TW201807254A - 表面處理鋼材 - Google Patents
表面處理鋼材 Download PDFInfo
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- TW201807254A TW201807254A TW106109774A TW106109774A TW201807254A TW 201807254 A TW201807254 A TW 201807254A TW 106109774 A TW106109774 A TW 106109774A TW 106109774 A TW106109774 A TW 106109774A TW 201807254 A TW201807254 A TW 201807254A
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- mass
- coating film
- plating layer
- content
- steel material
- Prior art date
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- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 258
- 239000010959 steel Substances 0.000 title claims abstract description 258
- 238000000576 coating method Methods 0.000 claims abstract description 168
- 239000011248 coating agent Substances 0.000 claims abstract description 165
- 229920005989 resin Polymers 0.000 claims abstract description 68
- 239000011347 resin Substances 0.000 claims abstract description 68
- 150000003682 vanadium compounds Chemical class 0.000 claims abstract description 60
- GVALZJMUIHGIMD-UHFFFAOYSA-H magnesium phosphate Chemical compound [Mg+2].[Mg+2].[Mg+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O GVALZJMUIHGIMD-UHFFFAOYSA-H 0.000 claims abstract description 56
- 150000001875 compounds Chemical class 0.000 claims abstract description 52
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 45
- 239000008199 coating composition Substances 0.000 claims abstract description 44
- 238000007747 plating Methods 0.000 claims description 369
- 239000011777 magnesium Substances 0.000 claims description 138
- 239000000463 material Substances 0.000 claims description 85
- 229910007981 Si-Mg Inorganic materials 0.000 claims description 78
- 229910008316 Si—Mg Inorganic materials 0.000 claims description 78
- 239000000049 pigment Substances 0.000 claims description 47
- 229910045601 alloy Inorganic materials 0.000 claims description 38
- 239000000956 alloy Substances 0.000 claims description 38
- 239000011701 zinc Substances 0.000 claims description 36
- 229910001297 Zn alloy Inorganic materials 0.000 claims description 35
- 239000004137 magnesium phosphate Substances 0.000 claims description 35
- 229910000157 magnesium phosphate Inorganic materials 0.000 claims description 35
- 229960002261 magnesium phosphate Drugs 0.000 claims description 35
- 235000010994 magnesium phosphates Nutrition 0.000 claims description 35
- 239000005056 polyisocyanate Substances 0.000 claims description 28
- 229920001228 polyisocyanate Polymers 0.000 claims description 28
- -1 vanadate alkaline earth metal salts Chemical class 0.000 claims description 28
- FJMNNXLGOUYVHO-UHFFFAOYSA-N aluminum zinc Chemical compound [Al].[Zn] FJMNNXLGOUYVHO-UHFFFAOYSA-N 0.000 claims description 26
- 229910052749 magnesium Inorganic materials 0.000 claims description 26
- 229910052725 zinc Inorganic materials 0.000 claims description 26
- 239000007864 aqueous solution Substances 0.000 claims description 25
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- 239000000470 constituent Substances 0.000 claims description 23
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 20
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- 239000004645 polyester resin Substances 0.000 claims description 16
- 239000010936 titanium Substances 0.000 claims description 16
- 229910052804 chromium Inorganic materials 0.000 claims description 13
- 229910052710 silicon Inorganic materials 0.000 claims description 13
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 12
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- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 10
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims description 9
- 239000004606 Fillers/Extenders Substances 0.000 claims description 8
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- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 claims description 8
- 229910052796 boron Inorganic materials 0.000 claims description 7
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 5
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- 239000001257 hydrogen Substances 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 claims description 5
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- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 4
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- 239000000440 bentonite Substances 0.000 claims description 2
- 229910000278 bentonite Inorganic materials 0.000 claims description 2
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 2
- 238000005253 cladding Methods 0.000 claims description 2
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- 229910052720 vanadium Inorganic materials 0.000 claims description 2
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 claims description 2
- 125000005462 imide group Chemical group 0.000 claims 1
- 239000010703 silicon Substances 0.000 claims 1
- 238000005260 corrosion Methods 0.000 abstract description 95
- 230000007797 corrosion Effects 0.000 abstract description 94
- 238000011282 treatment Methods 0.000 abstract description 56
- 239000007787 solid Substances 0.000 abstract description 34
- ZCDOYSPFYFSLEW-UHFFFAOYSA-N chromate(2-) Chemical compound [O-][Cr]([O-])(=O)=O ZCDOYSPFYFSLEW-UHFFFAOYSA-N 0.000 abstract description 16
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- 239000007789 gas Substances 0.000 description 27
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- 238000012360 testing method Methods 0.000 description 26
- DNWNZRZGKVWORZ-UHFFFAOYSA-N calcium oxido(dioxo)vanadium Chemical compound [Ca+2].[O-][V](=O)=O.[O-][V](=O)=O DNWNZRZGKVWORZ-UHFFFAOYSA-N 0.000 description 25
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 25
- 238000010438 heat treatment Methods 0.000 description 23
- 238000012545 processing Methods 0.000 description 23
- 230000037303 wrinkles Effects 0.000 description 23
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 description 20
- 239000000126 substance Substances 0.000 description 19
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- 238000006243 chemical reaction Methods 0.000 description 18
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- 230000002829 reductive effect Effects 0.000 description 17
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 16
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical group OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 15
