JP2018172787A - 亜鉛系めっき鋼板およびその製造方法 - Google Patents
亜鉛系めっき鋼板およびその製造方法 Download PDFInfo
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- JP2018172787A JP2018172787A JP2018055591A JP2018055591A JP2018172787A JP 2018172787 A JP2018172787 A JP 2018172787A JP 2018055591 A JP2018055591 A JP 2018055591A JP 2018055591 A JP2018055591 A JP 2018055591A JP 2018172787 A JP2018172787 A JP 2018172787A
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- steel sheet
- oxide layer
- zinc
- galvanized steel
- less
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
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- C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/48—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 not containing phosphates, hexavalent chromium compounds, fluorides or complex fluorides, molybdates, tungstates, vanadates or oxalates
- C23C22/53—Treatment of zinc or alloys based thereon
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Abstract
Description
[1]亜鉛系めっき鋼板の表面に酸化物層を有し、前記酸化物層は、平均厚さが20nm以上であり、前記酸化物層中には、Znを30mg/m2以上、Sを1.0mg/m2以上、平均粒子径が5.0μm以下であるポリエチレン粒子を30mg/m2以上1000mg/m2以下含有することを特徴とする亜鉛系めっき鋼板。
[2]亜鉛系めっき鋼板の表面に酸化物層を有し、前記酸化物層は、平均厚さが20nm以上であり、前記酸化物層中には、Znを30mg/m2以上、Sを1.0mg/m2以上、平均粒子径が5.0μm以下であるポリエチレン粒子を50mg/m2以上1000mg/m2以下含有することを特徴とする亜鉛系めっき鋼板。
[3]前記酸化物層には、硫酸基及び水酸基が存在することを特徴とする上記[1]または[2]に記載の亜鉛系めっき鋼板。
[4]前記酸化物層中に、さらに、Pを0.2mg/m2以上10mg/m2以下含有することを特徴とする上記[1]〜[3]のいずれか記載の亜鉛系めっき鋼板。
[5]前記亜鉛系めっき鋼板は、合金化溶融亜鉛めっき鋼板、溶融亜鉛めっき鋼板、電気亜鉛めっき鋼板のいずれかであることを特徴とする上記[1]〜[4]のいずれかに記載の亜鉛系めっき鋼板。
[6]上記[1]〜[5]のいずれかに記載の亜鉛系めっき鋼板の製造方法であって、
亜鉛系めっき鋼板を、硫酸イオンを3g/L以上、Znイオンを3g/L以上およびポリエチレン粒子を0.10g/L以上含有する酸性溶液に接触させることを特徴とする亜鉛系めっき鋼板の製造方法。
[7]前記酸性溶液は、pHが2〜6であり、温度が20℃〜80℃であることを特徴とする上記[6]に記載の亜鉛系めっき鋼板の製造方法。
[8]前記酸性溶液は、酸化剤を含有することを特徴とする上記[6]または[7]に記載の亜鉛系めっき鋼板の製造方法。
