JPWO2015080066A1 - 表面処理皮膜付き亜鉛系めっき鋼板およびその製造方法 - Google Patents
表面処理皮膜付き亜鉛系めっき鋼板およびその製造方法 Download PDFInfo
- Publication number
- JPWO2015080066A1 JPWO2015080066A1 JP2015512930A JP2015512930A JPWO2015080066A1 JP WO2015080066 A1 JPWO2015080066 A1 JP WO2015080066A1 JP 2015512930 A JP2015512930 A JP 2015512930A JP 2015512930 A JP2015512930 A JP 2015512930A JP WO2015080066 A1 JPWO2015080066 A1 JP WO2015080066A1
- Authority
- JP
- Japan
- Prior art keywords
- film
- surface treatment
- steel sheet
- zinc
- phosphoric acid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
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- 238000004381 surface treatment Methods 0.000 title claims abstract description 138
- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 81
- 239000010959 steel Substances 0.000 title claims abstract description 81
- 239000011701 zinc Substances 0.000 title claims abstract description 66
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 title claims abstract description 65
- 229910052725 zinc Inorganic materials 0.000 title claims abstract description 65
- 238000004519 manufacturing process Methods 0.000 title claims description 9
- 239000007788 liquid Substances 0.000 claims abstract description 103
- -1 zirconium carbonate compound Chemical class 0.000 claims abstract description 94
- NBIIXXVUZAFLBC-UHFFFAOYSA-N phosphoric acid Substances OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 58
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 52
- 238000000576 coating method Methods 0.000 claims abstract description 28
- 238000001035 drying Methods 0.000 claims abstract description 24
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- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 17
- 125000003700 epoxy group Chemical group 0.000 claims abstract description 12
- 239000007787 solid Substances 0.000 claims description 52
- 239000000839 emulsion Substances 0.000 claims description 39
- 229910052727 yttrium Inorganic materials 0.000 claims description 29
- 239000011248 coating agent Substances 0.000 claims description 24
- 229910001335 Galvanized steel Inorganic materials 0.000 claims description 20
- 239000008397 galvanized steel Substances 0.000 claims description 20
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 13
- 150000002816 nickel compounds Chemical class 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 claims description 10
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- 229910052751 metal Inorganic materials 0.000 description 7
