JP4733643B2 - マグネシウム豊富被覆剤および被覆系 - Google Patents
マグネシウム豊富被覆剤および被覆系 Download PDFInfo
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- JP4733643B2 JP4733643B2 JP2006539495A JP2006539495A JP4733643B2 JP 4733643 B2 JP4733643 B2 JP 4733643B2 JP 2006539495 A JP2006539495 A JP 2006539495A JP 2006539495 A JP2006539495 A JP 2006539495A JP 4733643 B2 JP4733643 B2 JP 4733643B2
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- Prior art keywords
- magnesium
- coating
- powder
- metal
- corrosion
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- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 title claims abstract description 120
- 238000000576 coating method Methods 0.000 title claims abstract description 103
- 239000011248 coating agent Substances 0.000 title claims abstract description 77
- 239000011777 magnesium Substances 0.000 title claims description 155
- 229910052749 magnesium Inorganic materials 0.000 title claims description 77
- 229910052751 metal Inorganic materials 0.000 claims abstract description 97
- 239000002184 metal Substances 0.000 claims abstract description 97
- 230000007797 corrosion Effects 0.000 claims abstract description 65
- 238000005260 corrosion Methods 0.000 claims abstract description 65
- 238000000034 method Methods 0.000 claims abstract description 62
- 239000011230 binding agent Substances 0.000 claims abstract description 47
- 229920000642 polymer Polymers 0.000 claims abstract description 37
- 229910000077 silane Inorganic materials 0.000 claims abstract description 21
- -1 silane modified epoxy isocyanate Chemical class 0.000 claims abstract description 17
- 239000008199 coating composition Substances 0.000 claims abstract description 15
- 239000002245 particle Substances 0.000 claims description 95
- 239000000843 powder Substances 0.000 claims description 69
- 239000000203 mixture Substances 0.000 claims description 47
- 229920001228 polyisocyanate Polymers 0.000 claims description 32
- 239000005056 polyisocyanate Substances 0.000 claims description 32
- 239000004593 Epoxy Substances 0.000 claims description 29
- 229910000838 Al alloy Inorganic materials 0.000 claims description 23
- 229910052782 aluminium Inorganic materials 0.000 claims description 23
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 22
- 238000009826 distribution Methods 0.000 claims description 22
- 150000001282 organosilanes Chemical class 0.000 claims description 22
- 150000001412 amines Chemical class 0.000 claims description 21
- 239000000049 pigment Substances 0.000 claims description 19
- 229910000861 Mg alloy Inorganic materials 0.000 claims description 14
- 229910052748 manganese Inorganic materials 0.000 claims description 5
- 239000011572 manganese Substances 0.000 claims description 5
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 2
- 229910045601 alloy Inorganic materials 0.000 abstract description 17
- 239000000956 alloy Substances 0.000 abstract description 17