[9]前記酸性溶液との接触時間は1秒以上500秒以下であることを特徴とする上記[6]〜[8]のいずれかに記載の亜鉛系めっき鋼板の製造方法。
[10]酸性溶液に接触後、Pイオンを0.01g/L以上含有する溶液に亜鉛系めっき鋼板を接触させることを特徴とする上記[6]〜[9]のいずれかに記載の亜鉛系めっき鋼板の製造方法。
亜鉛系めっき鋼板と金型等との摩擦係数が顕著に低下する。このため、高強度の亜鉛系めっき鋼板や、複雑な成形を施される比較的強度の低い亜鉛系めっき鋼板に対しても安定的に優れたプレス成形性を有することになる。バックドアなどの複雑形状化に必要とされる深絞り加工などの難成形時においても、プレス成形時の割れ危険部位での摺動抵抗が小さく張り出し性が良好である。
また、フッ素樹脂を含有しないため、溶接時にも有害ヒューム発生の懸念がない。
酸化物層中のZn含有量、S含有量については、重クロム酸アンモニウム2質量%+アンモニア水14質量%溶液で、酸化物層を溶解した溶液を、ICP発光分析装置を用いて分析することで定量することが可能である。
まず、鋼板に、亜鉛系めっき処理を施す。めっき処理を施す方法は特に限定されず、溶融亜鉛めっき、電気亜鉛めっき等の一般的な方法を採用可能である。また、めっきの処理条件は特に限定されず、適宜好ましい条件を採用すればよい。さらに、めっき後に、合金化処理を施してもよい。なお、合金化処理の方法は特に限定されず、一般的な方法を採用可能である。
酸化物層を形成する方法としては、亜鉛系めっき鋼板を、硫酸イオン、Znイオン、ポリエチレン粒子を含有する酸性溶液に接触させ、その後水洗を行う方法が挙げられる。なお、必要に応じて、水洗後に乾燥を行ってもよい。具体的には、鋼板を、硫酸イオン:3g/L以上、Znイオン:3g/L以上およびポリエチレン粒子:0.10g/L以上含有する酸性溶液と接触させた後、水洗を行う。平均粒子径が5.0μm以下であるポリエチレン粒子を用いるにあたって、ポリエチレン粒子の製造方法は特に限定しない。平均粒子径が5.0μm以下のポリエチレン製品を用いることもできる。
酸性溶液はpHが2〜6であることが好ましい。pHが2未満では亜鉛系めっき層の溶解が激しく、酸化物層の生成が抑制される場合がある。一方、pHが6超えの酸性溶液では溶液中のZnイオンが析出し、スラッジが発生してしまう場合があり、好ましくなく、酸化物の形成も十分ではない場合がある。よって、酸性溶液のpHは2以上6以下が好ましい。
酸化物層の平均厚さの測定
亜鉛系めっき鋼板に形成された酸化物層の厚みの測定には蛍光X線分析装置を使用した。測定時の管球の電圧および電流は30kVおよび100mAとし、分光結晶はTAPに設定してO−Kα線を検出した。O−Kα線の測定に際しては、そのピーク位置に加えてバックグラウンド位置での強度も測定し、O−Kα線の正味の強度が算出できるようにした。なお、ピーク位置およびバックグラウンド位置での積分時間は、それぞれ20秒とした。
重クロム酸アンモニウム2%+アンモニア水14質量%溶液を用いて、酸化物層のみを溶解し、その溶液を、ICP発光分析装置を用いて、Zn、S、Pの定量分析を実施した。
測定した値を単位面積あたりの含有量に換算し、その値を含有量とした。
走査型電子顕微鏡を用いて、加速電圧5kV、作動距離8.5mm、倍率5000倍でランダムに抽出した5視野を観察し、ポリエチレン粒子の平均粒子径、個数を求めた。観察視野中の単位面積当たりのポリエチレン粒子の合計体積を求め、密度と掛け合わせることで含有量を算出し、5視野の平均値を求めてポリエチレン粒子の含有量とした。
X線光電子分光装置を用いて、Zn、S、Oの存在形態について分析した。Al Ka モノクロ線源を使用し、Zn LMM、 S 2pに相当するスペクトルのナロー測定を実施した。
プレス成形性を評価するために、各供試材の摩擦係数を以下のようにして測定した。
[条件1]
図2に示すビードを用い、押し付け荷重N:400kgf、試料の引き抜き速度(スライドテーブル3の水平移動速度):100cm/minとした。
[条件2]
図3に示すビードを用い、押し付け荷重N:400kgf、試料の引き抜き速度(スライドテーブル3の水平移動速度):20cm/minとした。
