JP2010236074A - 表面処理剤、該表面処理剤を用いためっき鋼板の製造方法およびめっき鋼板 - Google Patents
表面処理剤、該表面処理剤を用いためっき鋼板の製造方法およびめっき鋼板 Download PDFInfo
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- JP2010236074A JP2010236074A JP2009088410A JP2009088410A JP2010236074A JP 2010236074 A JP2010236074 A JP 2010236074A JP 2009088410 A JP2009088410 A JP 2009088410A JP 2009088410 A JP2009088410 A JP 2009088410A JP 2010236074 A JP2010236074 A JP 2010236074A
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- plated steel
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- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- OGUCKKLSDGRKSH-UHFFFAOYSA-N oxalic acid oxovanadium Chemical compound [V].[O].C(C(=O)O)(=O)O OGUCKKLSDGRKSH-UHFFFAOYSA-N 0.000 description 1
- 239000004209 oxidized polyethylene wax Substances 0.000 description 1
- 235000013873 oxidized polyethylene wax Nutrition 0.000 description 1
- QLOKAVKWGPPUCM-UHFFFAOYSA-N oxovanadium;dihydrochloride Chemical compound Cl.Cl.[V]=O QLOKAVKWGPPUCM-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 229940085991 phosphate ion Drugs 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920005749 polyurethane resin Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000006748 scratching Methods 0.000 description 1
- 230000002393 scratching effect Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 description 1
- 125000005372 silanol group Chemical group 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 125000002813 thiocarbonyl group Chemical group *C(*)=S 0.000 description 1
- 229910000348 titanium sulfate Inorganic materials 0.000 description 1
- FOZHTJJTSSSURD-UHFFFAOYSA-J titanium(4+);dicarbonate Chemical compound [Ti+4].[O-]C([O-])=O.[O-]C([O-])=O FOZHTJJTSSSURD-UHFFFAOYSA-J 0.000 description 1
- JUWGUJSXVOBPHP-UHFFFAOYSA-B titanium(4+);tetraphosphate Chemical compound [Ti+4].[Ti+4].[Ti+4].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O JUWGUJSXVOBPHP-UHFFFAOYSA-B 0.000 description 1
- UDUKMRHNZZLJRB-UHFFFAOYSA-N triethoxy-[2-(7-oxabicyclo[4.1.0]heptan-4-yl)ethyl]silane Chemical compound C1C(CC[Si](OCC)(OCC)OCC)CCC2OC21 UDUKMRHNZZLJRB-UHFFFAOYSA-N 0.000 description 1
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 1
- UUUGYDOQQLOJQA-UHFFFAOYSA-L vanadyl sulfate Chemical compound [V+2]=O.[O-]S([O-])(=O)=O UUUGYDOQQLOJQA-UHFFFAOYSA-L 0.000 description 1
- 229940041260 vanadyl sulfate Drugs 0.000 description 1
- 229910000352 vanadyl sulfate Inorganic materials 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000001993 wax Substances 0.000 description 1
- 230000002087 whitening effect Effects 0.000 description 1