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- 239000002932 luster Substances 0.000 description 6
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- 229910000166 zirconium phosphate Inorganic materials 0.000 description 6
- 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 6
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- 150000001252 acrylic acid derivatives Chemical class 0.000 description 2
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- 239000003795 chemical substances by application Substances 0.000 description 2
- ZCDOYSPFYFSLEW-UHFFFAOYSA-N chromate(2-) Chemical compound [O-][Cr]([O-])(=O)=O ZCDOYSPFYFSLEW-UHFFFAOYSA-N 0.000 description 2
- 229920001577 copolymer Polymers 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- XPPKVPWEQAFLFU-UHFFFAOYSA-J diphosphate(4-) Chemical group [O-]P([O-])(=O)OP([O-])([O-])=O XPPKVPWEQAFLFU-UHFFFAOYSA-J 0.000 description 2
- 235000011180 diphosphates Nutrition 0.000 description 2
- 125000001301 ethoxy group Chemical group [H]C([H])([H])C([H])([H])O* 0.000 description 2
- 230000001771 impaired effect Effects 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
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- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 description 2
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- 125000002467 phosphate group Chemical group [H]OP(=O)(O[H])O[*] 0.000 description 2
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 2
- 125000002572 propoxy group Chemical group [*]OC([H])([H])C(C([H])([H])[H])([H])[H] 0.000 description 2
- CMZUMMUJMWNLFH-UHFFFAOYSA-N sodium metavanadate Chemical compound [Na+].[O-][V](=O)=O CMZUMMUJMWNLFH-UHFFFAOYSA-N 0.000 description 2
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- UNXRWKVEANCORM-UHFFFAOYSA-I triphosphate(5-) Chemical compound [O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O UNXRWKVEANCORM-UHFFFAOYSA-I 0.000 description 2
- 150000003682 vanadium compounds Chemical class 0.000 description 2
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- RRIWRJBSCGCBID-UHFFFAOYSA-L nickel sulfate hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-]S([O-])(=O)=O RRIWRJBSCGCBID-UHFFFAOYSA-L 0.000 description 1
- 229940116202 nickel sulfate hexahydrate Drugs 0.000 description 1
- AOPCKOPZYFFEDA-UHFFFAOYSA-N nickel(2+);dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O AOPCKOPZYFFEDA-UHFFFAOYSA-N 0.000 description 1