- 238000005452 bending Methods 0.000 description 15
- 230000000694 effects Effects 0.000 description 15
- 238000011156 evaluation Methods 0.000 description 14
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 13
- 239000000047 product Substances 0.000 description 13
- 239000007921 spray Substances 0.000 description 13
- 229920000877 Melamine resin Polymers 0.000 description 12
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- 238000000137 annealing Methods 0.000 description 12
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- 230000003449 preventive effect Effects 0.000 description 10
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 9
- 230000006872 improvement Effects 0.000 description 9
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 8
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- 238000005096 rolling process Methods 0.000 description 8
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- 230000008023 solidification Effects 0.000 description 8
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- 125000000524 functional group Chemical group 0.000 description 7
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 6
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- 239000011888 foil Substances 0.000 description 6
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- 229940043430 calcium compound Drugs 0.000 description 5
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- UPMLOUAZCHDJJD-UHFFFAOYSA-N 4,4'-Diphenylmethane Diisocyanate Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=C(N=C=O)C=C1 UPMLOUAZCHDJJD-UHFFFAOYSA-N 0.000 description 4
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- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 description 4
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- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 description 3
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- 238000002474 experimental method Methods 0.000 description 3
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- NIMLQBUJDJZYEJ-UHFFFAOYSA-N isophorone diisocyanate Chemical compound CC1(C)CC(N=C=O)CC(C)(CN=C=O)C1 NIMLQBUJDJZYEJ-UHFFFAOYSA-N 0.000 description 3
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- 239000006096 absorbing agent Substances 0.000 description 2
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- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical group C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 2
- 239000004566 building material Substances 0.000 description 2
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- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
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- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- JCGNDDUYTRNOFT-UHFFFAOYSA-N oxolane-2,4-dione Chemical compound O=C1COC(=O)C1 JCGNDDUYTRNOFT-UHFFFAOYSA-N 0.000 description 1
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- 239000002244 precipitate Substances 0.000 description 1
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- 230000001737 promoting effect Effects 0.000 description 1
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- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 1
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- 238000010301 surface-oxidation reaction Methods 0.000 description 1
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- 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
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 238000002076 thermal analysis method Methods 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- 239000012974 tin catalyst Substances 0.000 description 1
- 150000003606 tin compounds Chemical class 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- TWQULNDIKKJZPH-UHFFFAOYSA-K trilithium;phosphate Chemical compound [Li+].[Li+].[Li+].[O-]P([O-])([O-])=O TWQULNDIKKJZPH-UHFFFAOYSA-K 0.000 description 1
- UNXRWKVEANCORM-UHFFFAOYSA-I triphosphate(5-) Chemical compound [O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O UNXRWKVEANCORM-UHFFFAOYSA-I 0.000 description 1
- UNXRWKVEANCORM-UHFFFAOYSA-N triphosphoric acid Chemical compound OP(O)(=O)OP(O)(=O)OP(O)(O)=O UNXRWKVEANCORM-UHFFFAOYSA-N 0.000 description 1
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 1
- 150000003673 urethanes Chemical class 0.000 description 1
- WQEVDHBJGNOKKO-UHFFFAOYSA-K vanadic acid Chemical class O[V](O)(O)=O WQEVDHBJGNOKKO-UHFFFAOYSA-K 0.000 description 1
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- 239000000080 wetting agent Substances 0.000 description 1
- 150000003739 xylenols Chemical class 0.000 description 1
- XAEWLETZEZXLHR-UHFFFAOYSA-N zinc;dioxido(dioxo)molybdenum Chemical compound [Zn+2].[O-][Mo]([O-])(=O)=O XAEWLETZEZXLHR-UHFFFAOYSA-N 0.000 description 1
Classifications
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
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- C22C18/04—Alloys based on zinc with aluminium as the next major constituent
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Abstract
本發明之課題係提供一種不使用六價鉻而具備與鉻酸鹽處理為同等級以上的端部耐蝕性之表面處理鋼材。
一種在鋼材的表面上以隔著鍍敷層來形成塗膜而成之表面處理鋼材,且鍍敷層係藉由將鋼材浸漬於包含Mg的鋁鋅(galvalume)浴中而得到。其特徵如下:塗膜係使用含有塗膜形成性樹脂、交聯劑、指定的釩化合物、與第三磷酸鎂之塗料組成物所形成,釩化合物係滿足指定的導電率之化合物,且相對於塗膜形成性樹脂的固形分及交聯劑的固形分的合計100質量%,釩化合物的含量被限制在指定量,釩化合物係滿足指定的pH,相對於塗膜形成性樹脂的固形分及交聯劑的固形分的合計100質量%,第三磷酸鎂的含量為指定量。
Description
本發明係關於熔融鍍敷鋼板之非鉻酸鹽(chromate-free)之技術。
以往,在建材、汽車用的材料、家電製品用的材料等的用途中,熔融Zn-Al系鍍敷鋼材被廣泛地利用。其中55%鋁‧鋅合金鍍敷鋼板所代表之高鋁(25~75質量%)‧鋅合金鍍敷鋼板,與通常的熔融鋅鍍敷鋼板相較時,由於耐蝕性為優異因而需求繼續擴大。又,近年來特別是對於建材提出了進一步提升耐蝕性或加工性之要求,藉由對鍍敷層中添加Mg等的而謀求熔融Zn-Al系鍍敷鋼材之耐蝕性等的提升(參考例如專利文獻1)。
但,含有Mg之高鋁‧鋅合金鍍敷鋼板中,在鍍敷層的表面容易產生皺褶,因此,表面外觀之惡化將成為問題。進而因為該皺褶而在鍍敷層的表面產生陡峭的隆起,因而在對於鍍敷層施予化學轉化處理(chemical conversion treatment)而形成化學轉化處理層、或施予塗裝等而形成被覆層時,前述化學轉化處理層或被覆層的厚度容易變得不均勻。因此,存在著無法藉由塗裝等來使鍍
敷鋼板之耐蝕性之提升充分發揮之類的問題。
為了解決上述問題,專利文獻2係揭示著一種在鋼材的表面上鍍敷鋁‧鋅合金鍍敷層而成之熔融鍍敷鋼材,其特徵如下:前述鋁‧鋅合金鍍敷層係包含作為構成元素之Al、Zn、Si及Mg,且Mg含量為0.1~10質量%,前述鋁‧鋅合金鍍敷層係包含0.2~15體積%的Si-Mg相,相對於Mg全量,前述Si-Mg相中之Mg之質量比率為3%以上,前述鋁‧鋅合金鍍敷層係進而包含作為構成元素之0.02~1.0質量%的Cr。
鍍敷鋼板若長期間被使用時,因為表面之氧化致使鏽產生,因而美觀將變差,故在鍍敷鋼板的表面通常會施予防鏽處理。以往,作為防鏽處理,以使用優異的防腐蝕劑之鉻酸鹽之鉻酸鹽處理(chromat treatment)為一般的。然而,鉻酸鹽處理液中所包含之六價鉻,對於環境有造成不良影響之疑慮,故其使用日益被受限制。因此,至今提案著各種含有釩酸金屬鹽等的釩化合物之塗料。
例如專利文獻3及4中揭示著,作為防鏽顏料,係使用組合釋出磷酸離子之化合物與釋出釩酸離子之化合物之防鏽顏料。但,使用未含有該六價鉻的防鏽顏料所形成之塗膜,存在著對於室外機等的屋外用途之適用時耐蝕性不足等的問題。
又,專利文獻5及6中揭示著,將含有由(1)釩化合物、(2)金屬矽酸鹽等、及(3)磷酸系金
屬鹽所成之防鏽顏料之防鏽塗料組成物來作為防鏽顏料。然而,即使是該等的防鏽塗料組成物,亦與專利文獻1及2中所揭示之防鏽塗料為相同地,存在著對於屋外用途之適用時耐蝕性為不足,故仍有改善之空間。