- 229910000547 2024-T3 aluminium alloy Inorganic materials 0.000 abstract description 2
- 239000002987 primer (paints) Substances 0.000 description 45
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 28
- 239000000243 solution Substances 0.000 description 28
- 239000000463 material Substances 0.000 description 23
- 238000012360 testing method Methods 0.000 description 20
- 150000002739 metals Chemical class 0.000 description 19
- 239000011159 matrix material Substances 0.000 description 18
- 238000006243 chemical reaction Methods 0.000 description 15
- 238000009472 formulation Methods 0.000 description 14
- 239000011780 sodium chloride Substances 0.000 description 14
- 238000000157 electrochemical-induced impedance spectroscopy Methods 0.000 description 13
- 150000003839 salts Chemical class 0.000 description 13
- 229910052684 Cerium Inorganic materials 0.000 description 12
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 12
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 12
- 229910052757 nitrogen Inorganic materials 0.000 description 12
- 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 11
- 239000004971 Cross linker Substances 0.000 description 11
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 11
- 238000002360 preparation method Methods 0.000 description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 11
- ZCDOYSPFYFSLEW-UHFFFAOYSA-N chromate(2-) Chemical compound [O-][Cr]([O-])(=O)=O ZCDOYSPFYFSLEW-UHFFFAOYSA-N 0.000 description 10
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 10
- 239000012948 isocyanate Substances 0.000 description 10
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- 239000000758 substrate Substances 0.000 description 9
- 229910052802 copper Inorganic materials 0.000 description 8
- 239000010949 copper Substances 0.000 description 8
- 239000003431 cross linking reagent Substances 0.000 description 8
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 description 8
- 229920000647 polyepoxide Polymers 0.000 description 8
- 239000000047 product Substances 0.000 description 8
- YRIZYWQGELRKNT-UHFFFAOYSA-N 1,3,5-trichloro-1,3,5-triazinane-2,4,6-trione Chemical compound ClN1C(=O)N(Cl)C(=O)N(Cl)C1=O YRIZYWQGELRKNT-UHFFFAOYSA-N 0.000 description 7
- 229920002396 Polyurea Polymers 0.000 description 7
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 7
- 239000002585 base Substances 0.000 description 7
- 239000003822 epoxy resin Substances 0.000 description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 6
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 6
- 125000001931 aliphatic group Chemical group 0.000 description 6
- 125000003118 aryl group Chemical group 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 6
- 230000007613 environmental effect Effects 0.000 description 6
- 238000007654 immersion Methods 0.000 description 6