- JOCJYBPHESYFOK-UHFFFAOYSA-K nickel(3+);phosphate Chemical compound [Ni+3].[O-]P([O-])([O-])=O JOCJYBPHESYFOK-UHFFFAOYSA-K 0.000 description 1
- 229910000008 nickel(II) carbonate Inorganic materials 0.000 description 1
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 1
- ZULUUIKRFGGGTL-UHFFFAOYSA-L nickel(ii) carbonate Chemical compound [Ni+2].[O-]C([O-])=O ZULUUIKRFGGGTL-UHFFFAOYSA-L 0.000 description 1
- 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
- 231100000989 no adverse effect Toxicity 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 235000021317 phosphate Nutrition 0.000 description 1
- ACVYVLVWPXVTIT-UHFFFAOYSA-M phosphinate Chemical compound [O-][PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-M 0.000 description 1
- ACVYVLVWPXVTIT-UHFFFAOYSA-N phosphinic acid Chemical compound O[PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-N 0.000 description 1
- UEZVMMHDMIWARA-UHFFFAOYSA-M phosphonate Chemical compound [O-]P(=O)=O UEZVMMHDMIWARA-UHFFFAOYSA-M 0.000 description 1
- 239000001205 polyphosphate Substances 0.000 description 1
- 235000011176 polyphosphates Nutrition 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- GQJPVGNFTLBCIQ-UHFFFAOYSA-L sodium;zirconium(4+);carbonate Chemical compound [Na+].[Zr+4].[O-]C([O-])=O GQJPVGNFTLBCIQ-UHFFFAOYSA-L 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- ZQZCOBSUOFHDEE-UHFFFAOYSA-N tetrapropyl silicate Chemical compound CCCO[Si](OCCC)(OCCC)OCCC ZQZCOBSUOFHDEE-UHFFFAOYSA-N 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 150000003609 titanium compounds Chemical class 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 238000011179 visual inspection Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000003021 water soluble solvent Substances 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
- 150000003755 zirconium compounds Chemical class 0.000 description 1
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- 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
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- 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
- C23C22/42—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 containing also phosphates
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- C23C2/00—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
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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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- C23C22/07—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