- 230000037303 wrinkles Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- 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
- C23C22/00—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
- C23C22/05—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
- 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
- C23C22/40—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 molybdates, tungstates or vanadates
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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Abstract
鋼板の折り曲げ加工部の耐食性、耐溶剤性、アルカリ脱脂後の塗装性に優れた皮膜を金属材料表面に形成することができ、1液で貯蔵安定性に優れたクロムフリー表面処理剤、該表面処理剤を用いためっき鋼板の製造方法、およびめっき鋼板を提供する。
【解決手段】
特定のビスフェノール骨格を有する樹脂化合物、カチオン性ウレタン樹脂エマルション、シランカップリング剤、有機チタンキレート化合物、4価のバナジル化合物と水とを、各々所定の割合で配合し、pHが4〜5であることを特徴とする表面処理剤、該表面処理剤を用いためっき鋼板の製造方法、およびめっき鋼板。
【選択図】なし
Description
(B)第1〜3アミノ基及び第4アンモニウム塩基から選ばれる少なくとも1種のカチオン性官能基を有するカチオン性ウレタン樹脂エマルション(以下「カチオン性ウレタン(B)」という。)と
(C)活性水素含有アミノ基、エポキシ基、メルカプト基およびメタクリロキシ基から選ばれた少なくとも1種の反応性官能基を有する1種以上のシランカップリング剤と
(D)有機チタンキレート化合物と
(E)4価のバナジル化合物と
(F)水とを含み、
カチオン性ウレタン(B)の固形分含有量が、樹脂化合物(A)、カチオン性ウレタン(B)およびシランカップリング剤(C)の固形分合計量に対する質量比[(B)/{(A)+(B)+(C)}]で0.1〜0.3であり、
シランカップリング剤(C)の固形分含有量が、樹脂化合物(A)、カチオン性ウレタン(B)およびシランカップリング剤(C)の固形分合計量に対する質量比[(C)/{(A)+(B)+(C)}]で0.6〜0.85であり、
シランカップリング剤(C)の固形分含有量が、有機チタンキレート化合物(D)のチタン換算含有量に対する質量比{(C)/Ti}で50〜70であり、
4価のバナジル化合物(E)のバナジウム換算含有量が、有機チタンキレート化合物(D)のチタン換算含有量に対する質量比(V/Ti)で0.3〜0.5であり、
且つpHが4〜5であることを特徴とする表面処理剤。
該ワックス(W)の固形分含有量が、樹脂化合物(A)およびカチオン性ウレタン(B)の固形分合計量に対する質量比[(W)/{(A)+(B)}]で0.2〜0.4である上記(1)記載の表面処理剤。
本発明の表面処理剤を用いてめっき鋼板に表面処理皮膜を形成する場合においては、表面処理剤をめっき鋼板に塗布し、到達板温50〜180℃で乾燥し、該鋼板表面に片面当たりの付着量で0.2〜1.8g/m2の表面処理皮膜を形成させることが好ましい。付着量は0.3〜1.6g/m2がより好ましく、0.4〜1.4g/m2がより一層好ましい。付着量が0.2g/m2未満では十分な耐食性が得られず、1.8g/m2を超えると付着量の効果は飽和し、経済的に不利であるばかりか塗装性を低下させる。本発明の表面処理剤をめっき鋼板に塗布する方法としては、ロールコーター(3ロール方式、2ロール方式等)スクイズコーター、ダイコーターなど、いずれの方法でもよい。また、スクイズコーター等による塗布処理、あるいは浸漬処理、スプレー処理の後にエアーナイフ法やロール絞り法により塗布量の調節、外観の均一化、膜厚の均一化を行うことも可能である。
本発明の表面処理剤は、樹脂化合物(A)、カチオン性ウレタン(B)、シランカップリング剤(C)が主成分であり、これらの主成分により皮膜の骨格が形成される。
各サンプルについて塩水噴霧試験(JIS-Z-2371-2000)を行い、120時間経過後の白錆発生面積率で評価した。評価基準は以下の通りである。
◎:白錆発生面積率0%
○+:白錆発生面積率5%未満
○ :白錆発生面積率5%以上、10%未満
○−:白錆発生面積率10%以上、20%未満
△ :白錆発生面積率20%以上、40%未満
× :白錆発生面積率40%以上
各サンプルを直径2mmの棒(ステンレス製)を挟み込むようにして180°曲げて、万力を用いて絞め込んだ。この曲げたサンプルについて塩水噴霧試験(JIS-Z-2371-2000)を行い、72時間経過後の曲げ加工部外(表)側の白錆発生状態を評価した。評価基準は次の通りである。
◎:曲げ加工部に錆発生なし
○+:曲げ加工部の錆発生面積率が5%未満
○ :曲げ加工部の錆発生面積率が5%以上、10%未満
○−:曲げ加工部の錆発生面積率が10%以上、40%未満
△ :曲げ加工部の錆発生面積率が40%以上、80%未満
× :曲げ加工部の錆発生面積率が80%以上
アルカリ脱脂剤CL−N364S(日本パーカライジング(株)製)を20g/lの濃度で純水に溶解し、60℃に加温した。このアルカリ溶液に各サンプルを2分間浸漬し、取り出して水洗して乾燥した。各サンプルについて塩水噴霧試験(JIS-Z-2371-2000)を行い、72時間経過後の白錆発生面積率で評価した。評価基準は上記(1)に示した通りである。
各サンプルを赤外線イメージ炉にて30秒で板温500℃に加熱し、30秒間保持した後、室温まで自然放冷した時の表面外観を目視観察した。その評価基準は以下の通りである。
