JP6642774B1 - Snめっき鋼板及びSnめっき鋼板の製造方法 - Google Patents
Snめっき鋼板及びSnめっき鋼板の製造方法 Download PDFInfo
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- JP6642774B1 JP6642774B1 JP2019541379A JP2019541379A JP6642774B1 JP 6642774 B1 JP6642774 B1 JP 6642774B1 JP 2019541379 A JP2019541379 A JP 2019541379A JP 2019541379 A JP2019541379 A JP 2019541379A JP 6642774 B1 JP6642774 B1 JP 6642774B1
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- steel sheet
- plated steel
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- zirconium oxide
- zirconium
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- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 138
- 239000010959 steel Substances 0.000 title claims abstract description 138
- 238000004519 manufacturing process Methods 0.000 title claims description 23
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims abstract description 66
- 229910001928 zirconium oxide Inorganic materials 0.000 claims abstract description 66
- 239000010410 layer Substances 0.000 claims abstract description 60
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims abstract description 59
- 229910001887 tin oxide Inorganic materials 0.000 claims abstract description 59
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- 238000010438 heat treatment Methods 0.000 claims description 52
- 239000000463 material Substances 0.000 claims description 37
- 238000005868 electrolysis reaction Methods 0.000 claims description 30
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- -1 zirconium ions Chemical class 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 9
- 239000001301 oxygen Substances 0.000 claims description 9
- 229910052760 oxygen Inorganic materials 0.000 claims description 9
- GBNDTYKAOXLLID-UHFFFAOYSA-N zirconium(4+) ion Chemical compound [Zr+4] GBNDTYKAOXLLID-UHFFFAOYSA-N 0.000 claims description 7
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- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 4
- 229910052698 phosphorus Inorganic materials 0.000 description 4
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- 229910002651 NO3 Inorganic materials 0.000 description 2
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- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 2