- C23C22/08—Orthophosphates
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- 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
- C23C22/73—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 characterised by the process
- C23C22/77—Controlling or regulating of the coating process
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Abstract
Description
(1)亜鉛系めっき鋼板と、
該亜鉛系めっき鋼板上の第1皮膜と、該第1皮膜上の第2皮膜とを含む表面処理皮膜と、
を有する表面処理皮膜付き亜鉛系めっき鋼板であって、
前記第1皮膜は、炭酸ジルコニウム化合物(A)と、リン酸化合物(B)と、テトラアルコキシシラン(C)と、エポキシ基を有するシランカップリング剤(D)とを含有し、下記(I)の条件を満足するように調製された第1の表面処理液(X)を前記亜鉛系めっき鋼板の表面に塗布し、加熱乾燥して得たものであり、
前記第2皮膜は、炭酸ジルコニウム化合物(A)と、リン酸化合物(B)と、テトラアルコキシシラン(C)と、エポキシ基を有するシランカップリング剤(D)とを含有し、下記(II)の条件を満足するように調製された第2の表面処理液(Y)を前記第1皮膜の表面に塗布し、加熱乾燥して得たものであり、
前記第1および第2皮膜の合計付着量が、片面当たり0.2〜2.0g/m2であることを特徴とする表面処理皮膜付き亜鉛系めっき鋼板。
(I)前記第1の表面処理液(X)中の、前記リン酸化合物(B)のP換算の固形分質量(B1)と、前記炭酸ジルコニウム化合物(A)のZr換算の固形分質量(A1)との比(B1/A1)が0.30超え2.20以下
(II)前記第2の表面処理液(Y)中の、前記リン酸化合物(B)のP換算の固形分質量(B2)と、前記炭酸ジルコニウム化合物(A)のZr換算の固形分質量(A2)との比(B2/A2)が0.05超え0.46以下、かつ、前記(I)の固形分比(B1/A1)が0.30超え0.46以下の場合には、前記固形分比(B2/A2)が次式(a)を満足する。
(B1/A1)>(B2/A2) ・・・式(a)
(III)前記第1の表面処理液(X)に前記フッ素樹脂エマルション(H)を含む場合、該フッ素樹脂エマルション(H)の固形分質量と、前記第1の表面処理液(X)の全固形質量との比(H1/X1)が0.001〜0.100
(IV)前記第2の表面処理液(Y)に前記フッ素樹脂エマルション(H)を含む場合、該フッ素樹脂エマルション(H)の固形分質量と、前記第2の表面処理液(Y)の全固形質量との比(H2/Y2)が0.001〜0.100
上記(1)〜(4)のいずれか1項中の第2の表面処理液(Y)を前記第1皮膜の表面に塗布し、加熱乾燥して、前記第1皮膜の表面に第2皮膜を形成する工程と、
を有し、前記第1および第2皮膜からなる表面処理皮膜の合計付着量を、片面当たり0.2〜2.0g/m2とすることを特徴とする表面処理皮膜付き亜鉛系めっき鋼板の製造方法。
本発明において、ベースとなる亜鉛系めっき鋼板としては、そのめっき層中に亜鉛を含有する鋼板であればよく、特に制限はないが、溶融亜鉛めっき鋼板(GI)またはこれを合金化した合金化溶融亜鉛めっき鋼板(GA)、電気亜鉛めっき鋼板(EG)等の亜鉛めっき鋼板、Zn−Niめっき鋼板、Zn−Al−Mgめっき鋼板(例えばZn−6質量%Al−3質量%Mg合金めっき鋼板、Zn−11質量%Al−3質量%Mg合金めっき鋼板)、Zn−Alめっき鋼板(例えば、Zn−5質量%Al合金めっき鋼板、Zn−55質量%Al合金めっき鋼板)などを用いることが可能である。
本発明の表面処理皮膜付き亜鉛系めっき鋼板は、前記亜鉛系めっき鋼板と、該亜鉛系めっき鋼板の少なくとも片面に形成された表面処理皮膜とを有する。表面処理皮膜は、前記亜鉛系めっき鋼板上の第1皮膜と、該第1皮膜上の第2皮膜とを含む。第1皮膜は、後述の第1の表面処理液(X)を亜鉛系めっき鋼板の表面に塗布し、加熱乾燥して得たものである。第2皮膜は、後述の第2の表面処理液(Y)を前記第1皮膜の表面に塗布し、加熱乾燥して得たものである。
第1および第2の表面処理液(X,Y)は、炭酸ジルコニウム化合物(A)と、リン酸化合物(B)と、テトラアルコキシシラン(C)と、エポキシ基を有するシランカップリング剤(D)と、水とを含有し、さらに必要に応じて、ヒドロキシカルボン酸(E)、バナジン酸化合物(F)、ニッケル化合物(G)、およびフッ素樹脂エマルション(H)の少なくとも1つを含有させることもできる。
(B1/A1)>(B2/A2) ・・・式(a)
(B2/A2)が0.46を超えた場合、または、式(a)を満たさない場合には、表面処理皮膜を2層にした効果を得ることができず、すなわち、耐黒変性が低下し、耐黒変性の付着量依存性が大きくなる。(B2/A2)が0.05以下である場合は、リン酸化合物(B)が不足することによって第1皮膜との反応性が低下すること、およびZrが過剰となることによって、第1皮膜との密着性が劣りかつ皮膜が脆くなるため、厳しいプレス成形後の耐フレーク状めっき剥離性、平板部耐食性、プレス成形後の耐食性を十分に得ることができない。