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- 229910052760 oxygen Inorganic materials 0.000 description 6
- 239000001301 oxygen Substances 0.000 description 6
- 238000005507 spraying Methods 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 239000011701 zinc Substances 0.000 description 6
- 229910052725 zinc Inorganic materials 0.000 description 6
- FSNCEEGOMTYXKY-JTQLQIEISA-N Lycoperodine 1 Natural products N1C2=CC=CC=C2C2=C1CN[C@H](C(=O)O)C2 FSNCEEGOMTYXKY-JTQLQIEISA-N 0.000 description 5
- 229910000831 Steel Inorganic materials 0.000 description 5
- 230000002378 acidificating effect Effects 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 5
- 229920001688 coating polymer Polymers 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- BHXIWUJLHYHGSJ-UHFFFAOYSA-N ethyl 3-ethoxypropanoate Chemical compound CCOCCC(=O)OCC BHXIWUJLHYHGSJ-UHFFFAOYSA-N 0.000 description 5
- 229910052930 hexahydrite Inorganic materials 0.000 description 5
- 230000001976 improved effect Effects 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 5
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 5
- 239000000347 magnesium hydroxide Substances 0.000 description 5
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 5
- 238000005259 measurement Methods 0.000 description 5
- 230000007935 neutral effect Effects 0.000 description 5
- 238000006116 polymerization reaction Methods 0.000 description 5
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical compound [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 description 5
- 239000010959 steel Substances 0.000 description 5
- KUBDPQJOLOUJRM-UHFFFAOYSA-N 2-(chloromethyl)oxirane;4-[2-(4-hydroxyphenyl)propan-2-yl]phenol Chemical compound ClCC1CO1.C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 KUBDPQJOLOUJRM-UHFFFAOYSA-N 0.000 description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 4
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- PXKLMJQFEQBVLD-UHFFFAOYSA-N bisphenol F Chemical compound C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 0.000 description 4
- 229910052599 brucite Inorganic materials 0.000 description 4
- 230000001680 brushing effect Effects 0.000 description 4
- 239000011651 chromium Substances 0.000 description 4
- 238000004132 cross linking Methods 0.000 description 4
- 238000007598 dipping method Methods 0.000 description 4
- 239000003792 electrolyte Substances 0.000 description 4
- 239000006260 foam Substances 0.000 description 4
- 229910052742 iron Inorganic materials 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 230000007246 mechanism Effects 0.000 description 4
- 229910001092 metal group alloy Inorganic materials 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
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- 238000007254 oxidation reaction Methods 0.000 description 4
- 229910052761 rare earth metal Inorganic materials 0.000 description 4
- 150000002910 rare earth metals Chemical class 0.000 description 4