(3)脱脂性の評価方法
一部の鋼板については脱脂性の評価を行った。脱脂性の評価は、脱脂後の水濡れ率で評価を行った。作成した試験片に、スギムラ化学工業(株)製のプレス用洗浄油プレトンR352Lを片面2.0g/m2塗油したのち、日本パーカライジング(株)製のFC−E6403のアルカリ脱脂液を用いてサンプルの脱脂を行った。脱脂液にスギムラ化学工業(株)製のプレス用洗浄油プレトンR352Lを10g/Lを予め添加することで自動車生産ラインにおけるアルカリ脱脂液の劣化をシミュレートした。ここで、脱脂時間は60秒とし、温度は37℃とした。脱脂時は脱脂液を直径10cmのプロペラを150rpmの速度で攪拌した。脱脂完了から20秒後の試験片の水濡れ率を測定することで、脱脂性の評価を行った。
3cm角の鋼板の片面をテープでマスクし、塩酸(1+1)にヘキサメチレンテトラミンを添加させた液へ浸漬させ、片面のみポリエチレン以外の皮膜成分を溶解させた。溶液を孔径300nmのガラスフィルターを用いて濾過し、フィルター中にポリエチレンのみを分離捕集した。分離したポリエチレンを、パイロライザー(FRONTIER LAB社製マルチスポットパイロライザ)に導入し、50℃から650℃まで昇温させながらポリエチレンを熱分解した。これをガスクロマトグラフ質量分析装置(Agilent社製6890シリーズ)に導入し、マススペクトルを取得した。得られたマススペクトルについて、ポリエチレンの分解生成物の一つである質量電荷比(m/z)=41のプロファイルを抽出し、そのピーク高さを求めた。既知量のポリエチレンで同様の分析を行い作成した検量線を用いて、ポリエチレン粒子の含有量を単位面積あたりの重量として求めた。
2 試料台
3 スライドテーブル
4 ローラ
5 スライドテーブル支持台
6 ビード
7 第1ロードセル
8 第2ロードセル
9 レール
N 押付荷重
F 摺動抵抗力
Claims (10)
- 亜鉛系めっき鋼板の表面に酸化物層を有し、
前記酸化物層は、平均厚さが20nm以上であり、
前記酸化物層中には、Znを30mg/m2以上、Sを1.0mg/m2以上、平均粒子径が5.0μm以下であるポリエチレン粒子を30mg/m2以上1000mg/m2以下含有することを特徴とする亜鉛系めっき鋼板。 - 亜鉛系めっき鋼板の表面に酸化物層を有し、
前記酸化物層は、平均厚さが20nm以上であり、
前記酸化物層中には、Znを30mg/m2以上、Sを1.0mg/m2以上、平均粒子径が5.0μm以下であるポリエチレン粒子を50mg/m2以上1000mg/m2以下含有することを特徴とする亜鉛系めっき鋼板。 - 前記酸化物層には、硫酸基及び水酸基が存在することを特徴とする請求項1または2に記載の亜鉛系めっき鋼板。
- 前記酸化物層中に、さらに、Pを0.2mg/m2以上10mg/m2以下含有することを特徴とする請求項1〜3のいずれかに記載の亜鉛系めっき鋼板。
- 前記亜鉛系めっき鋼板は、合金化溶融亜鉛めっき鋼板、溶融亜鉛めっき鋼板、電気亜鉛めっき鋼板のいずれかであることを特徴とする請求項1〜4のいずれかに記載の亜鉛系めっき鋼板。
- 請求項1〜5のいずれかに記載の亜鉛系めっき鋼板の製造方法であって、
亜鉛系めっき鋼板を、硫酸イオンを3g/L以上、Znイオンを3g/L以上およびポリエチレン粒子を0.10g/L以上含有する酸性溶液に接触させることを特徴とする亜鉛系めっき鋼板の製造方法。 - 前記酸性溶液は、pHが2〜6であり、温度が20℃〜80℃であることを特徴とする請求項6に記載の亜鉛系めっき鋼板の製造方法。
- 前記酸性溶液は、酸化剤を含有することを特徴とする請求項6または7に記載の亜鉛系めっき鋼板の製造方法。
- 前記酸性溶液との接触時間は1秒以上500秒以下であることを特徴とする請求項6〜8のいずれかに記載の亜鉛系めっき鋼板の製造方法。
- 酸性溶液に接触後、Pイオンを0.01g/L以上含有する溶液に亜鉛系めっき鋼板を接触させることを特徴とする請求項6〜9のいずれかに記載の亜鉛系めっき鋼板の製造方法。
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