本発明の表面処理皮膜付き亜鉛系めっき鋼板の製造方法は、上記第1の表面処理液(X)を亜鉛系めっき鋼板の表面に塗布し、加熱乾燥して、前記亜鉛系めっき鋼板の表面に第1皮膜を形成する工程と、上記第2の表面処理液(Y)を前記第1皮膜の表面に塗布し、加熱乾燥して、前記第1皮膜の表面に第2皮膜を形成する工程と、を有する。
表1に示す各種亜鉛系めっき鋼板を供試板として使用した。なお、亜鉛系めっき層は鋼板の両面に形成され、表1中の付着量は片面当たりの亜鉛めっき層の付着量を意味する。
上記の供試板の表面を、日本パーカライジング(株)製パルクリーンN364Sを用いて処理し、表面の油分や汚れを取り除いた。次に、水道水で水洗して供試板表面が水で100%濡れることを確認した後、さらに純水(脱イオン水)を流しかけ、100℃雰囲気のオーブンで水分を乾燥した。
各成分を表2に示す組成(固形分質量比)にて水中で混合し、第1の表面処理液(X)および第2の表面処理液(Y)を得た。これらの表面処理液は、調製後、すぐに試験に使用した。
A1:炭酸ジルコニウムナトリウム
A2:炭酸ジルコニウムアンモニウム
B1:リン酸(H3PO4)
B2:リン酸二水素アンモニウム(NH4(H2PO4))
B3:ジホスホン酸(C2H8P2O7)
C1:テトラメトキシシラン
C2:テトラエトキシシラン
D1:3−グリシドキシプロピルトリエトキシシラン
D2:3−グリシドキシプロピルトリメトキシシラン
E1:リンゴ酸
E2:酒石酸
E3:クエン酸
F1:メタバナジン酸ナトリウム(NaVO3)
F2:メタバナジン酸アンモニウム(NH4VO3)
G1:硝酸ニッケル六水和物(Ni(NO3)2・6H2O)
G2:硫酸ニッケル六水和物(NiSO4・6H2O)
フッ素化アルキル基含有アクリレートとアクリル酸アルキルエステル共重合体として、最低造膜温度(MFT)が以下のものを用いた。
H1:MFT 5℃
H2:MFT 14℃
H3:MFT 33℃
H4:MFT 55℃
表1に示す各鋼板(鋼板の番号を表2の「鋼板」欄に示す)に対して前処理を行った各種供試板に、表2の各種第1の表面処理液(X)をバーコーターで塗布し、その後、水洗することなく、そのままオーブンに入れて、表2の「PMT」欄に示す最高到達板温(PMT:Peak Metal Temperature)で乾燥させ、表2に示す付着量(片面あたり)の第1皮膜を両面に形成した。次いで、第1皮膜の表面に、表2の各種第2の表面処理液(Y)をバーコーターで塗布し、その後、水洗することなく、そのままオーブンに入れて、表2の「PMT」欄に示す最高到達板温で乾燥させ、表2に示す付着量(片面あたり)の第2皮膜を両面に形成した。
得られた表面処理皮膜付き亜鉛系めっき鋼板(以下、単に「サンプル」という。)に対して、以下の(5−1)〜(5−9)の評価を行った結果を、表2に併せて示す。
各サンプルに対して、プレスを行わず平板の状態で、JIS−Z−2371−2000に準拠する塩水噴霧試験(SST)を実施した。120時間後の白錆発生面積率で平板部耐食性を評価した。評価基準は以下のとおりである。
(評価基準)
◎ :白錆面積率5%未満
○ :白錆面積率5%以上10%未満
○−:白錆面積率10%以上25%未満
△ :白錆面積率25%以上50%未満
× :白錆面積率50%以上100%以下
表面処理皮膜の膜厚が均一な各サンプルについて、プレスを行わず平板の状態で、80℃,98%RH環境下24時間保持前後のサンプル表面の色差△L*(JIS−Z−8729−2004に規定するL*、a*、b*表示系におけるCIE1976明度L*の差)の測定と目視観察にて、耐黒変性を評価した。評価基準は以下のとおりである。
(評価基準)
◎ :−2.5<△L*≦1 かつ、ムラが無い均一な外観
○ :−3<△L*≦−2.5 かつ、ムラが無い均一な外観
○−:−3.5<△L*≦−3 かつ、ムラが無い均一な外観
△ :−4<△L*≦−3.5 かつ、ムラが無い均一な外観
× :△L*≦−4 または、外観ムラあり
各サンプルに対して、第1皮膜、第2皮膜ともに表2の付着量の1.2倍の第2サンプルを準備した。各サンプルと、各サンプルに対応する第2サンプルの両方について、平板の状態で、(5−2)に記載の色差△L*の測定を行った。以下の式から、Δ(△L*)を求め、耐黒変性の付着量依存性を評価した。
Δ(△L*)=(サンプルにおける△L*)−(第2サンプルにおける△L*)
(評価基準)
◎ :−0.5<Δ(△L*)≦1.0
○ :−1.0<Δ(△L*)≦−0.5
○−:−1.5<Δ(△L*)≦−1.0
△ :−2.0<Δ(△L*)≦−1.5
× :Δ(△L*)≦−2.0
各サンプルについて、プレスを行わず平板の状態で、サンプル表面に脱イオン水を300μl滴下し、炉内温度100℃の熱風オーブンに10分間投入し、オーブンから取り出した後の水滴滴下跡を目視観察して、耐水しみ性を評価した。評価基準は以下のとおりである。
(評価基準)
◎ :水滴境界が見る角度によらず確認されない
○ :水滴境界が見る角度によって若干確認される
○−:水滴境界が見る角度によらず若干確認される
△ :水滴境界が見る角度によらずはっきり確認される
× :水滴境界が滴下範囲を超えてはっきり確認される
各サンプルに速乾性のプレス油(日本工作油株式会社製:無洗浄プレス工作油G−6231F)を塗油した状態で、以下のプレス条件の多段絞り成形を行い、金型に付着する汚れを拭き取ることなく10サンプル連続で成形した後、10個目のサンプル表面に付着した黒ずみの程度を目視で観察し、耐黒ずみ性を評価した。評価基準は以下のとおりである。
(プレス条件)
成形速度450mm/秒、ブランク径φ90mm
1段目:ポンチ径Φ49mm、ポンチとダイスのクリアランス1.0mm