- 102200082881 rs33936254 Human genes 0.000 description 4
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- 239000007858 starting material Substances 0.000 description 4
- 125000004665 trialkylsilyl group Chemical group 0.000 description 4
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- CHTHLHKDMPRBFZ-UHFFFAOYSA-N 1,2,3,4-tetrahydroquinoxalin-2-ol Chemical class C1=CC=C2NC(O)CNC2=C1 CHTHLHKDMPRBFZ-UHFFFAOYSA-N 0.000 description 3
- XCZKKZXWDBOGPA-UHFFFAOYSA-N 2-phenylbenzene-1,4-diol Chemical compound OC1=CC=C(O)C(C=2C=CC=CC=2)=C1 XCZKKZXWDBOGPA-UHFFFAOYSA-N 0.000 description 3
- 229910002012 Aerosil® Inorganic materials 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 125000003545 alkoxy group Chemical group 0.000 description 3
- 238000005275 alloying Methods 0.000 description 3
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 3
- 229910052791 calcium Inorganic materials 0.000 description 3
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- 150000002170 ethers Chemical class 0.000 description 3
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 3
- 230000007062 hydrolysis Effects 0.000 description 3
- 238000006460 hydrolysis reaction Methods 0.000 description 3
- 229910052744 lithium Inorganic materials 0.000 description 3
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 3
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- 125000003161 (C1-C6) alkylene group Chemical group 0.000 description 2
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- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 2
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- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 description 2
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- 231100000315 carcinogenic Toxicity 0.000 description 2
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- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 description 2
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- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 2
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- 239000003063 flame retardant Substances 0.000 description 2
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- ZFSLODLOARCGLH-UHFFFAOYSA-N isocyanuric acid Chemical compound OC1=NC(O)=NC(O)=N1 ZFSLODLOARCGLH-UHFFFAOYSA-N 0.000 description 2
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- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 2
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- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 description 2
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- KJAMZCVTJDTESW-UHFFFAOYSA-N tiracizine Chemical compound C1CC2=CC=CC=C2N(C(=O)CN(C)C)C2=CC(NC(=O)OCC)=CC=C21 KJAMZCVTJDTESW-UHFFFAOYSA-N 0.000 description 2
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- QTWJRLJHJPIABL-UHFFFAOYSA-N 2-methylphenol;3-methylphenol;4-methylphenol Chemical compound CC1=CC=C(O)C=C1.CC1=CC=CC(O)=C1.CC1=CC=CC=C1O QTWJRLJHJPIABL-UHFFFAOYSA-N 0.000 description 1