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- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 description 1
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- 150000002367 halogens Chemical class 0.000 description 1
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- 229910000166 zirconium phosphate Inorganic materials 0.000 description 1
- LEHFSLREWWMLPU-UHFFFAOYSA-B zirconium(4+);tetraphosphate Chemical compound [Zr+4].[Zr+4].[Zr+4].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LEHFSLREWWMLPU-UHFFFAOYSA-B 0.000 description 1
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- B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B15/043—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of metal
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- B32B15/18—Layered products comprising a layer of metal comprising iron or steel
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- C23C22/361—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 containing fluorides or complex fluorides containing also phosphates containing titanium, zirconium or hafnium compounds
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Abstract
Description
本願は、2018年3月1日に、日本国に出願された特願2018−036587号に基づき優先権を主張し、その内容をここに援用する。
[2]本発明の一態様に係るSnめっき鋼板の製造方法は、鋼板の少なくとも片面に、Snを0.1g/m2以上15g/m2以下含有するSnめっき層が形成された母材めっき鋼板に対して、ジルコニウムイオンを含有する溶液中への浸漬処理、又は、ジルコニウムイオンを含有する溶液中での陰極電解処理を施すことで、ジルコニウム酸化物を含有するジルコニウム酸化物層を形成させる第1の工程と;前記第1の工程の後、前記ジルコニウム酸化物層が形成された前記母材めっき鋼板を、酸素を含有する雰囲気下において、単位がKである加熱温度T、及び単位がHourである加熱時間tに関する以下の式1及び式2を共に満足する条件で加熱処理する第2の工程と;を有する。
0.11×exp(2400/T)<t<0.65×exp(2400/T)・・・(式1)
308<T<373 ・・・(式2)
[3]上記[2]の態様において、前記第2の工程における前記加熱処理が、酸素を含有し、かつ、水蒸気量が60体積%以上90体積%以下の範囲内である雰囲気下で実施されてもよい。
[4]上記[2]又は上記[3]の態様において、前記ジルコニウムイオンを含有する溶液のジルコニウムイオン濃度が、100ppm以上4000ppm以下であり、前記ジルコニウムイオンを含有する溶液のpH値が、3以上5以下であってもよい。
[5]上記[2]〜[4]の何れか1項に記載の態様において、前記第1の工程で、前記ジルコニウム酸化物層を、陰極電解処理により形成し、前記陰極電解処理における電流密度を、0.05A/dm2以上50A/dm2以下としてもよい。
図1に示すように、本実施形態に係るSnめっき鋼板10は、鋼板1の少なくとも片方の表面1aにSnめっき層2の形成された母材めっき鋼板3の表面に、所定量のジルコニウム酸化物と酸化スズとを含有する皮膜層4を有する。
なお、図1では、鋼板1の片面である表面1aのみにSnめっき層2及び皮膜層4がこの順に形成されている場合を示すが、この形態のみに限らない。すなわち、上記構成に加え、鋼板1の裏面1bに、Snめっき層2及び皮膜層4がこの順に形成されている場合も含まれる。このように両面にSnめっき層2が形成される場合、表面1aに形成されたSnめっき層2におけるSnの付着量が、0.1g/m2以上15g/m2以下であり、同時に、裏面1bに形成されたSnめっき層2におけるSnの付着量も、0.1g/m2以上15g/m2以下であってもよい。さらには、鋼板1の両面にSnめっき層2が形成されるが、それらのうちの一方におけるSnめっき層2のSnの付着量が0.1g/m2以上15g/m2以下であるものの、他方におけるSnめっき層2のSnの付着量が0.1g/m2以上15g/m2以下の範囲外であってもよい。