作為使防鏽塗料組成物之耐蝕性提升之手段,增加防鏽顏料之釩化合物的含量為有效。然而,因為釩化合物,特別是釩酸的1價或2價的陽離子鹽之水溶性高,若大量含有時,塗膜會變得容易吸濕。其結果塗膜之耐濕性會降低,而存在著塗膜中產生膨脹(blister)之類的問題。如此般的塗膜之膨脹也是耐蝕性降低之原因。
此外,例如專利文獻7中提案著兼具耐蝕性與耐濕性的未含有六價鉻之防鏽塗料組成物,並揭示著一種塗料組成物,其係含有塗料形成樹脂(a)、交聯劑(b)及釩酸鈣(c),且釩酸鈣(c)的1質量%水溶液的導電率為200~2,000μS/cm,相對於前述塗料形成樹脂(a)及交聯劑(b)的合計固形分100質量%,釩酸鈣(c)的含量為50~150質量%。
又,例如專利文獻8中揭示著一種塗料組成物,其係含有塗膜形成性樹脂(a)、交聯劑(b)、選自由五氧化釩及釩酸鹼土金屬鹽所成之群之至少1種的釩化合物(c)、與防鏽促進劑(d),前述釩化合物(c)係1質量%水溶液在溫度25℃下的導電率為200μS/cm~2,000μS/cm的化合物,且相對於前述塗膜形成性樹脂(a)的固形分及前述交聯劑(b)的固形分的合計
100質量%,前述釩化合物(c)的合計含量為5~150質量%,前述防鏽促進劑(d)係選自由水溶性化合物(d-1)及螯合物形成化合物(d-2)所成之群之至少1種以上的化合物,相對於前述塗膜形成性樹脂(a)的固形分及交聯劑(b)的固形分的合計100質量%,前述防鏽促進劑(d)的合計含量為1~150質量%,前述水溶性化合物(d-1)係1質量%水溶液在溫度25℃下的導電率為超過2,000μS/cm且在15,000μS/cm以下的化合物,且前述水溶性化合物(d-1)係選自由鹼土金屬的氫氧化物、釩酸化合物、及鈰化合物所成之群之至少1種以上的化合物,前述螯合物形成化合物(d-2)係具有多個配位部位、且該等的配位部位被配位於1個金屬離子的化合物,進而提案著具有長期間的優異的耐蝕性、及耐濕性、且短期耐蝕性試驗為顯示良好結果之上述塗料組成物。
進而,例如專利文獻9中揭示著一種塗料組成物,其係含有(A)含羥基之塗膜形成性樹脂、(B)交聯劑及(C)防鏽顏料混合物,該防鏽顏料混合物(C)係由(1)選自由五氧化釩、釩酸鈣、釩酸鎂及偏釩酸銨所成之群之至少1種的釩化合物、(2)至少含有鎂之選自由磷酸、亞磷酸及三聚磷酸所成之群之至少1種的酸的鹽之磷酸系金屬鹽、(3)鎂離子交換二氧化矽所形成,相關於該樹脂(A)及該交聯劑(B)的固形分總量,該釩化合物(1)的量為3~50質量%,該磷酸系金屬鹽(2)的量為1~50質量%、及該鎂離子交換二氧化矽
(3)的量為1~150質量%,且該防鏽顏料混合物(C)的量為10~150質量%。
專利文獻10中揭示著一種熔融鍍敷鋼材,其係在鋼材的表面上鍍敷鋁‧鋅合金鍍敷層所成之熔融鍍敷鋼材,其特徵如下:前述鋁‧鋅合金鍍敷層係包含作為構成元素之Al、Zn、Si及Mg,且Mg含量為0.1~10質量%,前述鋁‧鋅合金鍍敷層係包含0.2~15體積%的Si-Mg相,相對於Mg全量,前述Si-Mg相中之Mg之質量比率為3%以上,前述鋁‧鋅合金鍍敷層係進而包含作為構成元素之0.02~1.0質量%的Cr。
近年,認為因為是「酸性雨」而致使塗裝鋼板的塗膜產生腐蝕之現象。於此,所謂「酸性雨」係指來源自二氧化硫(SO2)或氮氧化物(NOx)等的酸性雨起因物質,由於溶入雨‧雪‧霧等中而導致大氣與平常相比為酸性化之現象、或環境與平常相比為酸性化之現象。又,從酸性雨起因物質釋出作為酸性雨而降下至地面為止,亦有跨越國境被移動數百甚至數千公里之情形,故可預測塗裝鋼板的腐蝕損害會橫跨廣大範圍,且今後亦將會增加。又,因為酸性雨起因物質在結露及具有濕氣的環境下會被水膜吸收,故有環境被氧化而產生腐蝕進行之情形。
特別是,近年在鍍敷鋼板上預先施予塗裝處理的預塗鋼板(precoated steel sheet)為增加,從切斷時所形成的切斷端部產生腐蝕的端部腐蝕(亦即,端部耐蝕
性)之問題將會變大。
[專利文獻1]日本特開平11-279735號公報
[專利文獻2]日本專利第5118782號
[專利文獻3]日本特公平5-50444號公報
[專利文獻4]日本專利第3461741號公報
[專利文獻5]日本專利第4323530號公報
[專利文獻6]日本特開2009-227748號公報
[專利文獻7]日本特開2011-184624號公報
[專利文獻8]日本特開2013-067699號公報
[專利文獻9]國際公開第2012/086494號
[專利文獻10]日本專利第5857156號
以往的非鉻酸鹽之開發中,雖已嘗試達到接近於鉻酸鹽處理之耐蝕性,卻無法得到與鉻酸鹽處理為同等級的耐蝕性。特別是,關於上述之端部耐蝕性,相較於鉻酸鹽處理為顯著不佳,故要求改善。
在此,本案發明之目的係提供一種不使用六價鉻而具備與鉻酸鹽處理為同等級以上的端部耐蝕性之表面處理鋼材。
為解決上述課題,本案發明相關的表面處理鋼材,其係在鋼材的表面上以隔著至少包含鋁‧鋅合金鍍敷層的底層來形成塗膜,其特徵在於:前述鋁‧鋅合金鍍敷層係包含作為構成元素之Al、Zn、Si、Cr及Mg,且Mg含量為0.1~10質量%、Cr含量為0.02~1.0質量%,前述鋁‧鋅合金鍍敷層係包含0.2~15體積%的Si-Mg相,相對於Mg全量,前述Si-Mg相中之Mg之質量比率為3%以上,前述塗膜係含有塗膜形成性樹脂(a)、交聯劑(b)、選自由釩酸鹼土金屬鹽及釩酸鎂所成之群之至少1種的釩化合物(c)、與第三磷酸鎂(d),前述釩化合物(c)係1質量%水溶液在溫度25℃下的導電率為200μS/cm~2,000μS/cm的化合物,且相對於前述塗膜形成性樹脂(a)及前述交聯劑(b)的合計100質量%,前述釩化合物(c)的含量為超過50質量%且在150質量%以下,前述釩化合物(c)係其1質量%水溶液的pH為6.5~11,相對於前述塗膜形成性樹脂(a)及前述交聯劑(b)的合計100質量%,前述第三磷酸鎂(d)的含量為3~150質量%。
依據本案發明,可提供一種不使用六價鉻而具備與鉻酸鹽處理為同等級以上的端部耐蝕性之表面處理
鋼材。
1(1a)‧‧‧鋼板
2‧‧‧熔融鍍敷浴
3‧‧‧退捲機
4‧‧‧加熱爐
5‧‧‧退火‧冷卻部
6‧‧‧爐鼻
7‧‧‧瓶
8‧‧‧沉浸輥
9‧‧‧噴射噴嘴
10‧‧‧冷卻裝置
101‧‧‧一次冷卻裝置
102‧‧‧二次冷卻裝置
11‧‧‧調質軋延‧形狀矯正裝置
12‧‧‧捲揚機
13‧‧‧線圈
14‧‧‧線圈
15‧‧‧運送輥
16‧‧‧退捲機
17‧‧‧捲揚機
18‧‧‧加熱爐
19‧‧‧線圈
20‧‧‧保溫容器
21‧‧‧運送輥
22‧‧‧中空的構件
[圖1]係表示熔融鍍敷處理裝置之一例之概略圖。
[圖2]係表示熔融鍍敷處理裝置之其他例之一部分之概略圖。
[圖3]係表示過時效處理所使用之加熱裝置保溫容器之例之概略圖。
[圖4]係表示本發明中作為釩化合物(c)之由0.7質量%的釩酸鈣與0.3質量%的第三磷酸鎂(d)所成的水溶液、與作為釩化合物(c)之1.0質量%的釩酸鈣的水溶液,在酸性區域中之pH緩衝能力之圖。
本實施形態之表面處理鋼材係在鋼材的表面上形成至少包含鋁‧鋅合金鍍敷層(以下,簡稱為「鍍敷層」)之底層,作為上層係使用塗料組成物來形成塗膜。作為鋼材,可舉出薄鋼板、厚鋼板、型鋼、鋼管、鋼線等的各種之構件。即,鋼材的形狀並無特別限制。又,本實施形態中,在鍍敷層與該鍍敷層之上,藉由與施予非鉻酸鹽化學轉化處理之化學轉化處理層來構成底層。關於該化學轉化處理層未特別限定內容。
鍍敷層係藉由熔融鍍敷處理所形成,作為構成元素包含Al、Zn、Si、Cr及Mg。將鍍敷層的全體設為100質量%時,Mg的含量為0.1~10質量%。因此,藉由Al特別是鍍敷層的表面的耐蝕性會提升,同時,藉由因Zn之犠牲防蝕作用,特別使表面處理鋼材的切斷端面之邊緣潛變(edge creep)會受到抑制,從而可提高表面處理鋼材的耐蝕性。更,藉由Si,鍍敷層中之Al與鋼材之間的過度合金化會受到抑制,在鍍敷層與鋼材之間所隔著的合金層(後述)可抑制表面處理鋼材的加工性之損害。進而,鍍敷層藉由適度地含有比Zn更為卑金屬的Mg,從而鍍敷層的犠牲防蝕作用將為強化,且表面處理鋼材之耐蝕性將進而提升。
將鍍敷層的全體設為100體積%時,鍍敷層中包含0.2~15體積%的Si-Mg相。Si-Mg相係以Si與Mg之金屬間化合物所構成之相,分散存在於鍍敷層中。鍍敷層中之Si-Mg相之體積比例越高,則越可抑制鍍敷層中之皺褶之產生。此係認為是,於表面處理鋼材之製造時在熔融鍍敷金屬冷卻並凝固而形成鍍敷層之程序中,於熔融鍍敷金屬完全地凝固前Si-Mg相在熔融鍍敷金屬中析出,該Si-Mg相抑制了熔融鍍敷金屬之流動之緣故。
將鍍敷層的全體設為100體積%時,Si-Mg相之體積比例為0.2~15體積%,較佳為0.2~10體積%,又較佳為0.4~5體積%。
鍍敷層中之Si-Mg相之體積比例,係與將鍍
敷層沿著其厚度方向切斷時之切斷面中之Si-Mg相的面積比例為相等。鍍敷層的切斷面中之Si-Mg相係可藉由電子顯微鏡觀察而清晰地確認。因此,藉由測定切斷面中之Si-Mg相的面積比例,從而可間接地測定鍍敷層中之Si-Mg相之體積比例。
鍍敷層係由Si-Mg相、與除此以外的含有Zn與Al的相所構成。含有Zn與Al的相,主要是由α-Al相(樹枝狀結晶組織)及Zn-Al-Mg共晶相(樹枝狀結晶間組織)所構成。含有Zn與Al的相係可因應鍍敷層的組成,進而能夠包含由Mg-Zn2所構成之相(Mg-Zn2相)、由Si所構成之相(Si相)、由Fe-Al金屬間化合物所構成之相(Fe-Al相)等各種的相。因此,鍍敷層中,含有Zn與Al的相之體積比例為99.8~85體積%,較佳為99.8~90體積%,又較佳為99.6~95體積%。
相對於鍍敷層中之Mg全量,Si-Mg相中之Mg之質量比率為3質量%以上。未包含在Si-Mg相中的Mg,係被包含在含有Zn與Al的相中。在含有Zn與Al的相中,Mg係被包含在α-Al相中、Zn-Al-Mg共晶相中、Mg-Zn2相中、鍍敷表面所形成之含有Mg之氧化物皮膜中等。Mg被包含在α-Al相中之情形時,Mg固溶在α-Al相中。
相對於鍍敷層中之Mg全量,Si-Mg相中之Mg之質量比率,係依據將Si-Mg相視為具有Mg2Si之化學計量組成而可算出。尚,實際上Si-Mg相可能含有除了
Si及Mg以外的Al、Zn、Cr、Fe等的元素,Si-Mg相中之Si與Mg的組成比亦可能在化學計量組成上稍有變動,但考慮該等而嚴格地決定Si-Mg相中之Mg量是非常困難的。因此,本發明中,在決定相對於鍍敷層中之Mg全量,Si-Mg相中之Mg之質量比率時,如同前述般,Si-Mg相係被視為具有Mg2Si的化學計量組成。
相對於鍍敷層中之Mg全量,Si-Mg相中之Mg之質量比率係藉由以下之式(1)而可算出。
R=A/(M×CMG/100)×100…(1)
R係表示相對於鍍敷層中之Mg全量,Si-Mg相中之Mg之質量比率(質量%)。A係表示鍍敷層的俯視圖中每單位面積的鍍敷層中之Si-Mg相中所包含之Mg含量(g/m2)。M係表示鍍敷層的俯視圖中之每單位面積的鍍敷層的質量(g/m2)。CMG係表示鍍敷層中之全Mg的含量(質量%)。
A係由以下之式(2)而可算出。
A=V2×ρ2×α…(2)
V2係表示鍍敷層的俯視圖中之每單位面積的鍍敷層中之Si-Mg相之體積(m3/m2)。ρ2係表示Si-Mg相之密度,其值為1.94×106(g/m3)。α係表示Si-Mg相中之Mg之含有質量比率,其值為0.63。
V2係由以下之式(3)而可算出。
V2=V1×R2/100…(3)
V1係表示鍍敷層的俯視圖中之每單位面積的鍍敷層之全體體積(m3/m2)。R2係表示鍍敷層中之Si-Mg相之體積比率(體積%)。
V1係由以下之式(4)而可算出。
V1=M/ρ1…(4)
ρ1係表示鍍敷層全體之密度(g/m3)。ρ1的值係以鍍敷層的組成為基礎,藉由將鍍敷層的構成元素在常溫下的密度進行加權平均而可算出。
本實施形態中,鍍敷層中之Mg,如上述般係以高的比率來被包含在Si-Mg相中。因此,在鍍敷層的表層中存在的Mg量將變少,據此可抑制鍍敷層的表層中之Mg系氧化皮膜的形成。因此,起因於Mg系氧化皮膜之鍍敷層的皺褶將受到抑制。相對於Mg全量,Si-Mg相中之Mg的比例越多,則越可抑制皺褶的產生。該比例係以5質量%以上為又較佳,以20質量%以上為更佳,以50質量%以上為特佳。Si-Mg相中之Mg,相對於Mg全量之比例的上限並無特別限制,該比例亦可為100質量%。
在鍍敷層中之50nm深度的最外層內,大小為直徑4mm、深度50nm的任意區域中,Mg含量較佳為未滿60質量%。該鍍敷層的最外層中之Mg含量,係可藉由輝光放電光譜分析(GD-OES:Glow Discharge-Optical
Emission Spectroscopy)來進行測定。難以得到精度為良好的定量濃度分析值之情形時,藉由比較鍍敷層中所包含多種的各元素的濃度曲線,只要未在鍍敷層的最外層確認到單獨MgO的氧化皮膜即可。
在鍍敷層的最外層中的Mg含量越少,越可抑制起因於Mg系氧化皮膜之皺褶。該Mg含量係以未滿40質量為又較佳,以未滿20質量%為更佳,以未滿10質量%為特佳。特別是在鍍敷層的厚度50nm的最外層內,以Mg含量為60質量%以上的部分為不存在為較佳,進而以Mg含量為40質量%以上的部分為不存在為較佳,以Mg含量為20質量%以上的部分為不存在為更佳。
對於Mg含量的物理性意義來進行說明。化學計量組成的MgO氧化物中之Mg含量係約60質量%。即,所謂Mg含量未滿60質量%,係指化學計量組成的MgO(單獨MgO的氧化皮膜)並不存在於鍍敷層的最外層、或該化學計量組成的MgO的形成受到明顯地抑制之意。本實施形態中,藉由抑制鍍敷層的最外層中之Mg的過量的氧化,可抑制單獨MgO的氧化皮膜的形成。在鍍敷層的最外層中,形成含有少量或大量Al、Zn、Sr等的除了Mg以外的元素的氧化物之複合氧化物,因此,可認為是鍍敷層的表層中之Mg的含量將相對地降低。
在鍍敷層表面中的Si-Mg相的面積比率係以30%以下為較佳。若在鍍敷層中存在Si-Mg相時,則在鍍敷層的表面Si-Mg相容易形成薄薄的網絡狀,若該Si-Mg
相的面積比率越大時,則鍍敷層的外觀會發生變化。Si-Mg相在鍍敷表面分布狀態為不均勻之情形時,藉由目視對於鍍敷層的外觀可觀察到光澤的不均勻。該光澤的不均勻係被稱為垂流之外觀不良。若在鍍敷層表面中的Si-Mg相的面積比率為30%以下時,則垂流會受到抑制,鍍敷層的外觀將為提升。進而,Si-Mg相在鍍敷層的表面較少,對於長期維持鍍敷層的耐蝕性也是有效地。若抑制Si-Mg相在對鍍敷層的表面的析出時,則Si-Mg相在對鍍敷層內部的析出量將會相對地增大。因此,鍍敷層內部的Mg量越多,據此在鍍敷層中將可長期發揮Mg的犠牲防蝕作用,從而據此將可長期維持鍍敷層的高耐蝕性。為了鍍敷層之外觀提升及鍍敷層的耐蝕性之維持,在鍍敷層表面中的Si-Mg相的面積比率係以20%以下為又較佳,以10%以下為更佳,以5%以下為特佳。