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- MIFGCULLADMRTF-UHFFFAOYSA-N 4-[(4-hydroxy-3-methylphenyl)methyl]-2-methylphenol Chemical compound C1=C(O)C(C)=CC(CC=2C=C(C)C(O)=CC=2)=C1 MIFGCULLADMRTF-UHFFFAOYSA-N 0.000 description 1
- FAUAZXVRLVIARB-UHFFFAOYSA-N 4-[[4-[bis(oxiran-2-ylmethyl)amino]phenyl]methyl]-n,n-bis(oxiran-2-ylmethyl)aniline Chemical compound C1OC1CN(C=1C=CC(CC=2C=CC(=CC=2)N(CC2OC2)CC2OC2)=CC=1)CC1CO1 FAUAZXVRLVIARB-UHFFFAOYSA-N 0.000 description 1
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Description
A.開路電位および電気化学インピーダンス分光EIS検討
まず、我々の研究所で配合したMg豊富プライマー(トップコートなし)の電気化学的検討を、3%NaCl溶液に浸漬した下塗りAl 2024 T−3合金の表面で行った。合金に接触している被膜に関して、腐食電位Ecorr、または開路電位(OCP)を監視し、エポキシ−ポリアミドポリマーマトリックスにおいて配合した3つのプライマーの組の(EIS)スペクトルを、時間の関数として記録した。OCPは、腐食反応が反応系の負極と正極の間に生じている際に得られる混合電位である。図2Aおよび2Bに示されているデータは、43、46および50%PVC(顔料容積濃度)におけるEckart(Eckagranules(商標))約50ミクロン(μm)平均粒径分布(PSD)Mg粉末に基づく3つのこれらのプライマーに関する。これらのデータは、プライマーだけからの最も有効な保護が約46%PVCであることを示し、これは、この系の推定CPVC(臨界顔料容積濃度)であった。
金属豊富被覆剤において、顔料容積濃度(PVC)は、透水性および凝集強度のような塗料特性が劇的に変化する領域において、高くかつ臨界PVCに近い。従って、トップコートなしの、希薄ハリソン溶液におけるProhesion(商標)繰返し暴露が、酸性電解質、空中酸素、CO2および水の、被膜Mg負極への容易接近を可能にする。Mg豊富プライマーを上塗りすることは、Prohesion(商標)の主な繰返し作用からプライマーを絶縁するかまたは遮蔽し、それにより、Al合金が酸性雨環境に暴露された場合に被膜にかき傷が付いたり隙間ができたりする過程が観察されるのを防止する。このような過程の発生をより良く観察するために、下塗りしたパネルをトップコートなしに、希薄ハリソン溶液へ直接的に暴露し、監視した。希薄ハリソン溶液のpHは約4.5であり、これは、Mg金属がCO2、SO4 2-およびOH-と容易に塩を形成するpHに対応する。これらの塩の形成は、3つの明確な事象に対応する所定時間間隔で、プライマーの表面および界面に発生することが観察された:
これらの極めて期待の持てる結果が、最適化努力を行わずに、市販(OTS)ポリマー系に基づく簡単なMg豊富被覆剤から得られた。それらの結果は、実際の系が野外暴露において遭遇し得る極めて一般的な暴露環境における、Mg顔料の酸化生成物が、Al 2024 T−3合金の塩基性(basic)腐食を生じなかったことを示している。さらに、Mg豊富系は、Al 2024 T−3に正極防食も与え、前処理においてクロメートを使用せず、かつプライマーにおいてクロメート顔料を使用しない完全にCr不含の系における有意な防食特性を与えた。われわれは、被覆ポリマー系を向上させるための検討も行い、さらに配合物検討も行った。これらの検討を実施例2に記載する。
A.被覆ポリマーの選択
一般に、二液型亜鉛エポキシ/ポリアミド高分子材料は、高い付着性および耐アルカリ性を有する架橋マトリックスを生じ、それによって亜鉛を含むいかなるアルカリ性反応も結合剤自体に影響を及ぼさないので、鋼の正極防食に使用されている(参照により本明細書に組み込まれる、Van Vliet,Prog.Organic Coatings,34:220−226(1998))。最近、エポキシ、エポキシアクリルおよびポリウレタン被覆剤と比較してかなり向上したエポキシシロキサン「ハイブリッド」被覆剤が報告されている(参照により本明細書に組み込まれる、Keijman,High Solids Coatings:Experience in Europe and USA − Paper 40,Proceedings PCE Conference,The Hague,The Netherlands 「Protecting industrial and marine structures with coatings」,March 1977)。高性能プライマー用のハイブリッドポリマーマトリックスは、少なくとも2つの異なるメカニズム下に架橋および網目形成に参加し得る少なくとも2種類の反応基を有するポリマー主鎖を含有する高分子複合材料または合金として設計される。
Mg豊富被覆剤用の向上したポリマーマトリックスの設計は、Al合金表面の最小限の調製を必要とし、かつ既存のゾル−ゲル技術から誘導される、調製容易多層法を含む。反応法は、オルガノシラン(N−β−(アミノエチル)−γ−アミノプロピルトリメトキシシラン)の初期塗布、次に、新規シラン改質架橋剤を使用することによって、表面からの有機層をバルクにグラフトすることを含む。被覆法は、「ゾル−ゲル」法に類似しているが、多層スキームを含み、該多層スキームはオルガノシラン基材処理を使用し、その処理により、湿分硬化ポリイソシアネートを適用し、該ポリイソシアネートは水との初期反応に関与して不安定カルバミン酸中間体を形成すると考えられ、該中間体はアミンおよび二酸化炭素に自発的に脱カルボキシル化する(図1A〜1Cに示す)。前記スキームを終了させるために、バルク/表面架橋剤を使用することによって、アミノ化表面からバルクへの、エポキシ、シラノールおよびイソシアネート間のさらなるバルク架橋反応を行うことが提案される。簡単に言えば、調製されたオルガノシラン改質面は、続いてプロピレンカーボネート中のポリイソシアネートの20%溶液で吹き付けられ(2つのポリイソシアネートプレポリマー:(i)1,6−ヘキサメチレンジイソシアネートホモポリマー(HMDI)トリマー(図1A〜1Cに示す)および(ii)4,4’−メチレンジフェニルイソシアネート(MDI)プレポリマー類似法の1つを使用)。湿潤面の均一被覆率は、未乾燥塗膜厚さ計で測定して約2ミル(50ミクロン(μm))であった。