なお、皮膜層4における、ジルコニウム酸化物の含有量、及び、XPSによるSn3d5/2の結合エネルギーのピーク位置を測定する際、皮膜層4の最表層の汚れによる測定精度への影響を排除する必要がある。そのために、被膜層4の最表層をエッチングし、皮膜層4の少し内部に入った位置(例えばエッチング前の表層位置よりも0.5nmの深さ位置)から5nm深さ位置までの範囲内で測定することが好ましい。
本実施形態に係るSnめっき鋼板10の母材として用いられる鋼板1は、特に規定されるものではなく、一般的な容器用のSnめっき鋼板に用いられている鋼板であれば、任意のものを使用可能である。このような鋼板1として、例えば、低炭素鋼や極低炭素鋼などが挙げられる。また、用いる鋼板1の製造方法や材質についても、特に規定されるものではなく、例えば、鋳造から熱間圧延、酸洗、冷間圧延、焼鈍、調質圧延等の工程を経て製造された鋼板を適宜利用することができる。
上記のような鋼板1の少なくとも片面には、Snめっきが施されて、Snめっき層2が形成される。かかるSnめっき層2によって、鋼板1の塗装後耐食性は向上する。なお、本明細書における「Snめっき」とは、金属Snによるめっきだけでなく、金属Snに不純物が混入しためっきや、金属Snに微量元素が含有されているめっきについても、含むものとする。
本実施形態に係るSnめっき鋼板10は、上記のようなSnめっき層2を有する母材めっき鋼板3の表面に、ジルコニウム酸化物と酸化スズの両者を含有する皮膜層4を有する。前述のように、かかる皮膜層4中におけるジルコニウム酸化物の含有量は、金属Zr量で、片面当たり1mg/m2以上30mg/m2以下の範囲内である。皮膜層4中における酸化スズは、XPSによるSn3d5/2の結合エネルギーのピーク位置が、金属Snの結合エネルギーのピーク位置から1.4eV以上1.6eV未満の範囲内にあり、かつ、酸化スズの還元に要する電気量が、5.0mC/cm2超20mC/cm2以下の範囲内である。
本実施形態に係るSnめっき鋼板10において、片面当たりのSn付着量は、金属Sn量として、0.1g/m2以上15g/m2以下とする。以下で詳述するように、本実施形態に係るSnめっき鋼板10の皮膜層4は、ジルコニウム酸化物層が形成されたSnめっき鋼板(素材)を所定の条件下で加熱処理して、Snめっき層2中のSnをジルコニウム酸化物層中に拡散させることで形成される。従って、上記片面当たりのSn付着量は、本実施形態に係るSnめっき鋼板10において、Snめっき層2中に存在する、皮膜層4中に拡散していないSnの含有量と、皮膜層4中に存在する酸化スズの金属Sn換算量と、の合計値である。
以下では、本実施形態に係るSnめっき鋼板の製造方法について、詳細に説明する。本実施形態に係るSnめっき鋼板の製造方法では、鋼板1の少なくとも片面に、片面当たりのSn付着量が0.1g/m2以上15g/m2以下となるようにSnめっき層2の形成された母材めっき鋼板3が、素材として用いられる。
308<T<373 ・・・(式102)
0.33×exp(2400/T)<t<0.44×exp(2400/T)・・・(式104)
<試験材>
板厚0.2mmの低炭素冷延鋼板(鋼板1に対応)に対し、前処理として、電解アルカリ脱脂、水洗、希硫酸浸漬酸洗、水洗した後、フェノールスルホン酸浴を用いて電気Snめっきを施し、更にその後、加熱溶融処理をした。Snめっきの付着量は、片面当たり約2.8g/m2を標準としたが、一部の試験材は、通電時間を変えることでSnめっきの付着量を変化させた。また、電気Snめっき後に加熱溶融処理をしない試験材も、あわせて作製した。Snめっき付着量は、蛍光X線法(リガク社製ZSX Primus)により測定することで特定した。
各試験材の皮膜層における片面当たりのZr付着量は、リガク社製ZSX Primusを用いて、蛍光X線法により測定した。得られたZr付着量を、以下の表1に併せて示した。
各試験材について、窒素ガスのバブリングにより溶存酸素を除去した0.001mol/Lの臭化水素酸水溶液中において、0.06mA/cm2の定電流で陰極電解し、酸化スズを還元除去するまでに要する時間と電流との積から、酸化スズの還元に要する電気量を測定した。測定した電気量を、以下の表1の「酸化スズ量」の欄に併せて示した。
各試験材について、XPS(ULVAC−PHI製PHI Quantera SXM)を用いてSn3d5/2の結合エネルギーのピーク位置を測定し、金属Snの結合エネルギーのピーク位置からのピーク位置のシフト量を算出した。得られたシフト量を、以下の表1の「Sn3d5/2の結合エネルギーピーク位置」の欄に併せて示した。
耐黄変性は、以下のようにして評価した。
上記のようにして作製した各試験材を、40℃、相対湿度80%に保持した恒温恒湿槽中に4週間載置する湿潤試験を行い、湿潤試験前後における色座標b*値の変化量△b*を求めて、評価した。変化量△b*が1以下であれば3点とし、1超過2以下であれば2点とし、2〜3であれば1点とし、3を超過していれば0点とし、評価1点以上を合格とした。なお、色座標b*は、市販の色差計であるスガ試験機製SC−GV5を用いて測定し、色座標b*の測定条件は、光源C、全反射、測定径30mmとした。