2段目:ポンチ径Φ39mm、ポンチとダイスのクリアランス0.8mm
3段目:ポンチ径Φ32mm、ポンチとダイスのクリアランス0.8mm
4段目:ポンチ径Φ27.5mm、ポンチとダイスのクリアランス0.8mm
5段目:ポンチ径Φ24.4mm、ポンチとダイスのクリアランス0.8mm
(評価基準)
◎ :プレス直後でも黒ずみがサンプル表面に付着していない。
○ :プレス直後は黒ずみがサンプル表面に面積率で5%以下付着しているが、時間とともに黒ずみが鋼板表面から流れてほとんど確認できなくなる。
○−:プレス直後に黒ずみがサンプル表面に面積率で5%以下付着しており、時間がたっても黒ずみが鋼板表面に残ったままである。
△ :黒ずみがサンプル表面に面積率で5%超、15%以下付着して、時間がたっても黒ずみが鋼板表面に残ったままである。
× :黒ずみがサンプル表面に面積率で15%超付着して、時間がたっても黒ずみが鋼板表面に残ったままである。
各サンプルに速乾性のプレス油(日本工作油株式会社製:無洗浄プレス工作油G−6231F)を塗油した状態で、以下の引き抜き条件で、金型に付着する汚れや剥離カスを拭き取ることなく同じ箇所を3回連続で平面引き抜きした後、サンプル表面に付着しためっき剥離カスの程度をルーペで拡大して目視観察し、耐めっき剥離性を評価した。評価基準は以下のとおりである。
(プレス条件)
ビード先端径0.5mm、押しつけ荷重200kgf、引き抜き速度16.7mm/秒、引き抜き距離100mm
(めっき剥離カスの評価基準)
◎ :めっき剥離カスが金属光沢を有さず、量が微量で細かい粒状である。
○ :めっき剥離カスが金属光沢を有さず、細かい粒状である。
○−:めっき剥離カスが金属光沢を有し、細かい粒状である。
△ :めっき剥離カスが金属光沢を有し、鱗片屑状である。
× :めっき剥離カスが金属光沢を有し、量が多くカンナ屑状である。
上記「(5−5)耐黒ずみ性」に示した多段絞り成形を行ったサンプルに対して、速乾性のプレス油が乾いた後、各サンプルについてJIS−Z−2371−2000に準拠する塩水噴霧試験を実施した。16時間後の白錆発生面積率で、連続高速プレス成形後耐食性を評価した。評価基準は以下のとおりである。
(評価基準)
◎ :白錆面積率5%未満
○ :白錆面積率5%以上10%未満
○−:白錆面積率10%以上25%未満
△ :白錆面積率25%以上50%未満
× :白錆面積率50%以上100%以下
電子式万能試験機(YONEKURA(株)製「CATY」)を用いて、各サンプルを延伸速度10mm/min、延伸率20%で延伸した。40℃での動粘度が51〜69mm2/s、100℃での動粘度が11.1〜14.9mm2/sの軸受け用油(NOKクリューバー(株)製「ALL TIME J 652」)を容器に入れ、鉛直に立てたサンプルの下端部を容器内の軸受け用油に浸した状態で85℃環境下3日間静置し、軸受け用油のしみ拡がり高さを測定した。評価基準は、以下のとおりである。
(評価基準)
◎ :滲み拡がり高さ0.5cm未満
○ :滲み拡がり高さ0.5cm以上1、5cm未満
○−:滲み拡がり高さ1.5cm以上3.0cm未満
△ :滲み拡がり高さ3.0cm以上4.5cm未満
× :滲み拡がり高さ4.5cm以上
電子式万能試験機(YONEKURA(株)製「CATY」)を用いて、各サンプルを延伸速度10mm/min、延伸率20%で延伸した。その後、各サンプルを85℃に加温した状態で、上記(5−8)に記載の軸受け用油を、サンプル表面に滴下し、滴下後85℃環境下3日間静置した。その後、各サンプルの接触角を固液界面解析装置(協和界面科学(株)製「Drop Master500」)により測定した。評価基準は、以下のとおりである。
(評価基準)
◎ :接触角40°以上
○ :接触角30°以上40°未満
○−:接触角20°以上30°未満
△ :接触角10°以上20°未満
× :接触角10°未満
表2に示すように、本発明例では、(5−5)連続高速プレス成形等の過酷なしごき加工を施した後の耐黒ずみ性、(5−6)連続高速プレス成形等の過酷なしごき加工を施した後の耐フレーク状めっき剥離性、(5−3)耐黒変性の付着量依存性がいずれも優れる表面処理皮膜付き亜鉛系めっき鋼板を得ることができた。これに対し、比較例では、上記(5−6)および(5−3)の少なくとも一方が優れなかった。
Claims (6)
- 亜鉛系めっき鋼板と、
該亜鉛系めっき鋼板上の第1皮膜と、該第1皮膜上の第2皮膜とを含む表面処理皮膜と、
を有する表面処理皮膜付き亜鉛系めっき鋼板であって、
前記第1皮膜は、炭酸ジルコニウム化合物(A)と、リン酸化合物(B)と、テトラアルコキシシラン(C)と、エポキシ基を有するシランカップリング剤(D)とを含有し、下記(I)の条件を満足するように調製された第1の表面処理液(X)を前記亜鉛系めっき鋼板の表面に塗布し、加熱乾燥して得たものであり、
前記第2皮膜は、炭酸ジルコニウム化合物(A)と、リン酸化合物(B)と、テトラアルコキシシラン(C)と、エポキシ基を有するシランカップリング剤(D)とを含有し、下記(II)の条件を満足するように調製された第2の表面処理液(Y)を前記第1皮膜の表面に塗布し、加熱乾燥して得たものであり、
前記第1および第2皮膜の合計付着量が、片面当たり0.2〜2.0g/m2であることを特徴とする表面処理皮膜付き亜鉛系めっき鋼板。
(I)前記第1の表面処理液(X)中の、前記リン酸化合物(B)のP換算の固形分質量(B1)と、前記炭酸ジルコニウム化合物(A)のZr換算の固形分質量(A1)との比(B1/A1)が0.30超え2.20以下