◎ :変色なし
○ :極僅かに褐色味あり
△ :淡い褐色に変色
× :褐色に変色
各サンプルについてメラミンアルキッド系塗料であるデリコン(登録商標)#700(大日本塗料(株)製)を塗装し、130℃で30分間焼付け、膜厚30μmの塗膜を形成した後、沸騰水に2時間浸漬し、直ちに、碁盤目(10×10個、1mm間隔)の鋼素地まで達するカットを入れた。更にエリクセン押し出し機にてカット部が外(表)側となる様に5mm押し出し加工を施し、接着テープによる貼着・剥離を行い、塗膜の剥離面積を測定した。評価の基準は以下の通りである。なお、エリクセン押し出し条件は、JIS-Z-2247-2006に準拠し、ポンチ径:20mm、ダイス径:27mm、絞り幅:27mmとした。
◎ :剥離なし
○+:剥離面積3%未満
○ :剥離面積3%以上、10%未満
○−:剥離面積10%以上、20%未満
△ :剥離面積20%以上、50%未満
× :剥離面積50%以上
上記(3)と同様のアルカリ脱脂を行い、その各サンプルに上記(5)と同様の塗装性試験を行った。評価基準も同じである。
各サンプルの表面にメタノールを染み込ませたガーゼを4.90N(500gf)の荷重をかけて押し付け、その荷重のまま10回往復するように擦った。その擦った痕を目視にて評価した。評価基準は以下の通りである。
◎ :痕跡なし。
○+:上から見ると痕跡が見えないが、斜めから見ると僅かに見える。
○ :上から見ると痕跡が見ないが、斜めから見ると明らかに見える。
○−:上から見て僅かに痕跡が見える。
△ :上から見て痕跡が明らかに見える。
× :皮膜が剥離している。
表8に示した各表面処理剤を40℃の恒温槽に30日間保管した。取り出して、各表面処理剤の外観を目視によって調べ、評価した。評価基準は次の通りである。更に、上記条件で保管した表面処理剤を使用して製造した表面処理皮膜を有するめっき鋼板について上記した(1)〜(3)の試験を行った。
◎:変化なし
○:極微量の沈殿が見られる
△:微量の沈殿が見られる、もしくはやや粘度が高くなった
×:多量の沈殿が見られる、もしくはゲル化した
各サンプルより直径100mmの円板状の試験片を切り出し、ポンチ径:50mm、ダイス径51.91mm、しわ押さえ力:1トンの条件でカップ状に成型した。成型品の絞り加工を受けた面(カップの側面外側)の外観を目視によって調べ、傷つき程度および黒化程度を評価した。評価基準は次の通りである。
◎ :全面に渡って殆ど変化なく、外観が均一
○+:極僅かに黒化が発生したが、外観は均一
○ :傷つきおよび黒化が少し発生し、外観が明らかに不均一
○−:局部的に傷つきおよび黒化が発生し、外観が明らかに不均一
△ : コーナー部を中心に傷つきおよび黒化が激しく発生
× :成型できずに割れた
Claims (4)
- (A)下記一般式(I)で表されるビスフェノール骨格を有する樹脂化合物(以下「樹脂化合物(A)」という。)と
(B)第1〜3アミノ基及び第4アンモニウム塩基から選ばれる少なくとも1種のカチオン性官能基を有するカチオン性ウレタン樹脂エマルション(以下「カチオン性ウレタン(B)」という。)と
(C)活性水素含有アミノ基、エポキシ基、メルカプト基およびメタクリロキシ基から選ばれた少なくとも1種の反応性官能基を有する1種以上のシランカップリング剤と
(D)有機チタンキレート化合物と
(E)4価のバナジル化合物と
(F)水とを含み、
カチオン性ウレタン(B)の固形分含有量が、樹脂化合物(A)、カチオン性ウレタン(B)およびシランカップリング剤(C)の固形分合計量に対する質量比[(B)/{(A)+(B)+(C)}]で0.1〜0.3であり、
シランカップリング剤(C)の固形分含有量が、樹脂化合物(A)、カチオン性ウレタン(B)およびシランカップリング剤(C)の固形分合計量に対する質量比[(C)/{(A)+(B)+(C)}]で0.6〜0.85であり、
シランカップリング剤(C)の固形分含有量が、有機チタンキレート化合物(D)のチタン換算含有量に対する質量比{(C)/Ti}で50〜70であり、
4価のバナジル化合物(E)のバナジウム換算含有量が、有機チタンキレート化合物(D)のチタン換算含有量に対する質量比(V/Ti)で0.3〜0.5であり、
且つpHが4〜5であることを特徴とする表面処理剤。
- 前記表面処理剤はワックス(W)を更に含み、
該ワックス(W)の固形分含有量が、樹脂化合物(A)およびカチオン性ウレタン(B)の固形分合計量に対する質量比[(W)/{(A)+(B)}]で0.2〜0.4である請求項1記載の表面処理剤。 - 請求項1または2に記載の表面処理剤をめっき鋼板に塗布し、到達板温50〜180℃で乾燥し、該鋼板表面に付着量が0.2〜1.8g/m2である表面処理皮膜を形成することを特徴とするめっき鋼板の製造方法。
- 請求項3記載のめっき鋼板の製造方法を用いて製造されためっき鋼板。
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JP2020100711A (ja) * | 2018-12-21 | 2020-07-02 | 株式会社放電精密加工研究所 | 水性防錆表面処理組成物および表面被覆金属部材 |
JP7232640B2 (ja) | 2018-12-21 | 2023-03-03 | 株式会社放電精密加工研究所 | 水性防錆表面処理組成物および表面被覆金属部材 |
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JP2021050370A (ja) * | 2019-09-20 | 2021-04-01 | Jfeスチール株式会社 | 表面処理皮膜付き亜鉛系めっき鋼板及びその製造方法 |
JP7099424B2 (ja) | 2019-09-20 | 2022-07-12 | Jfeスチール株式会社 | 表面処理皮膜付き亜鉛系めっき鋼板及びその製造方法 |
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