この検討に使用した材料の概要を表2に示す。
A.Mg豊富プライマーの臨界顔料容積濃度推定
臨界顔料容積濃度(CPVC)は、顔料+吸着層厚さ(d)のランダム稠密充填効率(random dense packing efficiency)の関数であり、これは実験的に求めなければならない。これは、文献に広く記載されており、最近の検討(参照により本明細書に組み込まれるBierwagen et al.,「Recent Studies of Particle Packing in Organic Coatings」,Prog.Organic Coatings,35:1−10(1999))は新たな事実を考慮している。これらのMg豊富系のCPVCを得る方法を、以下に記載する。2つのマグネシウム粉末、平均粒径分布(PSD)30μmのEckagranules(商標)PK31および平均PSD70μmのEckagranules(商標)PK51(図3A参照)を入手したままの状態で使用し、52%−PK31:48%−PK51容積で混合した。2つの粉末の52:48容積混合物は、各粉末単独の場合より高い嵩密度値を生じることが見出された。まず、プライマーの臨界顔料容積濃度(CPVC)は、全顔料上2%vol.におけるAerosil(商標)R202を使用して樹脂/粉末すり合わせ値(rub−up value)を得ることによって概算し、最終CPVCを、実験的に求めた樹脂すり合わせ値と組み合わせて、球状と想定した3つの顔料について、Eckart GmbHから提供されるPSDから算出した。図3Bは、3つの顔料混合物についての三成分図からの算出CPVCを示す。体積分率座標(PK31=0.51、PK51=0.47、およびR202=0.02)は、PVC=0.475の領域における理論CPVC値を与え、これは、図2Aおよび2BのEISデータから確認される実験的に推測したCPVCを裏付けている。
1.パネルおよび皮膜の作製。表2の材料からのプライマーを、6’’x3’’ Al 2024 T3 Q−panels(商標)に適用し、Scotch Brite(商標)パッドでこすり、濯ぎ、エチル−3−エトキシプロピオネート(「EEP」)で脱脂し、その後、10%燐酸溶液に60秒間浸漬し、蒸留水で濯いだ。Alパネルを、参照により本明細書に組み込まれるWalker,「Organo Silanes as Adhesion Promoters for Organic Coatings」,Journal of Coatings Technology,52(670):49−61(1980)に記載の方法によって表面改質した。Mg豊富被覆剤を、タッチアップスプレーガンで塗布し、被覆剤を35℃で14日間硬化させた。次に、下塗りしたパネルを、Extended Lifetime(商標)Topcoatで上塗りした。SEMおよびEDAX画像によって確認された平均膜厚(FT)は、約50±20ミクロン(μm)と推定されるプライマー膜厚、および約100±40ミクロン(μm)と推定されるトップコート膜厚を示す。
1.Mg豊富被覆剤の機械的特性。Instron(商標)モデル5542およびMerlin(2)ソフトウエアを使用して、ASTM D 2370−82に従って引張特性を測定した。DMTA測定は、Rheometricsモデル3−E動的機械分析器を使用して行った。
A.被覆ポリマーの粘弾性
表3は、5つのポリマー系の測定粘弾性を示す:Tg、貯蔵弾性率E’(最小値)、および計算架橋密度。記録されたガラス転移温度の有意な差は、完全硬化における個々の被覆剤化学特性に関係していると考えられる。架橋密度は(E’)から算出した:(T=Tg+50℃)、この温度において材料はゴム状である;νeは弾性的に有効な架橋密度である:νe=3E’/RT(T+Tg)。
表4は、被覆ポリマー皮膜の測定引張特性を示す。引張試験は、目に見える空隙のない被覆ポリマー皮膜ストリップにおいて行った。表4の機械的特性は、出発材料と比較して、ハイブリッド系の引張強度および引張弾性率特性の両方の向上を示す。引張弾性率は、その測定値が皮膜の引張強度より低い欠陥依存性であるので、皮膜の機械的特性のより優れた指標であることが既知である。高い引張弾性率は、物質が、より弾性であることも示し、これは、より高い硬化度または転化度を意味する。
難燃性(FR)被覆剤は、発火を遅らせ、延焼性を抑制する被覆剤である。燃焼性を評価する一般的な試験法は、限界酸素指数(LOI)試験(ASTM D 2863)であり、LOIが26未満の場合、材料は一般に燃焼性とみなされる。これらの被覆剤は全て、ある尺度において被膜不燃性に寄与し得る弗素化ELT(商標)トップコートで被覆された(図4A〜4D)。被膜燃焼性に関連して最もよく報告されるパラメーターは、材料の限界酸素指数(LOI)値である。エポキシ/ポリアミン系は、シラン改質セラマー(ceramer)エポキシドについて低値24〜高値32の間で変化する一方、弗素化ポリウレタンは50までである。向上した不燃性に寄与する他の要因は、イソシアヌレート結合の存在である。HMDIは、MDIのような他のウレタン結合より固有に高い熱安定性を有することが報告されているが、後者は約200℃で解離することが報告されている。一般に、燃焼性は、イソシアヌレートトリジン環の比率が増加すると共に減少する。
希薄ハリソン溶液、(NH4SO4)酸性雨条件におけるProhesion(商標)暴露の結果、従来の結合剤を使用したMg豊富被膜は約1000時間まで明瞭なけがき線を維持し、これに対し、ハイブリッド結合剤を使用して配合した被膜は、3000時間まで明瞭なけがき線を示し5000時間で破損の徴候を示した。プライマービヒクルの結合性が、これらの系の向上した防食に関連した主要な問題であると考えられる。Mg豊富プライマー被膜の全試料は、この暴露において、同様のトップコートを有する標準クロメート基剤系より優れた性能を示し、かつ、図5A〜5Eに見られるように、4800時間後のこれらのMg豊富系は、1800時間の暴露後の非着色プライマー/ELT(商標)系(図5E)より目視的に優れた性能を示した。
A.Mg豊富被膜の電解化学的検討