(II)前記第2の表面処理液(Y)中の、前記リン酸化合物(B)のP換算の固形分質量(B2)と、前記炭酸ジルコニウム化合物(A)のZr換算の固形分質量(A2)との比(B2/A2)が0.05超え0.46以下、かつ、前記(I)の固形分比(B1/A1)が0.30超え0.46以下の場合には、前記固形分比(B2/A2)が次式(a)を満足する。
(B1/A1)>(B2/A2) ・・・式(a) - 前記第1および第2の表面処理液(X,Y)の少なくとも一方において、前記リン酸化合物(B)が、無機リン酸化合物および有機リン酸化合物からなり、前記無機リン酸化合物のP換算の固形分質量(Bin)と、前記有機リン酸化合物のP換算の固形分質量(Bog)との比(Bin/Bog)が0.1〜1.5である請求項1に記載の表面処理皮膜付き亜鉛系めっき鋼板。
- 前記第1および第2の表面処理液(X,Y)の少なくとも一方が、ヒドロキシカルボン酸(E)、バナジン酸化合物(F)、およびニッケル化合物(G)の少なくとも1つを含有する請求項1または2に記載の表面処理皮膜付き亜鉛系めっき鋼板。
- 前記第1および第2の表面処理液(X,Y)の少なくとも一方にフッ素樹脂エマルション(H)を含有し、かつ下記(III)、(IV)、または、(III)および(IV)の条件を満たす請求項1〜3のいずれか1項に記載の表面処理皮膜付き亜鉛系めっき鋼板。
(III)前記第1の表面処理液(X)に前記フッ素樹脂エマルション(H)を含む場合、該フッ素樹脂エマルション(H)の固形分質量と、前記第1の表面処理液(X)の全固形質量との比(H1/X1)が0.001〜0.100
(IV)前記第2の表面処理液(Y)に前記フッ素樹脂エマルション(H)を含む場合、該フッ素樹脂エマルション(H)の固形分質量と、前記第2の表面処理液(Y)の全固形質量との比(H2/Y2)が0.001〜0.100 - 前記第1皮膜の付着量が片面当たり0.1〜1.5g/m2であり、前記第2皮膜の付着量が片面当たり0.1〜1.5g/m2である請求項1〜4のいずれか1項に記載の表面処理皮膜付き亜鉛系めっき鋼板。
- 請求項1〜4のいずれか1項中の第1の表面処理液(X)を亜鉛系めっき鋼板の表面に塗布し、加熱乾燥して、前記亜鉛系めっき鋼板の表面に第1皮膜を形成する工程と、
請求項1〜4のいずれか1項中の第2の表面処理液(Y)を前記第1皮膜の表面に塗布し、加熱乾燥して、前記第1皮膜の表面に第2皮膜を形成する工程と、
を有し、前記第1および第2皮膜からなる表面処理皮膜の合計付着量を、片面当たり0.2〜2.0g/m2とすることを特徴とする表面処理皮膜付き亜鉛系めっき鋼板の製造方法。
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WO2018070350A1 (ja) * | 2016-10-11 | 2018-04-19 | Jfeスチール株式会社 | 亜鉛系めっき鋼板用表面処理液、表面処理皮膜付き亜鉛系めっき鋼板の製造方法、及び表面処理皮膜付き亜鉛系めっき鋼板 |
CN117187900B (zh) * | 2023-11-03 | 2024-02-09 | 江苏省沙钢钢铁研究院有限公司 | 一种八宝粥罐用涂覆镀锡板及其制造方法 |
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JP2000248367A (ja) * | 1998-12-28 | 2000-09-12 | Nippon Steel Corp | 非クロム型処理亜鉛系めっき鋼板 |
JP2006009065A (ja) * | 2004-06-23 | 2006-01-12 | Jfe Steel Kk | 耐白錆性および塗装性に優れたリン酸塩複合被覆鋼板 |
JP5088095B2 (ja) | 2006-12-13 | 2012-12-05 | Jfeスチール株式会社 | 平板部耐食性、耐黒変性およびプレス成形後の外観と耐食性に優れた表面処理亜鉛系めっき鋼板、並びに亜鉛系めっき鋼板用水系表面処理液 |
JP5272563B2 (ja) | 2008-08-01 | 2013-08-28 | 新日鐵住金株式会社 | 亜鉛系めっき金属材料に適した表面処理液、亜鉛系めっき金属材料及び亜鉛系めっき鋼板の製造方法 |
US8906512B2 (en) * | 2008-10-08 | 2014-12-09 | Nippon Steel & Sumitomo Metal Corporation | Metal material having excellent corrosion resistance |
CN102257178B (zh) * | 2008-12-16 | 2014-05-07 | 日本帕卡濑精株式会社 | 金属材料用表面处理剂 |
JP5353342B2 (ja) | 2009-03-17 | 2013-11-27 | 新日鐵住金株式会社 | 表面処理亜鉛系めっき金属材料と表面処理液 |
JP5663915B2 (ja) * | 2009-03-31 | 2015-02-04 | Jfeスチール株式会社 | 亜鉛系めっき鋼板 |
WO2012165084A1 (ja) * | 2011-05-27 | 2012-12-06 | 関西ペイント株式会社 | 水性金属表面処理剤 |
JP5870570B2 (ja) * | 2011-09-14 | 2016-03-01 | Jfeスチール株式会社 | 亜鉛系めっき鋼板用の表面処理液ならびに亜鉛系めっき鋼板およびその製造方法 |
CN103059344B (zh) * | 2012-12-21 | 2014-01-08 | 淮阴师范学院 | 含硅磷的准球形胶囊状高效、协同、复合型阻燃剂 |
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