JP6605538B2 - 亜鉛系めっき鋼板用リン酸塩溶液、それを用いた耐変色性及びフィルム接着性に優れたリン酸塩処理亜鉛系めっき鋼板、並びにその製造方法 - Google Patents
亜鉛系めっき鋼板用リン酸塩溶液、それを用いた耐変色性及びフィルム接着性に優れたリン酸塩処理亜鉛系めっき鋼板、並びにその製造方法 Download PDFInfo
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- 229910019142 PO4 Inorganic materials 0.000 title claims description 124
- 239000010452 phosphate Substances 0.000 title claims description 124
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 title claims description 123
- 229910001335 Galvanized steel Inorganic materials 0.000 title claims description 24
- 239000008397 galvanized steel Substances 0.000 title claims description 24
- 238000004519 manufacturing process Methods 0.000 title claims description 11
- 238000002845 discoloration Methods 0.000 title description 13
- 239000011701 zinc Substances 0.000 claims description 53
- 229910000831 Steel Inorganic materials 0.000 claims description 47
- 239000010959 steel Substances 0.000 claims description 47
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 41
- 229910052725 zinc Inorganic materials 0.000 claims description 41
- 239000002253 acid Substances 0.000 claims description 12
- 239000003795 chemical substances by application Substances 0.000 claims description 10
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical group [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 9
- 239000010936 titanium Substances 0.000 claims description 9
- 229910052719 titanium Inorganic materials 0.000 claims description 9
- 230000003750 conditioning effect Effects 0.000 claims description 7
- 238000005238 degreasing Methods 0.000 claims description 4
- 239000000084 colloidal system Substances 0.000 claims 1
- 239000013078 crystal Substances 0.000 description 38
- 239000011248 coating agent Substances 0.000 description 12
- 238000000576 coating method Methods 0.000 description 12
- 239000011777 magnesium Substances 0.000 description 10
- 238000000034 method Methods 0.000 description 8
- 229910000576 Laminated steel Inorganic materials 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 6
- 239000000853 adhesive Substances 0.000 description 4
- 230000001070 adhesive effect Effects 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000005530 etching Methods 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 230000007797 corrosion Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000007747 plating Methods 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 238000010030 laminating Methods 0.000 description 2
- 238000003475 lamination Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- SPDJAIKMJHJYAV-UHFFFAOYSA-H trizinc;diphosphate;tetrahydrate Chemical group O.O.O.O.[Zn+2].[Zn+2].[Zn+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O SPDJAIKMJHJYAV-UHFFFAOYSA-H 0.000 description 2
- VZSRBBMJRBPUNF-UHFFFAOYSA-N 2-(2,3-dihydro-1H-inden-2-ylamino)-N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]pyrimidine-5-carboxamide Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C(=O)NCCC(N1CC2=C(CC1)NN=N2)=O VZSRBBMJRBPUNF-UHFFFAOYSA-N 0.000 description 1
- YLZOPXRUQYQQID-UHFFFAOYSA-N 3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]propan-1-one Chemical compound N1N=NC=2CN(CCC=21)CCC(=O)N1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F YLZOPXRUQYQQID-UHFFFAOYSA-N 0.000 description 1
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 description 1
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 description 1
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 description 1
- 229910001297 Zn alloy Inorganic materials 0.000 description 1
- 238000004873 anchoring Methods 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000005001 laminate film Substances 0.000 description 1
- 229910001425 magnesium ion Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910001453 nickel ion Inorganic materials 0.000 description 1