鍍敷層中之Mg的含量係如上述般為0.1~10質量%的範圍。若Mg的含量未滿0.1質量%時,則不能充分地確保鍍敷層的耐蝕性。若該含量多於10質量%時,則不僅是耐蝕性會降低、且於鍍敷鋼材之製造時,在熔融鍍敷浴中亦容易產生浮渣。該Mg的含量係進而以0.5質量%以上為較佳,進以1.0質量%以上為較佳。又,該Mg的含量係特別以5.0質量%以下為較佳,進而以3.0質量%以下為較佳。Mg的含量係以1.0~3.0質量%的範圍為特佳。
鍍敷層中之Al的含量係以25~75質量%的範
圍為較佳。若該含量為25質量%以上時,則鍍敷層中之Zn含量不會變得過量,可充分確保鍍敷層表面中之耐蝕性。若該含量為75質量%以下時,可充分發揮藉由Zn之犠牲防蝕效果,同時,鍍敷層的硬質化會受到抑制,從而表面處理鋼材的彎曲加工性將變高。進而,於鍍敷鋼材之製造時,從藉由使熔融鍍敷金屬的流動性不會過度地降低,而進一步抑制鍍敷層的皺褶之觀點而言,Al的含量係以75質量%以下為較佳。該Al的含量係特別以45質量%以上為較佳。又,該Al的含量係特別以65質量%以下為較佳。Al的含量係以45~65質量%的範圍為特佳。
鍍敷層中之Si的含量,相對於Al的含量以0.5~10質量%的範圍為較佳。Si相對於Al的含量若為0.5質量%以上時,則可充分地抑制鍍敷層中之Al與鋼材之過度的合金化。若該含量多於10質量%時,則不僅是藉由Si之作用會達到飽和,且於鍍敷鋼材之製造時,在熔融鍍敷浴中亦容易產生浮渣。該Si的含量係特別以1.0質量%以上為較佳。又,該Si的含量係特別以5.0質量%以下為較佳。Si的含量係以1.0~5.0質量%的範圍為特佳。
進而,鍍敷層中之Si:Mg的質量比以100:50~100:300的範圍為較佳。此情形時,特別促進鍍敷層中之Si-Mg層的形成,從而可進一步抑制鍍敷層中之皺褶的產生。該Si:Mg的質量比係進而以100:70~100:250為較佳,進而以100:100~100:200為較佳。
如同上述般,鍍敷層係含有Cr來作為構成元
素。此情形時,因Cr而可促進鍍敷層中之Si-Mg相的成長,鍍敷層中之Si-Mg相之體積比例會變高,同時,相對於鍍敷層中之Mg全量,Si-Mg相中之Mg的比例將會變高。據此,鍍敷層的皺褶會受到進一步的抑制。鍍敷層中的Cr的含量係0.02~1.0質量%的範圍。若鍍敷層中之Cr含量為未滿0.02%時,難以充分地確保鍍敷層的耐蝕性,同時,將難以充分地抑制鍍敷層的皺褶或垂流。若鍍敷層中的Cr的含量多於1.0質量%時,不僅是前述作用會達到飽和,且於鍍敷鋼材之製造時,在熔融鍍敷浴中亦容易產生浮渣,故塗裝後的塗膜平滑性將為降低。該Cr的含量係以0.05質量%以上為較佳。又,該Cr的含量係以0.5質量%以下為較佳。該Cr的含量係特別以0.07~0.2質量%的範圍為較佳。
在鍍敷層中之50nm深度的最外層內的Cr的含量係以100~500質量ppm為較佳。此情形時,鍍敷層的耐蝕性為進一步提升。此係認為是,因為若在最外層存在Cr時,則在鍍敷層會形成鈍態皮膜,因此,可抑制鍍敷層的陽極溶解之緣故。該Cr的含量係進而以150~450質量ppm為較佳,進而以200~400質量ppm為較佳。
鍍敷層與鋼材之間,以隔著含Al與Cr之合金層為較佳。本發明中,合金層係被視為與鍍敷層為不相同的層。合金層除了Al與Cr以外,亦可含有Mn、Fe、Co、Ni、Cu、Zn、Sn等的各種的金屬元素來作為構成元素。若存在如此般的合金層時,則藉由合金層中之Cr,
而可促進鍍敷層中之Si-Mg相的成長,鍍敷層中之Si-Mg相之體積比例會變高,同時,相對於鍍敷層中之Mg全量,Si-Mg相中之Mg的比例將變高。據此,鍍敷層的皺褶或垂流會受到進一步的抑制。特別是,相對於鍍敷層內的Cr的含有比例(質量比例),合金層中的Cr的含有比例(質量比例)之比以2~50的範圍為較佳。此情形時,因為會促進Si-Mg相在鍍敷層內的合金層附近之成長,故在鍍敷層的表面的Si-Mg相的面積比率會變低,因此,垂流會受到進一步抑制,同時,可進一步長期維持鍍敷層的耐蝕性。相對於鍍敷層內的Cr的含有比例,合金層中的Cr的含有比例之比係進而以3~40為較佳,進而以4~25為較佳。合金層中之Cr量係可藉由使用能量分散型X線分析裝置(EDS)測定鍍敷層的截面而導出。
合金層的厚度係以0.05~5μm的範圍為較佳。若該厚度為0.05μm以上時,可有效地發揮藉由合金層之上述作用。若該厚度為5μm以下時,則不易因合金層而損害表面處理鋼材之加工性。
若鍍敷層含有Cr時,則鍍敷層的彎曲加工變形後的耐蝕性亦會提升。其理由係可認為如下述般。若鍍敷層受到嚴格彎曲加工變形時,在鍍敷層及鍍敷層上的塗膜將有產生裂隙之情形。此時,水或氧通過裂隙而浸入鍍敷層內,鍍敷層內的合金直接暴露在腐蝕因子下。但,存在於鍍敷層,特別是存在於表層之Cr,以及存在於合金層之Cr會抑制鍍敷層之腐蝕反應,據此可抑制將裂隙作
為起點的腐蝕的擴大。為了特別提升鍍敷層於彎曲加工變形後的耐蝕性,在鍍敷層中之50nm深度的最外層內的Cr的含量係以300質量ppm以上為較佳,特別是以200~400質量ppm的範圍為較佳。又,為了特別提升鍍敷層於彎曲加工變形後的耐蝕性,相對於鍍敷層內的Cr的含有比例(質量比例),合金層中的Cr的含有比例(質量比例)之比以20以上為較佳,特別以20~30的範圍為較佳。
鍍敷層係以進而含有Sr來作為構成元素為較佳。此情形時,藉由Sr而可特別促進鍍敷層中之Si-Mg層的形成。進而,藉由Sr可抑制鍍敷層的表層中之Mg系氧化皮膜的形成。此係認為是,因為Sr的氧化膜比Mg系氧化皮膜更易於優先形成,而阻礙了Mg系氧化皮膜的形成之緣故。據此,進而可抑制鍍敷層中之皺褶的產生。鍍敷層中之Sr的含量係以1~1000質量ppm的範圍為較佳。該Sr的含量若未滿1質量ppm時,則無法發揮上述之作用,若該含量變得多於1000質量ppm時,則不僅是Sr的作用會達到飽和,於鍍敷鋼板之製造時,在熔融鍍敷浴中亦容易產生浮渣。該Sr的含量係特別以5質量ppm以上為較佳。又,該Sr的含量係特別以500質量ppm以下為較佳,進而以300質量ppm以下為較佳。該Sr的含量係進而以20~50質量ppm的範圍為較佳。
鍍敷層係以進而含有Fe來作為構成元素為較佳。此情形時,藉由Fe而可特別促進鍍敷層中之Si-Mg
層的形成。進而Fe亦有助於鍍敷層的顯微組織及鋅花(spangle)組織的微細化,據此鍍敷層的外觀及加工性為提升。鍍敷層中之Fe的含量係以0.1~1.0質量%的範圍為較佳。若該Fe的含量未滿0.1質量%時,則鍍敷層的顯微組織及鋅花組織會粗大化,而使鍍敷層的外觀惡化,同時,使加工性惡化。若該含量多於1.0質量%時,則鍍敷層的鋅花會過於微細化、或消失,從而藉由鋅花之外觀提升將消失,同時,於表面處理鋼材的製造時,在熔融鍍敷浴中容易產生浮渣,而使鍍敷層的外觀進一步惡化。該Fe的含量係特別以0.2質量%以上為較佳。又,該Fe的含量係特別以0.5質量%以下為較佳。Fe的含量係以0.2~0.5質量%的範圍為特佳。
鍍敷層係進而亦可含有選自由鹼土類元素、Sc、Y、鑭元素、Ti及B之元素來作為構成元素。
鹼土類元素(Be、Ca、Ba、Ra)、Sc、Y、及鑭元素(La、Ce、Pr、Nd、Pm、Sm、Eu等)係發揮與Sr相同之作用。鍍敷層中,該等成分的含量之總量,依質量比率計算,以1.0質量%以下為較佳。
若鍍敷層含有Ti及B中之至少一方時,藉由鍍敷層的α-Al相(樹枝狀結晶組織)的微細化來使鋅花微細化,因此,藉由鋅花而提升了鍍敷層的外觀。進而,藉由Ti及B中之至少一方,可進一步抑制在鍍敷層的皺褶的產生。此係認為是,因藉由Ti及B的作用下,Si-Mg相也微細化,該微細化的Si-Mg相,在熔融鍍敷金屬凝固
而形成鍍敷層的程序中,有效地抑制熔融鍍敷金屬的流動之緣故。進而,藉由如此般的鍍敷組織的微細化,使彎曲加工時的鍍敷層內的應力的集中緩和,而可抑制較大的裂隙的產生等,鍍敷層的彎曲加工性為進一步提升。為了發揮前述作用,熔融鍍敷浴2中之Ti及/或B的含量的合計,依質量比率計算為0.0005~0.1質量%的範圍為較佳。該Ti及/或B的含量的合計係特別以0.001質量%以上為較佳。又,該Ti及/或B的含量的合計係特別以0.05質量%以下為較佳。Ti及/或B的含量的合計係以0.001~0.05質量%的範圍為特佳。
Zn係在鍍敷層的構成元素全體之中,佔有除去Zn以外的構成元素的剩餘部分。
鍍敷層係以不包含上述以外的元素來作為構成元素為較佳。特別是,鍍敷層係以僅含有Al、Zn、Si、Mg、Cr、Sr、及Fe來作為構成元素、或僅含有選自該等的元素、以及鹼土類元素、Sc、Y、鑭元素、Ti及B之元素來作為構成元素為較佳。
但,雖然不用言及,但鍍敷層亦可含有Pb、Cd、Cu、Mn等的不可避免的雜質。該不可避免的雜質的含量係以盡可能少為較佳,特別是該不可避免的雜質的含量的合計,相對於鍍敷層,依質量比率計算較佳為1質量%以下。
較佳的實施形態中,藉由將鋼材浸漬於具有與鍍敷層的構成元素的組成為一致組成的熔融鍍敷浴中來實施。藉由熔融鍍敷處理而在鋼材與鍍敷層之間形成合金層,但因此產生之組成的變動係小到能夠被忽視的程度。
本實施形態中,準備例如含有25~75質量%的Al、0.5~10質量%的Mg、0.02~1.0質量%的Cr、相對於Al為0.5~10質量%的Si、1~1000質量ppm的Sr、0.1~1.0質量%的Fe、及Zn的熔融鍍敷浴。熔融鍍敷浴中之Si:Mg的質量比係以100:50~100:300的範圍為較佳。
又,其他的實施形態中,可準備例如含有25~75質量%的Al、0.02~1.0質量%的Cr、相對於Al為0.5~10質量%的Si、0.1~0.5質量%的Mg、0.1~0.6質量%的Fe、在1~500質量ppm的範圍的Sr,或進而含有選自由鹼土類元素、鑭元素、Ti及B之成分,並將剩餘部分設為Zn的熔融鍍敷浴。
藉由熔融鍍敷處理所形成的鍍敷層將難以產生皺褶。以往,含有Mg的熔融金屬(熔融鍍敷金屬)若藉由熔融鍍敷處理而附著於鋼材時,Mg容易在該熔融鍍敷金屬的表層濃縮,因此,形成Mg系氧化皮膜,起因於該Mg系氧化皮膜而容易在鍍敷層上產生皺褶。然而,若藉由使用具有上述組成之熔融鍍敷浴來形成鍍敷層時,附著於鋼材上的熔融鍍敷金屬的表層中之Mg的濃縮會受到抑制,故即使熔融鍍敷金屬流動,在鍍敷層的表面亦不易
產生皺褶。進而,該熔融鍍敷金屬內部的流動性會降低,而抑制熔融鍍敷金屬的流動本身,因此,更不易產生前述皺褶。
如前述般的Mg的濃縮及熔融鍍敷金屬的流動的抑制,係可認為是依據下述般的機制。
在附著於鋼材的表面上的熔融鍍敷金屬被冷卻而凝固的過程中,首先α-Al相作為初晶而被析出,並成長呈現樹枝狀結晶狀。若如此般進行富含Al的α-Al相的凝固時,則剩餘部分的熔融鍍敷金屬中(即,熔融鍍敷金屬之尚未凝固的成分中)的Mg與Si濃度將緩慢地變高。接著,若對鋼材進行冷卻使其溫度進一步降低時,則從剩餘部分的熔融鍍敷金屬之中會凝固析出含有Si的Si含有相(Si-Mg相)。該Si-Mg相,如上述般係由Mg與Si的合金所構成的相。藉由Cr、Fe及Sr可促進該Si-Mg相的析出‧成長。藉由熔融鍍敷金屬中之Mg併入該Si-Mg相中,可阻礙Mg向熔融鍍敷金屬的表層移動,而可抑制在該熔融鍍敷金屬的表層中之Mg的濃縮。
進而,熔融鍍敷金屬中之Sr亦有助於抑制Mg的濃縮。此係認為是,因為在熔融鍍敷金屬中,Sr係與Mg為相同容易氧化的元素,因而Sr與Mg爭相地在鍍敷表面形成氧化膜,結果是Mg系氧化皮膜的形成會受到抑制之緣故。
進而,藉由於如前述之初晶的α-Al相以外的剩餘部分的熔融鍍敷金屬中Si-Mg相的凝固成長,熔融鍍
敷金屬成為固液混相狀態,因此,熔融鍍敷金屬本身的流動性會降低,其結果是鍍敷層表面的皺褶的產生會受到抑制。
Fe在控制鍍敷層的顯微組織或鋅花方面是重要的。Fe對鍍敷層的組織產生影響的理由目前尚不明確,但可認為是,Fe係在熔融鍍敷金屬中與Si合金化,該合金於熔融鍍敷金屬的凝固時成為凝固核之緣故。
進而,Sr與Mg相同是卑元素,因而藉由Sr的作用下,進一步強化了鍍敷層的犠牲防蝕作用,從而進一步提升了表面處理鋼材的耐蝕性。Sr係也發揮抑制Si相及Si-Mg相的析出形態的針狀化的作用,因此,Si相及Si-Mg相會產生球狀化,而使鍍敷層中之裂隙的產生受到抑制。
於熔融鍍敷處理時,在鍍敷層與鋼材之間亦形成含有熔融鍍敷金屬中之Al的一部分的合金層。例如若在鋼材不施予預鍍敷之情形時,會形成以鍍敷浴中之Al與鋼材中之Fe作為主體的Fe-Al系的合金層。若在鋼材上施予預鍍敷之情形時,則形成包含鍍敷浴中之Al與預鍍敷的構成元素的一部分或全部、或進而包含鋼材中之Fe的合金層。
若鍍敷浴含有Cr之情形時,合金層係包含Al與進而一起的Cr來作為構成元素。合金層係因應鍍敷浴的組成、預鍍敷的有無、鋼材1的組成等,除Al與Cr以外還可含有Si、Mn、Fe、Co、Ni、Cu、Zn、Sn等的各種
的金屬元素來作為構成元素。
熔融鍍敷金屬中的Cr的一部分以比在鍍敷層中更高的濃度包含於合金層中。若形成如此般的合金層時,藉由合金層中之Cr而促進鍍敷層中之Si-Mg相的成長,從而鍍敷層中之Si-Mg相之體積比例會變高,同時,相對於鍍敷層中之Mg全量,Si-Mg相中之Mg的比例會變高。據此之效果係如上述般因而不重複說明。
若合金層的厚度過大時,則表面處理鋼材的加工性會降低,但藉由在熔融鍍敷浴中之Si的作用下,前述合金層的過量的成長會受到抑制,因此,可確保表面處理鋼材的良好的加工性。合金層的厚度係以0.05~5μm的範圍為較佳。若合金層的厚度為前述範圍時,表面處理鋼材的耐蝕性將會充分地提升,同時,加工性也將會充分地提升。
進而,在鍍敷層內於其表面附近使Cr的濃度保持在一定範圍,隨之使鍍敷層的耐蝕性進一步提升。該理由尚未明確,但可推測係因為Cr與氧結合而在鍍敷層的表面附近形成複合氧化膜之緣故。為了提升如此般的鍍敷層的耐蝕性,在鍍敷層中之50nm深度的最外層內的Cr的含量以100~500質量ppm為較佳。
若熔融鍍敷浴含有Cr時,鍍敷層的彎曲加工變形後的耐蝕性亦會提升。其理由係可認為如下述般。若受到嚴苛的彎曲加工變形時,則在鍍敷層及鍍敷層上的塗裝皮膜有產生裂隙之情形。此時,水或氧通過裂隙而進入
鍍敷層內,鍍敷層內的合金直接暴露在腐蝕因子下。但,存在於鍍敷層,特別是存在於表層之Cr,以及存在於合金層之Cr會抑制鍍敷層之腐蝕反應,據此可抑制將裂隙作為起點的腐蝕的擴大。
上述較佳的實施形態中所處理的熔融鍍敷金屬,係包含七成分以上的元素的多元系熔融金屬,其凝固過程極為複雜而理論上將難以預測,但本發明人透過在實驗下的觀察等,得到了上述重要的見解。
藉由對熔融鍍敷浴的組成進行如上述般的調整,則如上述般,可達成抑制鍍敷層中之皺褶或垂流、以及確保表面處理鋼材的耐蝕性與加工性。
若熔融鍍敷浴特別是含有Ca之情形時,可明顯抑制在熔融鍍敷浴中之浮渣的產生。若熔融鍍敷浴含有Mg之情形時,即使Mg的含量為10質量%以下,亦難以避免某種程度的浮渣的產生,為了確保表面處理鋼材的良好的外觀,需要除去來自鍍敷浴的浮渣,但若熔融鍍敷浴進一步含有Ca時,則起因於Mg的浮渣的產生將受到明顯地抑制。據此,進一步抑制了表面處理鋼材的外觀因浮渣而致使的惡化,同時,可減輕從熔融鍍敷浴除去浮渣所需要的勞力和時間。在熔融鍍敷浴中之Ca的含量係以100~5000質量ppm的範圍為較佳。藉由使該含量為100質量ppm以上,可有效地抑制在熔融鍍敷浴中之浮渣的產生。若Ca的含量過量時,則有可能產生起因於該Ca的浮渣之虞,但藉由使Ca的含量為5000質量ppm以下,
