / L manufactured by Nihon Parkerizing Co., Ltd.) on the surface of the steel plate and immersing at 40 ° C. for 3 seconds. Subsequently, gas was sprayed on the steel plate surface with the spraying pressure shown in Table 2. Air (air) was used as the gas. Next, a zinc phosphate-based steel sheet having a bath composition shown in Table 1 was sprayed onto the surface of the steel sheet to form a zinc phosphate-based film at 1.5 g / m 2 to produce a zinc phosphate-treated steel sheet. A gas nozzle was sprayed onto the surface of the steel sheet using a slit nozzle, and a spray was used to spray the zinc phosphate-based treatment liquid onto the steel sheet surface.
以上により得られたリン酸亜鉛処理鋼板に対して、鋼板表面のムラを目視にて観察し、液飛散ムラ、梨肌状ムラ、絞り不良ムラの有無を確認した。なお、液飛散ムラとは、表面調整液のスプレー散布にて、液の散布が不均一であることで飛散状に発生するムラである。梨肌状ムラとは、表面調整セクションの後段絞りロールの荒れにより、ロールが荒れた状態で表面調整液が局所的に不均一な状態に均されることで発生するムラである。絞り不良ムラとは、表面調整セクションの後段絞りロールが表面調整液を絞りきれずに、鋼板上の一部の表面調整液がそのまますり抜けることで発生するムラである。また、各ムラの判定において、○は均一でムラなし、△は一部にムラ有り、×は全面にムラ有りである。全ての評価項目において、評価結果全てが○の場合、もしくは評価結果が△が一つで○が２つの場合を合格とした。 With respect to the zinc phosphate-treated steel sheet obtained as described above, unevenness on the surface of the steel sheet was visually observed, and presence / absence of liquid scattering unevenness, pear skin unevenness and uneven drawing unevenness was confirmed. In addition, the liquid scattering unevenness is unevenness that occurs in a scattered state due to non-uniform liquid spraying in the surface adjustment liquid spray spraying. Pear skin-like unevenness is unevenness that occurs when the surface conditioning liquid is locally leveled in a non-uniform state when the roll is rough due to the roughening of the subsequent drawing roll of the surface adjustment section. Uneven drawing unevenness is unevenness that occurs when a part of the surface adjustment liquid on the steel sheet passes through the surface adjustment section without allowing the subsequent drawing roll to squeeze the surface adjustment liquid. In the determination of each unevenness, ○ is uniform and uneven, Δ is partially uneven, and × is uneven. In all the evaluation items, the case where all the evaluation results were ◯, or the case where the evaluation result was one △ and two ◯, was regarded as acceptable.
以上により得られた結果を条件と併せて表２に示す。 The results obtained as described above are shown in Table 2 together with the conditions.
表２より、本発明例では、ムラが軽減されることが判明した。Ｎｏ１２は、使用上問題なないものの、エアー吹付け圧力が高く、液が飛散した後のようなスプラッシュ状ムラが若干発生していた。
特に吹きつけ圧力を0.30MPa以上0.40MPa以下とした場合に、液飛散ムラ、梨肌状ムラ、絞り不良ムラの全てのムラに対して、ムラなしとなっていた。
From Table 2, it was found that unevenness was reduced in the example of the present invention. Although No 12 had no problem in use, the air spraying pressure was high, and some splash-like unevenness occurred after the liquid was scattered.
In particular, when the spraying pressure was 0.30 MPa or more and 0.40 MPa or less, there was no unevenness with respect to all the unevenness of liquid scattering, pear skin unevenness, and unevenness of drawing.
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| JPS6179782A (en) * | 1984-09-27 | 1986-04-23 | Nippon Parkerizing Co Ltd | Treatment of phosphate |
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