- -1 nitrate ions Chemical class 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 125000002467 phosphate group Chemical group [H]OP(=O)(O[H])O[*] 0.000 description 1
- 229910052827 phosphophyllite Inorganic materials 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
Images
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
- C23C22/07—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 phosphates
-
- 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
- C23C2/00—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
- C23C2/04—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor characterised by the coating material
- C23C2/06—Zinc or cadmium or alloys based thereon
-
- 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
- C23C2/00—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
- C23C2/50—Controlling or regulating the coating processes
- C23C2/52—Controlling or regulating the coating processes with means for measuring or sensing
- C23C2/526—Controlling or regulating the coating processes with means for measuring or sensing for visually inspecting the surface quality of the substrate
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/22—Electroplating: Baths therefor from solutions of zinc
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/48—After-treatment of electroplated surfaces
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Mechanical Engineering (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Quality & Reliability (AREA)
- Chemical Treatment Of Metals (AREA)
Description
亜鉛イオンは、リン酸塩結晶を形成するための必須成分である。若し、その含量が過度に低いと、リン酸塩結晶が粗大かつ不均一に形成されるという問題がある。そのため、500ppm以上含まれることが好ましく、800ppm以上含まれることがより好ましい。但し、その含量が過度に多いと、リン酸塩結晶が非常に密な針状に形成され、フィルム接着性が低下するという問題がある。そのため、2000ppm以下で含まれることが好ましく、1700ppm以下で含まれることがより好ましい。
ニッケルイオンは、リン酸塩皮膜の耐食性、耐熱性、及びフィルム接着性を向上させるために添加される成分である。本発明においてこのような効果を得るためには、50ppm以上含まれることが好ましく、300ppm以上含まれることがより好ましい。但し、その含量が過度に多いと、リン酸塩結晶が非常に密な針状に形成され、フィルム接着性が低下するという問題がある。そのため、1000ppm以下で含まれることが好ましく、400ppm以下で含まれることがより好ましい。
マグネシウムイオンは、リン酸塩皮膜の耐食性、耐熱性、及びフィルム接着性を向上させるために添加される成分である。さらに、本発明では、リン酸塩皮膜内のリン酸塩結晶を針状ではない長軸の長さ方向には短く、幅方向にはやや丸くて厚みがあるように形成する上で主な役割を果たす成分である。本発明において、このような効果をもたらすためには、3000ppm以上含まれることが好ましく、5000ppm以上含まれることがより好ましく、8000ppm以上含まれることがさらに好ましい。但し、その含量が過度に多いと、フォスフォフィライト組織のように過度に丸みのあるリン酸塩結晶が形成され、接着力の向上に有利でなくなり、さらに、耐食性、耐熱性などの物性も低下するという問題がある。そのため、40000ppm以下で含まれることが好ましく、30000ppm以下で含まれることがより好ましく、20000ppm以下で含まれることがさらに好ましい。
先ず、他の条件は全て同じとし、リン酸塩溶液中のZn2+濃度のみを変化 させて合計9個の試片を製造し、製造されたそれぞれの試片に対してリン酸塩結晶の形態(morphology)を観察し、フィルム接着性を評価した。このとき、全ての試片は製造時に、350ppmのNi+と、10000ppmのMg2+と、20000ppmのPO4 3−と、25000ppmのNO3 −とを含み、酸比としては10のリン酸塩溶液を用い(Zn2+濃度は下記表1に表記)、表面調整剤としてはチタン0.2重量%含有のチタンコロイド系活性処理剤を用い、リン酸塩皮膜の形成時の亜鉛系めっき鋼板の表面温度は55℃で、皮膜付着量は1.3〜1.5g/m2であった。
次に、他の条件は全て同じとし、リン酸塩溶液中のMg2+濃度のみを変化させて合計10個の試片を製造し、製造されたそれぞれの試片に対してリン酸塩結晶の形態(morphology)を観察し、フィルム接着性を評価した。このとき、全ての試片は製造時に、300ppmのNi+と、1000ppmのZn2+と、20000ppmのPO4 3−と、25000ppmのNO3 −とを含み、酸比としては10のリン酸塩溶液を用い(Mg2+濃度は下記表3に表記)、その他の条件はいずれも実施例1と同様にした。その結果を下記図2及び表4に示した。ここで、図2a〜図2hのそれぞれは、試片2−1乃至2−8の表面を観察したSEM像である。
Claims (5)
- 800〜1700ppmのZn2+と、50〜1000ppmのNi+と、8000〜20000ppmのMg2+と、5000〜40000ppmのPO 4 3− と、5000〜40000ppmのNO 3 − と、を含み、酸比(全酸度/遊離酸度)が2〜20である、亜鉛系めっき鋼板用リン酸塩溶液。
- 亜鉛系めっき鋼板を準備する段階と、
前記亜鉛系めっき鋼板の表面を脱脂する段階と、
前記脱脂された亜鉛系めっき鋼板の表面を、表面調整剤を用いて表面調整処理する段階と、
前記表面調整処理された亜鉛系めっき鋼板の表面に、リン酸塩溶液を用いてリン酸塩皮膜を形成する段階と、を含み、
前記リン酸塩溶液は、800〜1700ppmのZn2+と、50〜1000ppmのNi+と、8000〜20000ppmのMg2+と、5000〜40000ppmのPO 4 3− と、5000〜40000ppmのNO 3 − と、を含み、酸比(全酸度/遊離酸度)が2〜20である、
リン酸塩処理亜鉛系めっき鋼板の製造方法。 - 前記表面調整処理に用いられる表面調整剤はチタンコロイド系活性処理剤である、請求項2に記載のリン酸塩処理亜鉛系めっき鋼板の製造方法。
- 前記チタンコロイド系活性処理剤に含有されたチタンの含量は0.05〜0.6重量%である、請求項3に記載のリン酸塩処理亜鉛系めっき鋼板の製造方法。
- 前記リン酸塩皮膜を形成する際、前記亜鉛系めっき鋼板の表面温度は50〜70℃である、請求項2〜4のいずれか1項に記載のリン酸塩処理亜鉛系めっき鋼板の製造方法。
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US6753095B1 (en) * | 1999-08-09 | 2004-06-22 | Nippon Steel Corporation | Zinc-based metal plated steel sheet treated with phosphate being excellent in formability and method for production thereof |
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