則可抑制起因於Ca的浮渣。該含量係進一步以200~1000質量ppm的範圍為較佳。
藉由如上述般抑制鍍敷層的表面的皺褶,特別是以在鍍敷層的表面不存在高度大於200μm且陡峭度大於1.0的隆起為較佳。所謂陡峭度,係指依(隆起的高度(μm))÷(隆起的底面的寬(μm))所規定的值。隆起的底面係包含隆起的周圍的平坦面之假設的平面與隆起相交的部位。所謂隆起的高度係指從隆起的底面至隆起的頂端為止的高度。若陡峭度低之情形時,鍍敷層的外觀將進一步提升。進而,若在鍍敷層上重疊形成如後述般之塗膜之情形時,可防止隆起頂破前述塗膜,同時,能夠使前述塗膜的厚度容易地均勻化。據此,形成塗膜的表面處理鋼材的外觀將會提升,同時,藉由塗膜使表面處理鋼材能夠發揮進一步優異的耐蝕性等。
如此般的Mg的濃縮的程度、Si-Mg相的狀態、合金層的厚度及鍍敷層的表面隆起的陡峭度的調整,可藉由使用上述組成的熔融鍍敷浴來對鋼材施予熔融鍍敷處理而能夠達成。
於熔融鍍敷處理時,可對於形成含有選自Cr、Mn、Fe、Co、Ni、Cu、Zn、Sn之至少一種的成分的預鍍敷層的鋼材,施予用於形成鍍敷層的熔融鍍敷處理。藉由對於施予前述熔融鍍敷處理前的鋼材進行預鍍敷處理,而可在該鋼材的表面上形成預鍍敷層。藉由該預鍍敷層,提升了熔融鍍敷處理時的鋼材與熔融鍍敷金屬之濕潤
性,從而改善鋼材與鍍敷層之間的密著性。
預鍍敷層雖然會因為構成預鍍敷層的金屬的種類而相異,但亦有助於鍍敷層的表面外觀或耐蝕性之更加提升。例如在形成含有Cr的預鍍敷層之情形時,在鋼材與鍍敷層之間可促進含有Cr的合金層的形成,從而使表面處理鋼材的耐蝕性進一步提升。例如在形成含有Fe或Ni的預鍍敷層之情形時,鋼材與熔融鍍敷金屬之濕潤性為提升,從而大大地改善鍍敷層的密著性,進而促進Si-Mg相的析出,而使鍍敷層的表面外觀進一步提升。促進Si-Mg相的析出,係可認為是起因於預鍍敷層與熔融鍍敷金屬之反應而產生的。
預鍍敷層的附著量並無特別限定,但在鋼材的單面上的附著量以0.1~3g/m2的範圍為較佳。該附著量若未滿0.1g/m2時,則鋼材表面難以被預鍍敷層覆蓋,無法充分發揮藉由預鍍敷之改善效果。又若該附著量超過3g/m2之情形時,不僅改善效果會達到飽和且製造成本亦會變高。
以下,就用於對鋼材實施熔融鍍敷處理的熔融鍍敷處理裝置的概要、以及對於熔融鍍敷處理為適合的處理條件,一邊參考圖1等一邊進行說明。圖1係表示熔融鍍敷處理裝置的一例之概略圖。
處理對象之鋼材1係由碳鋼、合金鋼、不鏽鋼、鎳鉻鋼、鎳鉻鉬鋼、鉻鋼、鉻鉬鋼、錳鋼等的鋼鐵所形成之構件。作為鋼材1,可舉出薄鋼板、厚鋼板、型
鋼、鋼管、鋼線等的各種之構件。即,鋼材1的形狀並無特別限制。
於熔融鍍敷處理之前,亦可對鋼材1施予助熔劑處理(flux treatment)。藉由該助熔劑處理,能夠改善鋼材1與熔融鍍敷浴2的濕潤性及密著性。於被浸漬於熔融鍍敷浴2前,亦可對鋼材1施予加熱退火‧還原處理,亦可省略該處理。如上述般於熔融鍍敷處理之前,亦可對鋼材1施予預鍍敷處理。
以下,作為鋼材1若採用板材(鋼板1a)之情形時,即,製造熔融鍍敷鋼板時,對於熔融鍍敷鋼板之製造步驟進行說明。
圖1所表示之熔融鍍敷處理裝置係具備連續地運送鋼板1a的運送裝置。該運送裝置係由退捲機3、捲揚機12、及多個的運送輥15所構成。該運送裝置中,將長條的鋼板1a的線圈13(第一線圈13)存放在退捲機3。該第一線圈13由退捲機3開捲,鋼板1a由運送輥15一邊支撐一邊被運送至捲揚機12。進而,捲揚機12捲繞該鋼板1a,將鋼板1a的線圈12(第二線圈12)存放在該捲揚機12。
在該熔融鍍敷處理裝置中,從採用前述運送裝置之鋼板1a的運送路徑的上游側依序設置有加熱爐4、退火‧冷卻部5、爐鼻(snout)6、瓶7、噴射噴嘴9、冷卻裝置10、調質軋延‧形狀矯正裝置11。加熱爐4係對鋼板1a進行加熱。該加熱爐4係由無氧化爐等所構
成。退火‧冷卻部5係對鋼板1a進行加熱退火,接著進行冷卻。該退火‧冷卻部5係與加熱爐4連結,分別將退火爐設置在上游側,冷卻帶(冷卻機)設置在下游側。該退火‧冷卻部5內係保持在還原性氣氛下。爐鼻6係在其內部運送鋼板1a的筒狀構件,其一端與前述退火‧冷卻部5連結,另一端配置在瓶7內的熔融鍍敷浴2內。爐鼻6內與退火‧冷卻部5內相同地保持在還原性氣氛下。瓶7係儲存熔融鍍敷浴2的容器,其內部配置沉浸輥(sink roller)8。噴射噴嘴9係向鋼板1a噴射氣體。噴射噴嘴9設置在瓶7的上方。該噴射噴嘴9配置在可朝向從瓶7取出的鋼板1a的兩面噴射氣體的位置。冷卻裝置10係對附著於鋼板上的熔融鍍敷金屬進行冷卻。作為該冷卻裝置10係設置有空冷機、噴霧冷卻機機等,採用該冷卻裝置10對鋼板1a進行冷卻。調質軋延‧形狀矯正裝置11係對形成有鍍敷層的鋼板1a進行調質軋延及形狀矯正。該調質軋延‧形狀矯正裝置11具備有用於對鋼板1a進行調質軋延的平整機等、或用於對調質軋延後的鋼板1a進行形狀矯正的張力矯直機等。
使用該熔融鍍敷處理裝置的熔融鍍敷處理中,首先由退捲機3將鋼板1a開捲並連續地投放。該鋼板1a在加熱爐4中加熱後,被運送至還原性氣氛的退火‧冷卻部5,並用退火爐中進行退火,同時,在進行了附著於鋼板1a的表面的軋延油等的去除或氧化膜的還原去除等的表面清淨化後,於冷卻帶進行冷卻。接著,鋼板
1a通過爐鼻6,進而侵入瓶7而被浸漬於該瓶7內的熔融鍍敷浴2中。鋼板1a被沉浸輥8支撐在瓶7內,其運送方向轉換到上方,從熔融鍍敷浴2拉出。據此,將熔融鍍敷金屬附著於鋼板1a上。
接著,藉由從噴射噴嘴9向該鋼板1a的兩面噴射氣體,從而可調整附著於鋼板1a上的熔融鍍敷金屬的附著量。將藉由如此般的氣體的噴射進行附著量之調整方法稱為氣體摩擦接觸法。該熔融鍍敷金屬的附著量為合併鋼板1a的兩面合計,以調整為40~200g/m2的範圍為較佳。
作為氣體摩擦接觸法中向鋼板1a所噴射的氣體(摩擦接觸氣體)的種類,可舉出大氣、氮、氬、氦、水蒸氣等。該等的摩擦接觸氣體亦可在預備加熱後向鋼板1a噴射。本實施形態中藉由使用特定組成的熔融鍍敷浴2,本質上可抑制熔融鍍敷金屬中之Mg的表面氧化濃縮(熔融鍍敷金屬的表層中之Mg的氧化以及Mg濃度的上昇)。因此,即使是摩擦接觸氣體中包含氧、或摩擦接觸氣體的噴射所伴隨的氣流中包含氧,也不會損及發明的效果而可進行鍍敷附著量(附著於鋼板1a上的熔融鍍敷金屬的量)的調整。
鍍敷附著量的調整方法當然不限於前述氣體摩擦接觸法,可適用各種的附著量控制法。作為氣體摩擦接觸法以外的附著量控制法,可舉例如:使鋼板1a通過配置在熔融鍍敷浴2的浴面正上方的一對輥間的輥擠壓
法;在接近從熔融鍍敷浴2中拉出的鋼板1a處配置遮蔽板,並採用該遮蔽板來擦拭熔融鍍敷金屬的方法;對附著於鋼板1a上的熔融鍍敷金屬,使用電磁力而施加使其向下方移動的力的電磁力摩擦接觸法;不施加外力而利用自然重力落下來調整鍍敷附著量的方法等。亦可組合二種以上的鍍敷附著量的調整方法。
接著,在該鋼板1a被運送至比噴射噴嘴9的配置位置更靠上方後,藉由二個運送輥15支撐而向下方折返之方式來運送。即,鋼板1a係以逆U字狀的路徑運送。該逆U字狀的路徑中,鋼板1a在冷卻裝置10中藉由空冷或噴霧冷卻機等進行冷卻。據此,附著於鋼板1a的表面上的熔融鍍敷金屬凝固而形成鍍敷層。
為了藉由冷卻裝置10的冷卻來使熔融鍍敷金屬的凝固完全結束,鋼板1a上以藉由冷卻裝置10使熔融鍍敷金屬(或者鍍敷層)的表面溫度冷卻至300℃以下為較佳。熔融鍍敷金屬的表面溫度係例如用放射溫度計等來進行測定。如此般為了形成鍍敷層,該鋼板1a從鍍敷浴2中拉出後,在鋼板1a上的熔融鍍敷金屬的表面冷卻至300℃為止的期間的冷卻速度以5~100℃/sec的範圍為較佳。為了控制鋼板1a的冷卻速度,冷卻裝置10以具備有用於沿著其運送方向及板寬方向來調節鋼板1a的溫度的溫度控制機能為較佳。冷卻裝置10亦可沿著鋼板1a的運送方向分割成多個。圖1中,在比噴射噴嘴9的配置位置更靠上方的運送路徑中,設置有冷卻鋼板1a的一次冷卻
裝置101、與在一次冷卻裝置101的下游側設置來冷卻鋼板1a的二次冷卻裝置102。一次冷卻裝置101與二次冷卻裝置102亦可進一步分割成多個。此情形時,例如可在一次冷卻裝置101中將鋼板1a冷卻至熔融鍍敷金屬的表面為300℃或者300℃以下的溫度,進而在二次冷卻裝置102中,將鋼板1a冷卻至導入調質軋延‧形狀矯正裝置11時的溫度為100℃以下。
在鋼板1a冷卻的過程中,鋼板1a上的熔融鍍敷金屬的表面溫度為500℃以上之期間時,熔融鍍敷金屬的表面的冷卻速度以50℃/sec以下為較佳。此情形時,鍍敷層表面中之Si-Mg相的析出特別會受到抑制,因此,可抑制垂流的產生。該溫度區域的冷卻速度對Si-Mg相的析出行為產生影響的理由目前尚不明確,但可認為是,該溫度區域的冷卻速度越快時,則熔融鍍敷金屬中之厚度方向的溫度梯度會變大,因此,在溫度更低的熔融鍍敷金屬的表面優先促進Mg-Si層的析出,其結果為在鍍敷最表面的Si-Mg相的析出量變多。該溫度區域的冷卻速度係以40℃/sec以下為更佳,以35℃/sec以下為特佳。
對冷卻後的鋼板1a採用調質軋延‧形狀矯正裝置11施予調質軋延後,再施予形狀矯正。調質軋延之壓下率係以0.3~3%的範圍為較佳。形狀矯正之鋼板1a的延伸率係以3%以下為較佳。
接著,鋼板1a係用捲揚機12進行捲揚,將鋼板1a的線圈14存放在該捲揚機12。
於如此般的熔融鍍敷處理時,瓶7內的熔融鍍敷浴2的溫度,以高於該熔融鍍敷浴2的凝固開始溫度,且較前述凝固開始溫度高溫40℃以下的溫度為較佳。瓶7內的熔融鍍敷浴2的溫度,以高於熔融鍍敷浴2的凝固開始溫度,且較前述凝固開始溫度高溫25℃以下的溫度為更佳。若如此般限制熔融鍍敷浴2的溫度的上限時,則在鋼板1a從熔融鍍敷浴2拉出後,直到附著於該鋼板1a上的熔融鍍敷金屬凝固所需要的時間將可縮短。其結果是附著於鋼板1a上的熔融鍍敷金屬處於能夠流動的狀態的時間亦會縮短,因此,鍍敷層更加難以產生皺褶。若前述熔融鍍敷浴2的溫度較熔融鍍敷浴2的凝固開始溫度高溫20℃以下時,則可特別顯著地抑制鍍敷層中之皺褶的產生。
在鋼板1a從熔融鍍敷浴2中拉出時,可拉出至非氧化性氣氛或低氧化性氣氛中,進而亦可在該非氧化性氣氛或低氧化性氣氛中,藉由氣體摩擦接觸法對鋼板1a施予熔融鍍敷金屬的附著量的調整。因此,例如圖2所表示般,從熔融鍍敷浴2拉出的鋼材1,在比熔融鍍敷浴2更靠上游側的運送路徑(從熔融鍍敷浴2朝向上方的運送路徑)中,以被中空的構件22所包圍,同時,該中空的構件22的內部充滿氮氣等的非氧化性氣體或低氧化性氣體為較佳。所謂非氧化性氣體或低氧化性氣體係指與大氣相比較,氧濃度較低的氣體之意。非氧化性氣體或低氧化性氣體的氧濃度係以1000ppm以下為較佳。充滿非
氧化性氣體或低氧化性氣體的氣氛為非氧化性氣氛或低氧化性氣氛,在該氣氛中氧化反應會受到抑制。噴射噴嘴9被配置在中空的構件22的內側。中空的構件22被設置在從熔融鍍敷浴2內(熔融鍍敷浴2的上部)開始遍及該熔融鍍敷浴2的上方且包圍鋼材1的運送路徑。進而,從噴射噴嘴9所噴射的氣體也以氮氣等的非氧化性氣體或低氧化性氣體為較佳。此情形時,從熔融鍍敷浴2拉出的鋼板1a由於被暴露在非氧化性氣氛或低氧化性氣氛中,因而附著於鋼板1a上的熔融鍍敷金屬的氧化會受到抑制,從而該熔融鍍敷金屬的表層更加難以形成Mg系氧化皮膜。因此,可進一步抑制鍍敷層中之皺褶的產生。亦可使包含鋼板1a的運送路徑的熔融鍍敷處理裝置的一部分、或者熔融鍍敷處理裝置的全部配置在非氧化性氣氛或低氧化性氣氛中,來替代中空的構件22的使用。
對於熔融鍍敷處理後的鋼板1a,進而以施予過時效處理(overageing treatment)為較佳。此情形時,表面處理鋼材的加工性會進一步提升。過時效處理係藉由使鋼板1a在一定溫度範圍內保持一定時間來實施。
圖3係表示過時效處理中所使用的裝置,其中分別是圖3(a)表示加熱裝置、圖3(b)表示保溫容器20。加熱裝置係具備連續地運送熔融鍍敷處理後的鋼板1a的運送裝置。該運送裝置係與熔融鍍敷處理裝置中之運送裝置為相同的,由退捲機16、捲揚機17、及多個的運送輥21所構成。在藉由該運送裝置之鋼板1a的運送
路徑上,設置感應加熱爐等的加熱爐18。保溫容器20能夠在內部存放鋼板1a的線圈19,且只要是具有隔熱性的容器即可並無特別限制。保溫容器20亦可是大型的容器(保溫室)。
在對鋼板1a施予過時效處理之情形時,首先採用吊車或台車等從熔融鍍敷處理裝置的捲揚機12,搬送熔融鍍敷處理後的鋼板1a的線圈14,將其存放在加熱裝置的退捲機16中。在加熱裝置中,首先從退捲機16將鋼板1a開捲而連續地投放。該鋼板1a在加熱爐18中加熱至適合於過時效處理的溫度後,用捲揚機17捲揚,從而將該鋼板1a的線圈19存放在捲揚機17。
接著,採用吊車或台車等從捲揚機17來運搬鋼板1a的線圈19,將其存放在保溫容器20內。在該保溫容器20內使前述鋼板1a的線圈19保持一定時間,從而對鋼板1a施予過時效處理。
依據本實施形態,在鋼板1a的表面上所形成的鍍敷層係含有Mg,由於在鍍敷層的表面上僅存在些許的Mg系氧化皮膜,因而在過時效處理時,在鋼板1a的線圈中鍍敷層彼此之間即使是重疊,在鍍敷層間亦難以產生灼燒或熔化接著。因此,即便是過時效處理時的保溫時間為長時間、或者是保溫溫度為高溫,亦難以產生灼燒,能夠對鋼板1a施予充分的過時效處理。據此,大大地提升了熔融鍍敷鋼板的加工性,同時,過時效處理的效率為提升。
在過時效處理時,特別以藉由加熱裝置使加熱後的鋼板1a的溫度成為180~220℃的範圍,即,鋼板1a的溫度為前述範圍內的狀態下使鋼板從保溫容器外向保溫容器內移動為較佳。在保溫容器內的鋼板1a的保持時間y(hr)係以滿足下述式(1)為較佳。
5.0×1022×t-10.0≦y≦7.0×1024×t-10.0…(1)
(但150≦t≦250)
式(1)中之t(℃)係前述保持時間y(hr)中之鋼板1a的溫度(保持溫度),在鋼板1a產生溫度變動之情形下為其最低溫度。
尚,本實施形態中,熔融鍍敷處理裝置及加熱裝置是個別的裝置,但藉由使熔融鍍敷處理裝置具備加熱爐21,熔融鍍敷處理裝置亦可兼作加熱裝置。該等的裝置中,亦可因應所需對各種的要素進行追加、除去、置換等而適當地設計變更。本實施形態之熔融鍍敷處理裝置及加熱裝置係適於鋼材1為鋼板1a之情形,但熔融鍍敷處理裝置、加熱裝置等的構成係可因應鋼材1的形狀等而進行各種設計變更。在對鋼材1施予鍍敷前處理之情形時,該鍍敷前處理亦可因應鋼材1的種類、形狀等進行各種變更。
對如此般施予熔融鍍敷處理、或者進而施予過時效處理的鋼材1,可重疊在鍍敷層上進行非鉻酸鹽化學轉化處理,並在其上形成使用塗料組成物而成的塗膜。
本發明之塗料組成物係含有塗膜形成性樹脂(a)、交聯劑(b)、選自由釩酸鹼土金屬鹽之至少1種的釩化合物(c)、與第三磷酸鎂(d)。又,因應所需亦可含有密著性提升成分、體質顏料等的添加劑。在塗膜之上亦可塗布其他的塗料來作為面塗層。