耐硫化黒変性は、以下のようにして評価した。
上記のようにして作製した各試験材の表面に、市販の缶用エポキシ樹脂塗料を乾燥質量で7g/m2塗布した後、200℃で10分焼き付け、24時間室温に置いた。その後、得られた各試験材を所定のサイズに切断し、0.3質量%のリン酸二水素ナトリウム、0.7質量%のリン酸水素ナトリウム、0.6質量%のL−システイン塩酸塩をそれぞれ含有する水溶液中に浸漬し、密封容器中で121℃・60分のレトルト処理を行い、試験後の外観から評価した。試験前後で外観の変化が全く認められなければ2点とし、僅かに黒変が認められれば(黒変した面積が10%以下であれば)1点とし、試験面の10%超過の領域に黒変が認められれば0点とし、評価1点以上を合格とした。
塗膜密着性は、以下のようにして評価した。
上記のようにして作製した各試験材を、上記[耐黄変性]に記載の方法で湿潤試験した後、表面に、市販の缶用エポキシ樹脂塗料を乾燥質量で7g/m2塗布し、200℃で10分焼き付け、24時間室温に置いた。その後、得られた各試験材に対し、鋼板表面に達する傷を碁盤目状に入れ(3mm間隔で縦横7本ずつの傷)、その部位のテープ剥離試験をすることで評価した。テープ貼り付け部位の塗膜が全て剥離していなければ2点とし、碁盤目の傷部周囲で塗膜剥離が認められれば1点とし、碁盤目の枡内に塗膜剥離が認められれば0点とし、評価1点以上を合格とした。
塗装後耐食性は、以下のようにして評価した。
上記[塗膜密着性]に記載の方法で作製及び湿潤試験した各試験材の表面に、市販の缶用エポキシ樹脂塗料を乾燥質量で7g/m2塗布した後、200℃で10分焼き付け、24時間室温に置いた。その後、得られた各試験材を40mm×40mmのサイズに切断し、市販のトマトジュースに60℃の温度環境下で7日間浸漬した後の錆の発生有無を、目視にて評価した。錆が全く認められなければ2点とし、僅かに錆が認められれば(発錆した面積が5%以下であれば)1点とし、錆が5%超認められれば0点とし、評価1点以上を合格とした。
また、総合性能として、各種性能の評点の合計を求め、その合計値が8点又は9点である場合を「Very Good」とし、6点又は7点である場合を「Good」とし、4点又は5点である場合を「Fair」とし、何れか一つの性能において0点が存在する場合は、合計値を0点として「Bad」とし、評点Very Good、Good、Fairを合格とした。
板厚0.2mmの低炭素冷延鋼板に対し、前処理として、電解アルカリ脱脂、水洗、希硫酸浸漬酸洗、水洗した後、フェノールスルホン酸浴を用いて電気Snめっきを施し、更にその後、加熱溶融処理をした。Snの付着量は、片面当たり2.8g/m2とした。
2 Snめっき層
3 母材めっき鋼板
4 皮膜層
10 Snめっき鋼板
Claims (5)
- 鋼板、及び、前記鋼板の少なくとも片面にSnめっき層を有する母材めっき鋼板と;
前記母材めっき鋼板上に位置する、ジルコニウム酸化物と酸化スズとを含有する皮膜層と;
を備え、
片面当たりのSnの付着量が、0.1g/m2以上15g/m2以下であり、
前記皮膜層中における前記ジルコニウム酸化物の含有量が、金属Zr量で1mg/m2以上30mg/m2以下の範囲内であり、
前記皮膜層中における前記酸化スズのX線光電子分光法によるSn3d5/2の結合エネルギーのピーク位置が、金属Snの結合エネルギーのピーク位置から1.4eV以上1.6eV未満の範囲内にあり、
前記酸化スズの還元に要する電気量が、5.0mC/cm2超20mC/cm2以下の範囲内である、
Snめっき鋼板。 - 鋼板の少なくとも片面に、Snを0.1g/m2以上15g/m2以下含有するSnめっき層が形成された母材めっき鋼板に対して、ジルコニウムイオンを含有する溶液中への浸漬処理、又は、ジルコニウムイオンを含有する溶液中での陰極電解処理を施すことで、ジルコニウム酸化物を含有するジルコニウム酸化物層を形成させる第1の工程と;
前記第1の工程の後、前記ジルコニウム酸化物層が形成された前記母材めっき鋼板を、酸素を含有する雰囲気下において、単位がKである加熱温度T、及び単位がHourである加熱時間tに関する以下の式1及び式2を共に満足する条件で加熱処理する第2の工程と;
を有する、Snめっき鋼板の製造方法。
0.11×exp(2400/T)<t<0.65×exp(2400/T)・・・(式1)
308<T<373 ・・・(式2) - 前記第2の工程における前記加熱処理は、酸素を含有し、かつ、水蒸気量が60体積%以上90体積%以下の範囲内である雰囲気下で実施される、請求項2に記載のSnめっき鋼板の製造方法。
- 前記ジルコニウムイオンを含有する溶液のジルコニウムイオン濃度は、100ppm以上4000ppm以下であり、前記ジルコニウムイオンを含有する溶液のpH値は、3以上5以下である、請求項2又は3に記載のSnめっき鋼板の製造方法。
- 前記第1の工程で、
前記ジルコニウム酸化物層を、陰極電解処理により形成し、
前記陰極電解処理における電流密度を、0.05A/dm2以上50A/dm2以下とする、
請求項2〜4の何れか1項に記載のSnめっき鋼板の製造方法。
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