高いpH、中性pHおよび低いpH条件下に、トップコートを有する50%PVC(CPVCより大)のMg豊富プライマーのEIS試験を行った。3%NaCl溶液中、pH条件を変化させて、円形にけがいたMg豊富被膜を浸漬に付すことを伴うEIS試験法を使用した。この方法は、この研究において開発された種々のプライマー配合物を識別するのを助けるために使用した。けがいた条件下に、系を、酸性(pH2.8)、中性および塩基性(pH2.0)3%NaCl浸漬に付すことで、広い範囲の暴露条件における配合物の比較が可能になった。Mg豊富Al 2024 T−3パネルを、Deft 99 GY−001 ELT(商標)(極めて耐化学薬品性の被覆剤)で上塗りし、けがき、次に、連続浸漬に付した。3つの被覆系をMg豊富被覆剤として評価し、2つは市販の既製品であり、1つは前記のハイブリッドシラン改質エポキシ−尿素であった。簡単に言えば、3つの被覆系は以下の通りであった:
被膜を切ってAl 2024 T−3面を露出させる直径1.0cmの円形けがき線を有する試料上に、円筒形電極セルを取り付けた。円筒に、以下の組成の電解質を装填した:(1) NaOHでpH12.0に調節した3質量%NaClにおいて塩基性;(2)HClでpH2.8に調節した3質量%NaClにおいて酸性;(3)pH6.2の3.0質量%NaClにおいて中性。実施例3に記載したEIS試験法を使用して、各試験の間で調節した11日間にわたるpHにおいて、インピーダンス測定を行った。中性3%NaCl溶液への浸漬によって非損傷被膜に何が起きているかを調べるために、けがいていない上塗り皮膜も電気化学的に検査した。
けがき暴露試験(図6A〜6C(塩基性条件pH12)および7A〜7C(酸性条件pH2.8))から得た目視結果は、高いpHおよび低いpH条件下に、従来の被覆ポリマー、即ちMC−PURおよびエポキシ/シッフ塩基、を使用して配合したMg豊富被覆剤は、これらのpH極値において弱点を有することを示した。高いpH12において、試料A(E23、MC−PUR)およびC(ハイブリッドエポキシ−マンニッヒ塩基)は、浸漬暴露後にふくれを生じた。低いpH2.8において、浸漬暴露によって皮膜が基材から剥がれ、持ち上がった。アミノ−シラン改質ハイブリッドポリマーマトリックス(試料B)は、より一般的なポリマーと比較して、付着性および反応性において、Mg豊富被覆剤におけるかなり高いpH耐性系を与えた。11日間の試験後のけがいた試料において目に見える差異がないことは、中性pH6.2の条件が、プライマー被膜/界面においてより高い安定性を与えることを示している。
A.動的および機械的特性の結果
ポリマー皮膜の粘弾性DMTA測定は、ハイブリッドシラン改質エポキシ−尿素/ウレタンが、母材と同じ架橋密度において、より低いTgを示すことを明らかにし、これは、IPNマトリックス全体におけるバルク(−N−R−Si−O−Si−R−N−)結合の形成を示唆している。さらに、シラン改質エポキシ−尿素ハイブリッドの引張特性は、それらの母材より優れていた。
試験した4つの系のいずれに関しても、PVCに関する燃焼性の違いは観察されなかった。2つの従来の被覆剤、ポリ尿素(MC−PUR)および(エポキシ/ポリアミド)は、剥離し、液化し、灰化し、続いて急速にマグネシウムが灰化した。ハイブリッド−E23A、MDIは、液化も剥離もしなかったが、少量の木炭を形成し、マグネシウムは灰化しなかった。脂肪族の、N−アルキルイソシアヌレート含有ハイブリッドN3300は、炭化せず、Mgも灰化しなかった。このMg豊富被覆剤は、(−Al−O−Si−)結合によってAl基材に、より共有的に結合し、この付加的共有結合が、被膜燃焼性を減少させるのに正の影響を与えたと推測される。
顔料Mg含有量を43、46および50%PVCとなるように変化させた4つの被覆系において行ったASTM D5894−96の結果は、希薄ハリソン溶液への暴露の関数としてのPVCにおいて、明確な傾向を示さなかった。しかし、ハイブリッド配合物における50%PVC試料は、僅かにより優れた性能を示した。シラン改質エポキシ−MDIハイブリッド系は、最も優れた性能を示し、破損まで約5000時間であり、一方、脂肪族シラン改質エポキシ−HMDIハイブリッド被膜は、3000〜3400時間の範囲で破損した。他の2つの従来Mg豊富被覆系:ポリ尿素(MC−PUR)およびエポキシ/ポリアミドは、2000〜2600時間で破損し、2つの従来の市販被覆系の間に明確な差異はなかった。
Mg豊富プライマー配合物を、実験室量から2.2Lにスケールアップした。この配合バッチ用に選択したPVCは、系のPVCよりわずかに高いと考えられる数値50であった。以下の工程に従ってスケールアップを行った:(1)出発物質の調製、(2)Mg粉末の調製、(3)パネル表面の調製、(4)タイコートの調製/塗布、および(5)Mg粉末混合物の調製/塗布。
Claims (7)
- 金属の耐食性を向上させるために金属を処理する方法であって、マグネシウム粉末および結合剤を含有する被覆剤を金属表面に塗布することを含む方法であって、前記金属が、アルミニウムまたはアルミニウム合金であり、前記マグネシウムの量は、顔料容積濃度(PVC)が43%〜50%になるように選択される方法。
- 前記マグネシウム粉末が、第一マグネシウム粒子粉末および第二マグネシウム粒子粉末の混合物を含み、
前記第一マグネシウム粒子粉末および前記第二マグネシウム粒子粉末が、実質的に異なる平均粒径分布を有し、
前記混合物の嵩密度が前記第一マグネシウム粒子粉末の嵩密度より大きく、前記混合物の嵩密度が前記第二マグネシウム粒子粉末の嵩密度より大きい、請求項1に記載の方法。 - 前記第一マグネシウム粒子粉末が、平均粒径25μm〜35μmを有し、第二マグネシウム粒子粉末が、平均粒径65μm〜75μmを有する、請求項2に記載の方法。
- 前記結合剤が高分子結合剤であり、前記高分子結合剤が、ポリイソシアネートプレポリマーおよびエポキシプレポリマーを含む請求項1に記載の方法。
- 該被覆剤の塗布前に、金属表面をアミン含有オルガノシランと接触させることをさらに含む、請求項1に記載の方法。
- 前記マグネシウム粉末が、(i)マグネシウムおよび(ii)マンガンを含むマグネシウム合金の粉末である、請求項1に記載の方法。
- マグネシウム粉末、およびシラン改質エポキシイソシアネートハイブリットポリマーまたはプレポリマーを含む、被覆組成物。
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US60/562,883 | 2004-04-16 | ||
PCT/US2004/033089 WO2005051551A1 (en) | 2003-11-13 | 2004-10-07 | Magnesium rich coatings and coating systems |
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