本發明之塗料組成物中所使用之塗膜形成性樹脂(a)係熱硬化性樹脂。作為熱硬化性樹脂,只要是具有能夠與後述的交聯劑(b)反應的官能基、且具有塗膜形成能力的樹脂即可並無特別限制,可舉例如環氧樹脂及其變性物(丙烯酸變性環氧樹脂等);聚酯樹脂及其變性物(胺基甲酸酯變性聚酯樹脂、環氧變性聚酯樹脂、聚矽氧變性聚酯樹脂等);丙烯酸樹脂及其變性物(聚矽氧變性丙烯酸樹脂等);胺基甲酸酯樹脂及其變性物(環氧變性胺基甲酸酯樹脂等);酚樹脂及其變性物(丙烯酸變性酚樹脂、環氧變性酚樹脂等);苯氧基樹脂;醇酸樹脂及其變性物(胺基甲酸酯變性醇酸樹脂、丙烯酸變性醇酸樹脂等);氟樹脂;聚苯醚樹脂;聚醯胺醯亞胺樹脂;聚醚醯亞胺樹脂等的樹脂。該等的樹脂可僅單獨使用1種,亦可併用2種以上。
上述之中,作為塗膜形成性樹脂(a),就所得到之塗膜的彎曲加工性或所得到之塗膜的耐濕性、耐蝕性及耐候性平衡之觀點而言,可使用環氧樹脂、聚酯樹脂
或該等的變性物等的熱硬化性樹脂,可從該等中選擇1種以上來使用。作為熱硬化性樹脂,較佳為選自含羥基之環氧樹脂、含羥基之聚酯樹脂及含有羥基的該等的變性物中之1種以上來使用。若環氧樹脂、聚酯樹脂及該等的變性物具有羥基時,則作為交聯劑(b)係可選擇各種的胺基樹脂、各種的異氰酸酯化合物。其結果是藉由從各種的交聯劑(b)之中選擇具有所期望的性質的交聯劑(b),而能夠賦予塗膜多樣的物性,因此為特佳。
上述含羥基之環氧樹脂(包含含羥基之環氧樹脂變性物)的數平均分子量(Mn)係以1,400~15,000為較佳,以2,000~10,000為又較佳,以2,000~4,000為特佳。上述含羥基之環氧樹脂的玻璃轉移溫度(Tg)係以60~120℃為較佳,以60~85℃為又較佳。又,上述含羥基之聚酯樹脂(包含含羥基之聚酯樹脂變性物)的數平均分子量(Mn)係以1,800~40,000為較佳,以2,000~30,000為又較佳,以10,000~20,000為特佳。上述含羥基之聚酯樹脂的玻璃轉移溫度(Tg)係以0~80℃為較佳,以10~40℃為又較佳。所使用的含羥基之環氧樹脂及/或含酸基之聚酯樹脂的數平均分子量(Mn)係藉由設為上述範圍內,則與後述的交聯劑(b)之交聯反應可充分地進行,且塗膜的耐濕性亦變得充分,伴隨於此可確保耐蝕性之同時,所得到之塗料組成物將成為適當黏度而操作性變得良好。又,塗膜中所包含之釩化合物、第三磷酸鎂的溶出將變得適當,在酸性環境條件下的耐蝕性為良好,故為較
佳。又,所使用的含羥基之環氧樹脂及/或含羥基之聚酯樹脂的玻璃轉移溫度(Tg)藉由設為上述範圍內,則塗膜的透濕性不會變得過高,塗膜的耐濕性將為充分、且耐蝕性亦變得良好。
作為上述含羥基之環氧樹脂(包含含羥基之環氧樹脂變性物),可舉例如三菱化學製的商品名「jER1004」、「jER1007」、「E1255HX30」(雙酚A骨架)、「YX8100BH30」(於此「jER」為註冊商標)。又,作為含羥基之聚酯樹脂(包含含羥基之聚酯樹脂變性物),可舉例如DIC製的商品名「BECKOLITE 47-335」、東洋紡製的商品名「VYLON 220」、「VYLON UR3500」、「VYLON UR5537」、「VYLON UR8300」等(於此「VYLON」為註冊商標)。
尚,本說明書中,所謂數平均分子量(Mn)係指使用凝膠滲透層析法(GPC)所測定的以標準聚苯乙烯的分子量為基準而由色譜所算出的值。又,本說明書中,所謂玻璃轉移溫度(Tg)係指使用熱分析裝置(Seiko Instruments製的商品名「TMA100/SSC5020」)進行測定的值。
本發明之塗料組成物中之塗膜形成性樹脂(a)的含量,通常為全固形分中10~80質量%,以20~70質量%為較佳。藉由設為10質量%以上,則彎曲加工性、塗裝作業性、塗膜強度將為良好。又,藉由塗膜形成性樹脂(a)的含量設為80質量%以下,則可得到充分的耐蝕
性。
本發明之塗料組成物亦可含有熱可塑性樹脂(j)來作為塗膜形成性樹脂(a)以外的樹脂。作為熱可塑性樹脂(j),可舉例如氯化聚乙烯、氯化聚丙烯等的氯化烯烴系樹脂;將氯乙烯、乙酸乙烯酯、偏二氯乙烯等作為單體成分的均聚物或共聚物;纖維素系樹脂;縮醛樹脂;醇酸樹脂;氯化橡膠系樹脂;變性聚丙烯樹脂(酸酐變性聚丙烯樹脂等);氟樹脂(例如偏二氟乙烯樹脂、氟乙烯樹脂、氟化烯烴與乙烯醚之共聚物、氟化烯烴與乙烯酯之共聚物)等。熱可塑性樹脂(j)可僅單獨使用1種,亦可併用2種以上。藉由併用熱可塑性樹脂(j),能夠將塗膜物性調製成所期望的性質。
交聯劑(b)係與熱硬化性樹脂反應而形成硬化塗膜者。作為交聯劑(b)可舉出:將聚異氰酸酯化合物的異氰酸酯基以含活性氫之化合物封端所得之封端聚異氰酸酯化合物(f)、胺基樹脂(g)、酚樹脂等,其中,以使用選自由封端聚異氰酸酯化合物(f)、及在1個分子中具有平均1個以上的羥甲基或亞胺基之胺基樹脂(g)所成之群之1種以上為較佳。
作為構成上述聚異氰酸酯化合物及上述封端聚異氰酸酯化合物(f)的聚異氰酸酯化合物並無特別限制,可使用以往周知者。例如有1,4-四亞甲基二異氰酸
酯、1,6-六亞甲基二異氰酸酯、1,12-十二亞甲基二異氰酸酯、環己烷-1,3-或1,4-二異氰酸酯、1-異氰酸基-3-異氰酸基甲基-3,5,5-三甲基環己烷(別名異佛酮二異氰酸酯;IPDI)、二環己基甲烷-4,4’-二異氰酸酯(別名:氫化MDI)、2-或4-異氰酸基環己基-2’-異氰酸基環己基甲烷、1,3-或1,4-雙-(異氰酸基甲基)-環己烷、雙-(4-異氰酸基-3-甲基環己基)甲烷、1,3-或1,4-α,α,α’α’-四甲基二甲苯撐基二異氰酸酯、2,4-或2,6-二異氰酸基甲苯、2,2’-、2,4’-或4,4’-二異氰酸基二苯基甲烷(MDI)、1,5-萘二異氰酸酯、p-或m-伸苯基二異氰酸酯、二甲苯二異氰酸酯、二苯基-4,4’-二異氰酸酯等。又,可使用各二異氰酸酯彼此的環化聚合物(異氰脲酸酯型)、進而亦可使用異氰酸酯‧縮二脲體(雙脲型)、加成物型。聚異氰酸酯化合物可僅單獨使用1種,亦可併用2種以上。異氰脲酸酯型的聚異氰酸酯化合物係本發明中較佳使用的1種。
上述之中,作為聚異氰酸酯化合物係以使用在分子內含有1以上的芳香族官能基的芳香族聚異氰酸酯化合物為較佳。藉由使用芳香族聚異氰酸酯化合物,可使塗膜的耐濕性提升,同時,可使塗膜強度提升。作為較佳使用的芳香族聚異氰酸酯化合物,可舉出2,4-或2,6-二異氰酸基甲苯(TDI)、2,2’-、2,4’-或4,4’-二異氰酸基二苯基甲烷(MDI)、二甲苯二異氰酸酯(XDI)、萘二異氰酸酯(NDI)等。
依據JIS K 7301-1995測定的構成封端聚異氰酸酯化合物(f)的聚異氰酸酯化合物的異氰酸酯基含有率,在聚異氰酸酯化合物的固形分中通常為3~20%,較佳為5~15%。藉由將異氰酸酯基含有率設為上述較佳的範圍的下限值以上,塗膜的硬化性將為充分,故為較佳。另一方面,藉由將異氰酸酯基含有率設為上述較佳的範圍的上限值以下,所得到之塗膜的交聯密度成為適當且耐蝕性為良好,故為較佳。
作為上述封端聚異氰酸酯化合物(f)中所使用的含活性氫之化合物(封端化劑)並無特別限制,可舉出具有-OH基(醇類、酚類等)、=N-OH基(肟類等)、=N-H基(胺類、醯胺類、醯亞胺類、內醯胺類等)的化合物、或具有-CH2-基(活性亞甲基)的化合物、唑類。例如有酚、甲酚、二甲酚、ε-己內醯胺、σ-戊內醯胺、γ-丁內醯胺、甲醇、乙醇、n-、i-、或t-丁醇、乙二醇單乙基醚、乙二醇單丁基醚、二乙二醇單乙基醚、丙二醇單甲基醚、苄醇、甲醯胺肟、乙醛肟、丙酮肟、甲基乙基酮肟、二乙醯單肟、苯甲酮肟、環己烷肟、丙二酸二甲酯、乙醯乙酸乙酯、乙醯丙酮、吡唑等。含活性氫之化合物可僅單獨使用1種,亦可併用2種以上。
封端聚異氰酸酯化合物(f)的熱解離溫度,會與構成此者的聚異氰酸酯化合物及含活性氫之化合物的種類或觸媒的有無及其量而相異,但本發明中,以熱解離溫度(無觸媒狀態)為120~180℃之封端聚異氰酸酯化合
物(f)為較佳使用。藉由使用在該範圍內顯示出解離溫度的封端聚異氰酸酯化合物(f),可使塗料的穩定性提升,又,由於與塗膜形成性樹脂(a)的交聯反應性為優異,因而可得到耐濕性為良好的塗膜。作為解離溫度為120~180℃之封端聚異氰酸酯化合物(f),可舉例如住化Bayer Urethane製的商品名「Desmodur BL3175」、「DESMOTHERM2170」等(於此「Desmodur」、「DESMOTHERM」為註冊商標)。
作為上述胺基樹脂(g),可舉出三聚氰胺樹脂、脲樹脂等,其中以三聚氰胺樹脂為較佳使用。所謂「三聚氰胺樹脂」係指一般是由三聚氰胺與醛所合成的熱硬化性的樹脂之意,且在三嗪核1分子中具有3個反應性官能基-NX1X2。作為三聚氰胺樹脂,可示例:包含作為反應性官能基之-N-(CH2OR)2〔R係烷基,以下相同〕的完全烷基型;包含作為反應性官能基之-N-(CH2OR)(CH2OH)的羥甲基型;包含作為反應性官能基之-N-(CH2OR)(H)的亞胺基型;包含作為反應性官能基之-N-(CH2OR)(CH2OH)與-N-(CH2OR)(H)、或包含-N-(CH2OH)(H)的羥甲基/亞胺基型之4種類。
本發明中,上述三聚氰胺樹脂之中,以使用三嗪核中具有平均1個以上的羥甲基或亞胺基的三聚氰胺樹脂(以下稱為三聚氰胺樹脂(g1))為較佳,即,以使用羥甲基型、亞胺基型或羥甲基/亞胺基型三聚氰胺樹脂或該等的混合物為較佳。三聚氰胺樹脂(g1)即使在無觸
媒下與塗膜形成性樹脂(a)的交聯反應性亦為優異,可得到耐濕性為良好的塗膜。作為三聚氰胺樹脂(g1),可舉例如日本Cytec Industries製的商品名「Mycoat715」等。
本發明之塗料組成物中之交聯劑(b)的含量,相對於塗膜形成性樹脂(a)的固形分100質量%,以固形分為10~80質量%為較佳,又較佳為20~70質量%。相對於塗膜形成性樹脂(a)的固形分100質量%,藉由將交聯劑(b)的含量(固形分換算)設為10質量%以上,則與塗膜形成性樹脂(a)的交聯反應將會充分地進行、且塗膜的透濕性將成為適當,從而塗膜的耐濕性為良好、且耐蝕性為良好。又,相對於塗膜形成性樹脂(a)的固形分100質量%,藉由將交聯劑(b)的含量(固形分換算)設為80質量%以下,則塗膜中之防鏽顏料的溶出為充分,而耐蝕性為良好。
防鏽顏料之釩化合物(c)係由選自由釩酸鹼土金屬鹽及釩酸鎂所成之群之至少1種所成的釩酸金屬鹽。釩化合物(c)係具有特定的導電率,具體而言其1質量%水溶液的導電率在溫度25℃下為200μS/cm~2,000μS/cm。藉由使用指定量的具有該範圍內的導電率的釩化合物(c),可得到耐蝕性與耐濕性為同時提升的塗膜。又,具有該範圍內的導電率的釩化合物(c),因展現適度的
溶解性,不僅是被塗物(鋼板等)的塗裝面,亦可有效地防止端面部的腐蝕。若導電率未滿200μS/cm時,則釩化合物從塗膜向被塗物(鋼板等)的溶出會變少,結果導致耐蝕性降低。又,若導電率超過2,000μS/cm時,塗膜的透濕性變得過高(水易過度浸入塗膜),塗膜的耐濕性會降低,伴隨於此耐蝕性亦會降低。釩化合物(c)的1質量%水溶液的導電率,較佳為200~1,000μS/cm。尚,釩酸金屬鹽中之釩的原子價為3、4、5中之任一,所謂釩酸,原釩酸、與偏釩酸、焦釩酸等的縮合釩酸亦皆為包含。作為釩酸鹼土金屬鹽係以釩酸鈣為較佳。
本說明書中,所謂「1質量%水溶液」係指相對於離子交換水99g添加試樣(例如釩化合物(c))1g,藉以室溫下攪拌4小時後所得到之溶液。但,若添加的試樣在水中的溶解度未滿1質量%之情形時,所添加的試樣亦可不完全溶解在離子交換水中。上述導電率係使用導電度計(例如東亞DKK製導電率計「CM-30ET」),測定該1質量%水溶液在溫度25℃下的導電率時的值。
上述釩酸鈣係以其1質量%水溶液的pH為6.5~11.0為較佳,7.0~10.0為又較佳。藉由使pH設為該範圍內,可顯著地提高本發明的表面處理鋼材的耐蝕性。若釩酸鈣的1質量%水溶液的pH為上述範圍外之情形時,有容易產生鐵、鋅或鋁等的基材的腐蝕之虞。
尚,此處所謂「1質量%水溶液」係與上述意思相同,上述pH係使用pH計(堀場製作所製「F-
54」)測定1質量%水溶液的pH時的值。
本發明中,上述釩化合物(c)的含量,相對於後述之塗膜形成性樹脂(a)的固形分及交聯劑(b)的固形分的合計100質量%為超過50質量%且在150質量%以下,較佳為60~100質量%。若釩化合物(c)的含量,相對於塗膜形成性樹脂(a)及交聯劑(b)的合計固形分100質量%為50質量%以下時,則釩化合物(c)從塗膜向鋼材1的溶出會變少,結果導致耐蝕性降低。又,若釩化合物(c)的含量超過150質量%時,則塗膜的透濕性過高,水容易過度浸入塗膜,塗膜的耐濕性會降低,隨著耐濕性之降低,耐蝕性亦會降低。如此般,本發明中藉由將由防鏽顏料之特定的釩化合物(c)、塗膜形成性樹脂(a)與交聯劑(b)所成之樹脂固形分的比率調整至適當的範圍,能夠同時得到高水準的耐濕性與耐蝕性。
本發明中所使用之釩化合物(c)的調製方法並無特別限制,可使用任何方法。例如若釩化合物(c)為釩酸鈣之情形時,可藉由將鈣化合物與釩酸鹽及/或五氧化釩在水中混合並使其反應而得。藉由該反應所得到之固體(通常為白色固體)因應所需亦可提供予水洗、脫水、乾燥、粉碎等的處理。
作為用於調製釩酸鈣的鈣化合物,可示例如碳酸鈣、氫氧化鈣、氧化鈣、氯化鈣、硝酸鈣、乙酸鈣及硫酸鈣。進而,甲酸鈣等的有機酸的鈣化合物也適合於使用。作為釩酸鹽,可示例釩酸鈣、釩酸鈉、釩酸銨,但並
非限定於該等中。
若使鈣化合物與釩酸鹽反應來調製釩酸鈣之情形時,藉由調整鈣化合物與釩酸鹽及/或五氧化釩的使用比率,可得到展現出所期望的導電率的釩酸鈣。又,為了將導電率調整至上述範圍內,亦可將展現出不同導電率的2種以上的釩酸鈣進行均勻地混合。
同樣地,若釩化合物(c)為釩酸鎂之情形時,可藉由將鎂化合物與釩酸鹽及/或五氧化釩在水中混合並使其反應而得。藉由該反應所得到之固體(通常為白色固體)因應所需亦可提供予水洗、脫水、乾燥、粉碎等的處理。
作為用於調製釩酸鎂的鎂化合物,可示例碳酸鎂、氫氧化鎂、氧化鎂、氯化鎂、硝酸鎂、乙酸鎂及硫酸鎂。進而甲酸鎂等的有機酸的鎂化合物也適合於使用。作為釩酸鹽,可示例釩酸鈣、釩酸鈉、釩酸銨,但並非限定於該等中。
即使是使鎂化合物與釩酸鹽及/或五氧化釩反應來調製釩酸鎂之情形時,亦可藉由調整鎂化合物與釩酸鹽及/或五氧化釩之使用比率,得到展現出所期望的導電率的釩酸鎂。又,為了將導電率調整至上述範圍內,亦可將展現出不同的導電率的2種以上的釩酸鎂進行均勻地混合。
第三磷酸鎂(d)係一般由「Mg3(PO4)2‧8H2O」所成,以8水合物的形式來市售。又,第三磷酸鎂(d)在酸性區域中具有高pH緩衝能力,例如圖4所表示般,藉由與上述釩化合物(c)併用,與僅使用上述釩化合物(c)相比時,酸性區域中之pH緩衝能力會格外地提高,其結果藉由將第三磷酸鎂(d)與上述釩化合物(c)併用,從而可發揮提升在酸性環境條件中之塗膜的耐蝕性的效果。於此,圖4係用於表示由作為釩化合物(c)之0.7質量%的釩酸鈣與0.3質量%的第三磷酸鎂(d)所成的水溶液、與作為釩化合物(c)之1.0質量%的釩酸鈣的水溶液在酸性區域中之pH緩衝作用。圖4所表示之pH緩衝作用的實驗方法係如下述般。
1.使用鹽酸或氫氧化鈉來調整水溶液的初期pH。
2.在已調整初期pH的水溶液中,添加1質量%的防鏽顏料並進行攪拌。
3.測定藉以上述「2.」所調製的防鏽顏料1質量%的水溶液在24小時後的pH。
圖4中,藉由使用水溶液調製後24時間的pH為在一點鏈線所表示的6.5~11的範圍內的防鏽顏料,在冷延鋼板或包含鋅或鋁的鍍敷鋼板之情形中,可得到顯示高耐蝕性的塗膜。因此,如圖4所表示般,與單獨使用釩酸鈣相比,在釩酸鈣中併用第三磷酸鎂之情形時,因為
在pH為3附近的酸性區域的緩衝作用高,由此可推斷具有使用包含釩酸鈣與第三磷酸鎂的塗膜組成物所成的塗膜的塗裝鋼板,在酸性環境條件下之耐蝕性為提升。
第三磷酸鎂(d)的含量,若使用上述8水合物之情形時,也是基於「Mg3(PO4)2」的質量來進行換算,相對於塗膜形成性樹脂(a)的固形分及交聯劑(b)的固形分的合計100質量%為1~150質量%。若未滿1質量%時,則第三磷酸鎂(d)從塗膜向鋼材1的溶出會變少,結果導致pH緩衝能力降低,在酸性環境條件下之耐蝕性為降低。又,若第三磷酸鎂(d)的含量超過150質量%時,則塗膜的透濕性變得過高,水容易過度浸入塗膜,塗膜的耐濕性會降低,隨著耐濕性之降低,在酸性環境條件下之耐蝕性亦會降低。
本發明中,考慮酸性區域中之pH緩衝能力而使用第三磷酸鎂(d)。於此,與第三磷酸鎂相比,第三磷酸鹼土金屬鹽之第三磷酸鈣之從塗膜向鋼材1的溶出為少,故即使是等量添加在酸性區域中之pH的緩衝能力亦為不足,其結果導致在酸性環境條件下的腐蝕性降低。又,第三磷酸鹼金屬鹽之第三磷酸鋰及第三磷酸鈉,係因塗膜的透濕性過高,水容易過度浸入塗膜,故塗膜的耐濕性會降低,隨著耐濕性之降低,耐蝕性亦會降低。又,磷酸鎂之中,與第一磷酸鎂(Mg(H2PO4)2‧4H2O)及第二磷酸鎂(MgHPO4‧3H2O)相比,水溶液中的pH呈鹼性的「第三磷酸鎂」在酸性區域的pH緩衝作用高,因而具
有使用包含第三磷酸鎂的塗裝組成物所成的塗膜的鋼材1在酸性環境條件下之耐蝕性為提升。
第三磷酸鎂(d)與釩化合物(c)的總含量,作為釩化合物(c)的質量與第三磷酸鎂(d)的「Mg3(PO4)2」的質量的合計質量,相對於塗膜形成性樹脂(a)的固形分及交聯劑(b)的固形分的合計100質量%為51~210質量%。藉由將第三磷酸鎂(d)與釩化合物(c)的總含量設為上述範圍內,則釩化合物(c)及第三磷酸鎂(d)從塗膜向鋼材1會適量溶出,因此可維持耐蝕性、且亦可維持塗膜的耐濕性。
釩化合物(c)與第三磷酸鎂(d)的質量比,將第三磷酸鎂(d)作為「Mg3(PO4)2」進行換算為60:150~150:1,較佳為60:50~150:50,又較佳為60:25。若釩化合物(c)與第三磷酸鎂(d)的質量比係將第三磷酸鎂(d)作為「Mg3(PO4)2」進行換算並藉由設為60:150~150:1,在酸性條件下的耐蝕性與通常的中性條件下的耐蝕性皆可成為良好。
本發明之塗料組成物係進而亦可含有選自由矽烷系偶合劑、鈦系偶合劑及鋯系偶合劑所成之群之至少1種的化合物來作為密著性提升成分。藉由密著性提升成分的添加,可使與被塗物的密著性提升,進一步可使塗膜的耐濕性提升。
作為上述密著性提升成分並無特別限制,可使用以往周知者。若舉出作為適合於使用的密著性提升成分的具體例,有Toray Dow Corning製的商品名「DOW CORNING TORAY Z-6011」、「DOW CORNING TORAY Z-6040」等的矽烷系偶合劑(於此,「DOW CORNING」為註冊商標);Matsumoto Fine Chemical製的商品名「OrgatixTC-401」、「OrgatixTC-750」等的鈦系偶合劑;Matsumoto Fine Chemical製的商品名「OrgatixZC-580」、「OrgatixZC-700」等的鋯系偶合劑,其中以矽烷系偶合劑為較佳使用。
密著性提升成分的含量,相對於塗膜形成性樹脂(a)及交聯劑(b)的合計固形分100質量%,以0.1~20質量%為較佳。藉由密著性提升成分的含量為0.1質量%以上,可得到耐濕性提升效果。又,藉由密著性提升成分的含量為20質量%以下,則塗料組成物的儲藏穩定性為良好。
本發明之塗料組成物進而亦可含有碳酸鈣、硫酸鋇、黏土、滑石、雲母、二氧化矽、氧化鋁及膨潤土等的體質顏料。藉由體質顏料的添加,因為可使塗膜強度提升,同時,在塗膜表面會產生凹凸,而與面塗塗膜的密著性為提升等的理由,則耐濕性會變得良好。相對於塗膜形成性樹脂(a)及交聯劑(b)的合計固形分100質量%,體質顏
料的含量以1~40質量%為較佳。藉由體質顏料的含量為1質量%以上,可得到耐濕性提升效果。又,藉由體質顏料的含量為40質量%以下,塗膜的透濕性為適當,而塗膜的耐濕性良好,耐蝕性亦為良好。
作為交聯劑(b)若使用封端聚異氰酸酯化合物(f)及/或聚異氰酸酯化合物之情形時,本發明之塗料組成物亦可含有硬化觸媒。作為硬化觸媒可舉例如錫觸媒、胺觸媒、鉛觸媒等,其中以有機錫化合物為較佳使用。作為有機錫化合物,可使用例如二月桂酸二丁基錫(DBTL)、二氧化二丁基錫、四-n-丁基-1,3-二乙醯氧基錫氧烷等。
又,作為交聯劑(b)即使是使用三聚氰胺樹脂(g1)之情形時,本發明之塗料組成物亦可含有硬化觸媒。作為此情形時的硬化觸媒,可舉例如羧酸、磺酸之類的酸觸媒等,其中以十二烷基苯磺酸、對甲苯磺酸等為較佳使用。
上述硬化觸媒的含量,相對於塗膜形成性樹脂(a)及交聯劑(b)的合計固形分100質量%,通常為0.1~10質量%,以0.1~1質量%為較佳。藉由硬化觸媒的含量為0.1~10質量%,塗料組成物的儲藏穩定性為良好。
本發明之塗料組成物因應所需亦可含有上述以外的其
他的添加劑。作為其他的添加劑,有例如上述釩化合物(c)以外的防鏽顏料;上述體質顏料以外的體質顏料;著色顏料、染料等的著色劑;光輝性顏料;溶劑;紫外線吸收劑(苯甲酮系紫外線吸收劑等);抗氧化劑(酚系、硫醚系、受阻胺系抗氧化劑等);可塑劑;表面調整劑(聚矽氧、有機高分子等);止垂流劑;增黏劑;蠟等的滑劑;顏料分散劑;顏料濕潤劑;調平劑;防分色劑;防沉澱劑;消泡劑;防腐劑;防凍劑;乳化劑;防霉劑;抗菌劑;穩定劑等。該等的添加劑可僅單獨使用1種,亦可併用2種以上。
作為上述釩化合物(c)以外的防鏽顏料,可使用非鉻系防鏽顏料,可舉例如五氧化釩、鉬酸鹽顏料(鉬酸鋅、鉬酸鍶等)、磷鉬酸鹽顏料(磷鉬酸鋁系顏料等)、鈣二氧化矽系顏料、三聚磷酸鹽等的磷酸鹽系防鏽顏料、矽酸鹽系防鏽顏料等的非鉻系防鏽顏料。該等可僅單獨使用1種,亦可併用2種以上。本發明之塗料組成物係因含有指定量的具有指定的導電率及pH的釩化合物(c),故展現充分高的耐蝕性,但因應所需在不損及所得到之塗膜的耐濕性、耐蝕性、耐藥品性等的範圍內,亦可使用如上述般的釩化合物(c)以外的防鏽顏料。
作為上述著色顏料,可舉例如二氧化鈦、碳黑、石墨、氧化鐵、煤塵等的無機著色顏料;酞青藍、酞青綠、喹吖酮、苝、蒽嘧啶、咔唑紫、蒽吡啶、偶氮橙、黃烷士酮(flavanthrone)黃、異吲哚啉黃、偶氮黃、陰
丹士林(indanthrone)藍、dibromo anza slon red、苝紅、偶氮紅、蒽醌紅等的有機著色顏料;鋁粉、氧化鋁粉、青銅粉、銅粉、錫粉、鋅粉、磷化鐵、微粒化鈦等。該等可僅單獨使用1種,亦可併用2種以上。
作為上述光輝性顏料,可舉例如鋁箔、青銅箔、錫箔、金箔、銀箔、鈦金屬箔、不鏽鋼箔、鎳‧銅等的合金箔、箔狀酞青藍等的箔顏料。該等可僅單獨使用1種,亦可併用2種以上。
作為上述溶劑,可舉例如:水;乙二醇單丁基醚(丁基溶纖劑)、二乙二醇單丁基醚、三乙二醇單乙基醚、丙二醇單甲基醚、丙二醇單乙基醚、丙二醇單丙基醚、二丙二醇單甲基醚、二丙二醇單乙基醚、丙二醇單甲基醚乙酸酯等的二醇系有機溶劑;甲醇、乙醇、異丙醇等的醇系有機溶劑;二噁烷、四氫呋喃等的醚系有機溶劑;3-甲氧基丁基乙酸酯、乙酸乙酯、乙酸異丙酯、乙酸丁酯等的酯系有機溶媒;甲基乙基酮、丙酮、甲基異丁基酮、環己酮、異佛酮等的酮系有機溶劑;以及N-甲基-2-吡咯啶酮、甲苯、戊烷、iso-戊烷、己烷、iso-己烷、環己烷、溶劑石油腦、礦油精、Solvesso 100、Solvesso 150(皆為芳香族烴系溶劑)等。該等可僅單獨使用1種,亦可併用2種以上。本發明之塗料組成物可以是水系塗料,亦可是有機溶劑系的塗料。
本發明之塗料組成物係可藉由將例如塗膜形成性樹脂(a)、交聯劑(b)及釩化合物(c)、體質顏
料、密著性提升成分、硬化觸媒及其他的添加劑,使用輥磨、球磨機、珠磨機、卵石磨機、沙磨機、瓶磨機、塗料搖擺器、分散型攪拌器等的混合機中進行混合從而調製。或本發明之塗料組成物係亦可由包含塗膜形成性樹脂(a)及釩化合物(c)的主劑成分、與交聯劑(b)的交聯劑成分所成的雙液型塗料。
本發明之塗料組成物係可適用於被稱為底層塗料的底塗塗料。此情形時,對於面塗塗料可使用聚酯樹脂系塗料、氟樹脂系塗料等周知的材料。
藉由本發明之塗料組成物所成之塗膜,如上述般,被形成在鋼材的指定的鍍敷層(簡言之,係包含Al、Zn、Si、Cr及Mg,且Mg含量為0.1~10質量%、Cr含量為0.02~1.0質量%、Si-Mg相為0.2~15體積%,相對於Mg全量,前述Si-Mg相中之Mg之質量比率為3%以上的鋁‧鋅合金鍍敷層)之上。據此,可得到與以往的鉻酸鹽處理為同等級以上的耐蝕性(特別是端部耐蝕性)經提高的表面處理鋼板。
作為本發明之塗料組成物的塗布方法,可採用輥塗布、真空噴塗、靜電噴塗、簾流動塗布等以往周知的方法。使用本發明之塗料組成物所形成的本發明的塗膜,係將塗料組成物塗布在鋼材1的鍍敷層後,藉由進行加熱被塗物的焙燒處理而可形成。據此,可得到本發明的
表面處理鋼材。尚,焙燒溫度通常為180~250℃,焙燒時間通常為10~200秒。
使用本發明之塗料組成物所得到之塗膜(本發明的塗膜)的膜厚(乾燥膜厚)通常為1~30μm,較佳為1~10μm。
本發明的塗膜,係因形成此者的塗料組成物含有指定量的具有指定的導電率的釩化合物(c),故通常顯示105~1012Ω‧cm2的濕潤電阻值。雖然會因為塗料組成物中使用的樹脂或交聯劑的種類、含有的添加劑的種類與量、焙燒條件等,而塗膜的濕潤電阻值會變動,但大致而言若塗膜的濕潤電阻值在上述範圍內時,意味著塗膜具有適度的透濕性,相反地亦展現出良好的耐濕性。即,若濕潤電阻值未滿105Ω‧cm2時,則意味著塗膜的透濕性過高、且耐濕性低,因此,有容易產生膨脹或剝離等的傾向。又,濕潤電阻值若超過1012Ω‧cm2,則意味著塗膜的透濕性過低,塗膜中之防鏽顏料的溶出受到阻礙而有耐蝕性降低的傾向。本發明的塗膜的濕潤電阻值係較佳為106~1011Ω‧cm2。尚,所謂塗膜的濕潤電阻值,係指將乾燥塗膜厚15μm的塗膜,在5%食鹽水(NaCl水溶液)中藉以35℃下使其濕潤1小時後,外加電壓的波高±0.5V所測定的直流電阻值。對於塗膜的濕潤電阻值測定之詳細條件係在後述的實施例中描述。
本發明人發現,藉由組合本發明相關的鍍敷層與塗膜,可得到與以往的鉻酸鹽處理為同等級以上的耐蝕性(特別是端部耐蝕性),故進而創作本發明。表示實施例及比較例並對於該效果進行更具體的說明。但,本發明並非被限定於以下之實施例中。下述實施例中,「份」及「%」只要未特意言及係質量基準。
藉由使鋼板浸漬於熔融金屬中從而形成鍍敷層。實施例1~2、實施例5~18、比較例4~13及參考例1中,以可得到55%Al-2%Mg-1.6%Si-0.03%Cr-鋅合金鍍敷鋼板之方式來調整熔融金屬的成分。實施例3中,以可得到55%Al-0.5%Mg-1.6%Si-0.03%Cr-鋅合金鍍敷鋼板之方式來調整熔融金屬的成分。實施例4中,以可得到55%Al-5%Mg-1.6%Si-0.03%Cr-鋅合金鍍敷鋼板之方式來調整熔融金屬的成分。比較例1中,以可得到55%Al-11%Mg-1.6%Si-0.03%Cr-鋅合金鍍敷鋼板之方式來調整熔融金屬的成分。比較例14中,以可得到55%Al-2%Mg-1.6%Si-0.01%Cr-鋅合金鍍敷鋼板之方式來調整熔融金屬的成分。比較例15中,以可得到55%Al-2%Mg-1.6%Si-1.1%Cr-鋅合金鍍敷鋼板之方式來調整熔融金屬的成分。比較例2及參考例2中,以可得到55%Al-1.6%Si-鋅合金鍍敷鋼板之方式來調整熔融金屬的成分。比較例3中,以可得到熔融鋅鍍敷鋼板之方式來調整熔融金屬的成分。
作為釩酸鹼土金屬鹽係使用釩酸鈣。釩酸鈣係如下述般來進行調整。
將碳酸鈣(CaCO3)622g、與五氧化釩(V2O5)378g添加在水10L中,昇溫至60℃後,以相同溫度下攪拌2小時。將所得到之反應生成物(白色固體)進行水洗後脫水,並藉以100℃進行乾燥後,藉由粉碎從而可得到釩酸鈣。
〔i〕在利用離子交換水洗淨的聚乙烯製細口瓶中,添加離子交換水99g及試樣1g。
〔ii〕投入利用離子交換水洗淨的攪拌子(stirrer chip),並在室溫下攪拌4小時。
〔iii〕攪拌後,使用導電度計(東亞DKK製導電率計「CM-30ET」)及pH計(堀場製作所製「F-54」)來測定導電率及pH。
除了釩酸鈣以外之其他的防鏽顏料之詳細係如下述般。
1.「偏釩酸鈉」:市售試劑
2.「五氧化釩」:市售試劑
3.「SHIELDEX C303」:GRACE JAPAN製、鈣離子
交換二氧化矽微粒子
4.「第三磷酸鎂」:市售試劑
5.「第一磷酸鎂」:市售試劑
6.「第二磷酸鎂」:市售試劑
7.「第三磷酸鈣」:市售試劑
8.「釩酸鎂」:市售試劑
9.「鉻酸鍶」:strontium chromate:Kikuchicolor公司製
依據表1~表4所表示之調配組成來調製塗料組成物。
表1~表4所表示之各種調配成分之詳細係如下述般。
(1)「沈降性硫酸鋇B-55」:堺化學工業製、沈降性硫酸鋇。
(2)「黏土1號」:丸尾CALCIUM製、黏土。
(3)「Yunigurosu1000」丸尾CALCIUM製、碳酸鈣
(4)「滑石SSS」日本滑石製、滑石
(5)「GASIL HP260」INEOS SILICAS製、二氧化矽粉(v)「DBTL」:日東化成製、「TVS Tin Lau」〔二月桂酸二丁基錫、不揮發分:100%〕。
將厚度0.35mm的鋁鋅鍍敷鋼板進行鹼脫脂後,藉由將NIPPON PAINT SURF CHEMICALS製的有機無機複合處理劑「Surf Coat EC2310」塗布在鋼板表面及背面,並施予非鉻酸鹽化學轉化處理且進行乾燥。接著,在所得到之鋼板的背面上,以乾燥塗膜成為7μm之方式來塗布上述所得到之塗料組成物,並藉以最高到達溫度180℃進行30秒鐘焙燒,從而形成背面塗膜。接著,以乾燥塗膜成為5μm之方式來塗布實施例1~18、比較例1~13中任一之塗料組成物於鋼板的表面上,並藉以最高到達溫度200℃進行30秒鐘焙燒,從而形成表面底塗塗膜。進而,在上述底塗塗膜上,以乾燥塗膜成為10μm之方式來塗布日本Nipponpaint Industrial Coatings製的聚酯系面塗塗料
「NSC300HQ」,並藉以最高到達溫度210℃進行40秒鐘焙燒,從而形成表面面塗塗膜,而得到塗裝鋼板。又,關於參考例1、2,作為化學轉化處理係以使用NIPPON PAINT SURF CHEMICALS製的「NRC300」來施予鉻酸鹽處理,並以同條件下將含有鉻酸鍶之該底塗塗料及面塗塗料進行塗布、焙燒乾燥。
接著,對於所表示之項目<1>~<8>進行表面處理鋼板之評估試驗。將結果合併表示於表5~表8中。
將上述所得到之各表面處理鋼板切斷成5cm×10cm,將所得到之試片在95℃以上的沸騰水中浸漬5小時後,取出並依據ASTM D714-56來評估表面側的塗裝外觀(平面部份膨脹評估)。ASTM D714-56係將各膨脹的大小(平均徑)和密度,與標準判定照片進行比對並進行評估,來表示等級記號。膨脹的大小和密度係以分級為各4個等級,依以下的表9中之組合以滿分為5分的分數來實施評估。
無異常:5
又,對於在95℃以上的沸騰水中浸漬5小時後的試片,進行棋盤格膠帶附著試驗(棋盤格密著性試驗)並進行評估。棋盤格膠帶附著試驗係根據JISK-5400 8.5.2(1990)棋盤格膠帶法,將切口的隙間間隔設為1mm並做出100個棋盤格,在其表面上使玻璃紙製黏著膠帶密著,並調查快速地剝離時在塗面上殘留的棋盤格的數量。
將上述所得到之各表面處理鋼板切斷成5cm×10cm,將所得到之試片在5%濃度的苛性蘇打水溶液中浸漬24小時後,取出並利用自來水洗淨,依據ASTM D714-56將表面側的塗裝外觀進行平面部份膨脹之評估。關於該評估,係對照於耐沸騰水性試驗中所使用的上述表9,並以滿分5分來進行計分。
對於各實施例及比較例之樣品,係以寬7cm、長15cm的尺寸來進行裁斷。此時,交互進行從表面之切斷與從背面之切斷,製作了在各試片的截面上具有上毛邊(由背面切斷)、下毛邊(由表面切斷)之兩者之試片,並藉以聚酯膠帶來密封塗裝鋼板的上端及下端部。對於該試驗樣品,藉由JIS K 5400 9.1所規定之試驗方法來進行鹽水噴霧試驗1000小時,並對於平面部份的塗膜及裁切部來觀察白鏽、發泡之產生狀況。關於平面部份的鏽‧膨脹係依據ASTM D714-56來進行評估,同時,對照於耐沸騰水性試驗中所使用的上述表9,並以滿分5分來進行計分;關於端部的鏽‧膨脹係以任意的5處來計測其劣化寬度,並依下述之基準來計分平均值。
◎:2mm以下、○:4mm以下、△:6mm以下、×:超過6mm
對於各實施例及比較例之樣品,進行2T加工(夾著2片鋼板並用虎嘴箝將各樣品彎曲180度之加工),藉由實施上述之鹽水噴霧試驗,觀察在彎曲部分中之白鏽之產生狀況,並對照於上述表9後以滿分5分來進行計分。
如表3及表7之比較例2所表示般,將本案發明之塗料組成物塗布在熔融55%鋁-1.6%矽-鋅合金鍍敷鋼板時,平面部份中之膨脹評估係與參考例1及2為相同高之評估,但端部耐蝕性之評估為×。又,如比較例3所表示般,將本案發明之塗料組成物塗布在熔融鋅鍍敷鋼板時,平面部份中之膨脹評估係與參考例1及2為相同高之評估,但端部耐蝕性之評估為△。另一方面,本案發明之實施例中,不僅只平面部份中之膨脹評估,連端部耐蝕性亦與參考例1及2為相同高之評估。亦即,雖然機制尚不明確,但可得知本案發明之表面處理鋼板係具備與施予鉻酸鹽處理的鍍敷鋼板為同等級以上的高的端部耐蝕性。尚,比較例15係具備與實施例相同的高的耐蝕性,但因為喪失塗膜之平滑性,故為本發明之範圍外。此係認為是,因Cr的過量添加而導致在浴中產生浮渣之緣故。
將上述所得到之各表面處理鋼板切斷成5cm×10cm,對於所得到之試片藉由測定鉛筆硬度來評估耐擦傷性。根據JIS-K 5400的8.4.1(1993)之方法,用改變鉛筆芯的硬度時塗膜的破裂來調查塗膜之刮痕抵抗性,將未發現塗
膜破裂時的最高硬度作為其塗膜的鉛筆硬度。
根據JIS G3322:2012的14.2.2彎曲試驗所規定之方法施予180度密著彎曲後,在加工部使用玻璃紙製黏著膠帶來將塗膜表面進行壓黏後拉開膠帶,並觀察塗膜的剝離狀態。若未發現塗膜的剝離時,於密著彎曲時夾著相同板厚的鍍敷鋼板並再次進行180度彎曲,重覆進行膠帶剝離評估,將未產生塗膜剝離的夾持板的片數作為評估要點(例如2片時標記為2TT)。
根據JIS G3322:2012的14.2.4衝撃試驗所規定之方法,從50cm的高度使500g的重物落下至試驗面,之後使用玻璃紙製黏著膠帶將塗膜表面進行壓黏並朝鉛垂方向拉起,利用目視來觀察塗膜的剝離面積,依下述之基準以滿分5分來進行計分。
5:未剝離 4:10%以下 3:20%以下 2:50%以下 1:超過50%的剝離
根據JIS G3322:2012的14.2.5棋盤格試驗所規定之
方法,以1mm寬的裁切來製作100個方格目,使用玻璃紙製黏著膠帶將塗膜表面進行壓黏並朝鉛垂方向拉起,計算未產生剝離的方格目來作為評估。
Claims (14)
- 一種表面處理鋼材,其係在鋼材的表面上隔著至少包含鋁‧鋅合金鍍敷層的底層來形成塗膜,其特徵在於:前述鋁‧鋅合金鍍敷層係包含作為構成元素之Al、Zn、Si、Cr及Mg,且Mg含量為0.1~10質量%、Cr含量為0.02~1.0質量%,前述鋁‧鋅合金鍍敷層係包含0.2~15體積%的Si-Mg相,相對於Mg全量,前述Si-Mg相中之Mg之質量比率為3%以上,前述塗膜係含有塗膜形成性樹脂(a)、交聯劑(b)、選自由釩酸鹼土金屬鹽及釩酸鎂所成之群之至少1種的釩化合物(c)、與第三磷酸鎂(d),前述釩化合物(c)係1質量%水溶液在溫度25℃下的導電率為200μS/cm~2,000μS/cm的化合物,且相對於前述塗膜形成性樹脂(a)及前述交聯劑(b)的合計100質量%,前述釩化合物(c)的含量為超過50質量%且在150質量%以下,前述釩化合物(c)係其1質量%水溶液的pH為6.5~11,相對於前述塗膜形成性樹脂(a)及前述交聯劑(b)的合計100質量%,前述第三磷酸鎂(d)的含量為3~150質量%。
- 如請求項1之表面處理鋼材,其中,前述塗膜係進而含有選自由碳酸鈣、硫酸鋇、黏土、滑石、雲母、二氧化 矽、氧化鋁及膨潤土所成之群之至少1種的體質顏料(e),相對於前述塗膜形成性樹脂(a)及前述交聯劑(b)的合計100質量%,前述體質顏料(e)的含量為1~40質量%。
- 如請求項1或2之表面處理鋼材,其中,前述塗膜形成性樹脂(a)係包含選自由數平均分子量為2,000~10,000、且玻璃轉移溫度為60~120℃之含羥基之環氧樹脂,及數平均分子量為2,000~30,000、且玻璃轉移溫度為0~80℃之含羥基之聚酯樹脂所成之群之至少1種。
- 如請求項1~3中任一項之表面處理鋼材,其中,前述交聯劑(b)係包含選自由將聚異氰酸酯化合物的異氰酸酯基以含活性氫之化合物封端所得之封端聚異氰酸酯化合物(f),及在1個分子中平均具有1個以上的羥甲基或亞胺基之胺基樹脂(g)所成之群之至少1種,相對於前述塗膜形成性樹脂(a)100質量%,前述交聯劑(b)的含量為10~80質量%。
- 如請求項4之表面處理鋼材,其中,前述聚異氰酸酯化合物係芳香族聚異氰酸酯化合物。
- 如請求項1~5中任一項之表面處理鋼材,其中,前述塗料組成物係進而含有選自由矽烷系偶合劑、鈦系偶合劑 及鋯系偶合劑所成之群之至少1種的偶合劑(h),相對於前述塗膜形成性樹脂(a)及前述交聯劑(b)的合計100質量%,前述偶合劑(h)的含量為0.1~20質量%。
- 如請求項1~6中任一項之表面處理鋼材,其中,將乾燥塗膜厚15μm的塗膜在35℃的5%食鹽水中濕潤1小時後,作為該塗膜的直流電阻值之濕潤電阻值為105~1012Ω‧cm2。
- 如請求項1~7中任一項之表面處理鋼材,其中,在前述鋁‧鋅合金鍍敷層中之50nm深度的最外層內,大小為直徑4mm、深度50nm的任意區域中,Mg含量為未滿60質量%。
- 如請求項1~8中任一項之表面處理鋼材,其中,在前述鋁‧鋅合金鍍敷層中之50nm深度的最外層內,Cr含量為100~500質量ppm的範圍。
- 如請求項1~9中任一項之表面處理鋼材,其中,在前述鋁‧鋅合金鍍敷層與前述鋼材之間係中介存在含Al與Cr之合金層,相對於前述鋁‧鋅合金鍍敷層內之Cr的質量比例,該合金層中的Cr的質量比例之比為2~50的範圍。
- 如請求項1~10中任一項之表面處理鋼材,其中,前述鋁‧鋅合金鍍敷層的表面中之Si-Mg相的比例,依面積比率計算為30%以下。
- 如請求項1~11中任一項之表面處理鋼材,其中,前述鋁‧鋅合金鍍敷層中:Al的含量為25~75質量%,相對於Al,Si的含量為0.5~10質量%,且Si:Mg的質量比為100:50~100:300。
- 如請求項1~12中任一項之表面處理鋼材,其中,前述鋁‧鋅合金鍍敷層係進而包含作為構成元素之1~1000質量ppm的Sr。
- 如請求項1~13中任一項之表面處理鋼材,其中,前述鋁‧鋅合金鍍敷層係進而含有0.0005~0.1質量%範圍的作為構成元素的由Ti及B中之至少一方所成之成分。
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JP5547376B2 (ja) | 2008-03-19 | 2014-07-09 | 関西ペイント株式会社 | 防錆塗料組成物 |
ES2657614T3 (es) * | 2010-02-18 | 2018-03-06 | Nippon Steel & Sumikin Coated Sheet Corporation | Material de acero metalizado por inmersión en caliente y método para producir el mismo |
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JP5814941B2 (ja) | 2010-12-22 | 2015-11-17 | 関西ペイント株式会社 | 耐食性に優れる塗料組成物 |
MY166355A (en) | 2011-08-24 | 2018-06-25 | Nippon Steel & Sumitomo Metal Corp | Surface-treated hot-dip plated steel |
JP5732672B2 (ja) | 2011-09-21 | 2015-06-10 | 日本ペイント株式会社 | 塗料組成物、塗膜、及び塗装鋼板 |
JP5341270B1 (ja) | 2012-04-25 | 2013-11-13 | 日新製鋼株式会社 | 黒色めっき鋼板の製造方法および黒色めっき鋼板の成形体の製造方法 |
WO2015012290A1 (ja) | 2013-07-25 | 2015-01-29 | 日本ファインコーティングス株式会社 | 塗料組成物、塗膜、および塗装鋼板 |
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2016
- 2016-04-26 JP JP2016088071A patent/JP6087461B1/ja active Active
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2017
- 2017-03-07 US US15/766,639 patent/US11136659B2/en active Active
- 2017-03-07 CA CA3005266A patent/CA3005266C/en active Active
- 2017-03-07 CN CN201780002354.1A patent/CN108026648A/zh active Pending
- 2017-03-07 MX MX2018009384A patent/MX2018009384A/es unknown
- 2017-03-07 WO PCT/JP2017/009035 patent/WO2017187799A1/ja active Application Filing
- 2017-03-07 KR KR1020177037903A patent/KR101868530B1/ko active IP Right Grant
- 2017-03-07 NZ NZ741908A patent/NZ741908A/en unknown
- 2017-03-07 EP EP17789088.6A patent/EP3354772B1/en active Active
- 2017-03-07 SG SG11201801742XA patent/SG11201801742XA/en unknown
- 2017-03-07 ES ES17789088T patent/ES2850627T3/es active Active
- 2017-03-07 AU AU2017257044A patent/AU2017257044B2/en active Active
- 2017-03-07 MY MYPI2018700831A patent/MY172928A/en unknown
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
TWI701358B (zh) * | 2018-03-29 | 2020-08-11 | 日商神戶製鋼所股份有限公司 | 塗裝鋅鍍敷鋼板 |
Also Published As
Publication number | Publication date |
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CA3005266C (en) | 2018-11-27 |
NZ741908A (en) | 2019-07-26 |
EP3354772B1 (en) | 2020-12-30 |
TWI737701B (zh) | 2021-09-01 |
US11136659B2 (en) | 2021-10-05 |
CA3005266A1 (en) | 2017-11-02 |
EP3354772A1 (en) | 2018-08-01 |
KR20180025877A (ko) | 2018-03-09 |
JP6087461B1 (ja) | 2017-03-01 |
EP3354772A4 (en) | 2019-09-25 |
US20180305802A1 (en) | 2018-10-25 |
KR101868530B1 (ko) | 2018-06-19 |
SG11201801742XA (en) | 2018-04-27 |
PH12018500849B1 (en) | 2018-11-05 |
PH12018500849A1 (en) | 2018-11-05 |
ES2850627T3 (es) | 2021-08-31 |
JP2017197795A (ja) | 2017-11-02 |
AU2017257044B2 (en) | 2019-02-07 |
WO2017187799A1 (ja) | 2017-11-02 |
CN108026648A (zh) | 2018-05-11 |
AU2017257044A1 (en) | 2018-05-24 |
MX2018009384A (es) | 2018-09-05 |
MY172928A (en) | 2019-12-14 |
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