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(12) United States Patent (10) Patent No.: US 7,507,480 B2 Sugama (45) Date of Patent: Mar USOO7507480B2 (12) United States Patent (10) Patent No.: US 7,507,480 B2 Sugama (45) Date of Patent: Mar. 24, 2009 (54) CORROSION-RESISTANT METAL SURFACES 6,239,205 B1 5/2001 Hasegawa et al. 6,254,980 B1 7/2001 Tadokoro et al. (75) Inventor: Toshifumi Sugama, Wading River, NY 6,297.302 B1 10/2001 Heeks et al. (US) 6,312,812 B1 1 1/2001 Hauser et al. 6,469,119 B2 10/2002 Basil et al. (73) Assignee: Brookhaven Science Associates, LLC, 6,551482 B2 4/2003 Yamamoto et al. Upton, NY (US) 6,554,989 B2 4/2003 Muramoto et al. 6,608, 129 B1 8, 2003 Koloski et al. (*) Notice: Subject to any disclaimer, the term of this 6,686,406 B2 2/2004 Tomomatsu et al. patent is extended or adjusted under 35 6,716,895 B1 4/2004 Terry U.S.C. 154(b) by 597 days. 6,749,945 B2 6/2004 Knobbe et al. 6,770,690 B2 8/2004 Fujiki et al. (21) Appl. No.: 11/141,674 2001/0006731 A1 7/2001 Basil et al. 2002/O121442 A1 9, 2002 Muramoto et al. (22) Filed: May 31, 2005 2002/0136911 A1 9/2002 Yamamoto et al. 2003/00928.12 A1 5/2003 Nakada et al. (65) Prior Publication Data 2004/0022950 A1 2/2004 Jung et al. 2004/0116551 A1 6/2004 Terry US 2006/026976O A1 Nov.30, 2006 (51) Int. Cl. FOREIGN PATENT DOCUMENTS CSK 3/22 (2006.01) AU 3.2947/84 3, 1985 (52) U.S. Cl. .................. 428/447; 524/780; 106/287.11; EP O 769 540 4f1997 427/387 (58) Field of Classification Search ................. 428/447: 106/287.11: 524/780; 427/387 OTHER PUBLICATIONS See application file for complete search history. M. Bethencourt, et al., “Lanthanide Compounds as Environmentally Friendly Corrosion Inhibitors of Aluminum Alloys: A Review'. Cor (56) References Cited rossion Science, vol. 40, No. 11, pp. 1803-1819 (1998). U.S. PATENT DOCUMENTS T. Sugama et al., “Polyaminopropylsiloxane Coatings for Geothermal Air-cooled Condensers'. Recent Res. Devel. Mat. Sci., vol. 4, pp. 3,142,655 A 7, 1964 Bobear 695-710 (2003). 3,855,172 A 12/1974 Iler et al. M.A. Arenas et al., “Inhibition of 5083 Aluminium Alloy and 3,884,850 A 5, 1975 Koda et al. Galvanised Steel by Lanthanide Salts', Corrosion Science, vol. 43. 4,366,278 A 12, 1982 Hamada et al. pp. 157-170 (2001). 4,637,889 A 1, 1987 Kishimoto et al. Y. Xingwen et al., "Corrosion Behavior of Rare Earth Metal (REM) 4,701,488 A 10, 1987 Williams Conversion Coatings on Aluminum Alloy LY12. Material Science 4,749,550 A 6, 1988 Goldie et al. and Engineering, vol. A284, pp. 56-63 (2000). 4,948,826 A 8, 1990 Hirai S. Virtanen et al., “A Surface Analytical and Electrochemical Study 4,992,115 A 2f1991 Ikeda on the Role of Cerium in the Chemical Surface Treatment of Stainless 5,008,317 A 4, 1991 Wolfer et al. Steels”, Corrosion Science, vol. 39, No. 10-11, pp. 1897-1913 5,035,745 A 7, 1991 Lin et al. (1997). 5,099,006 A 3, 1992 Gradeffet al. M. Forsyth et al., “ATR Characterization of Synergistic Corrosion 5,175,202 A 12/1992 Kissel Inhibition of Mild Steel Surfaces by Cerium Salicylate'. Corrosion 5, 198487 A 3, 1993 Kissel Science, vol. 44, pp. 2651-2656 (2002). 5,204,384 A 4, 1993 Matsushita et al. L.S. Kasten et al., “An XPS Study of Cerium Dopants. In Sol-Gel 5,231,156 A 7, 1993 Lin Coatings For Aluminum 2024-T3', Surface and Coatings Technol 5.330,794. A 7, 1994 Bosco et al. ogy, vol. 140, pp. 11-15 (2001). 5,344,712 A 9, 1994 Basil et al. 5,384.357 A 1/1995 Levinson et al. (Continued) 5,399,192 A 3, 1995 Yamasoe 5.449,736 A 9, 1995 Cabasso et al. Primary Examiner Margaret G Moore 5,470,910 A 1 1/1995 Spanhel et al. (74) Attorney, Agent, or Firm Lori-Anne Neiger 5,635,548 A 6, 1997 Kittle et al. 5,698,483. A 12/1997 Ong et al. (57) ABSTRACT 5,718,907 A 2f1998 Labarre 5,750,610 A 5, 1998 Burns et al. 5,777,001 A 7/1998 Seeney et al. The present invention relates to metal Surfaces having thereon 5,789,082 A 8/1998 Treadway an ultrathin (e.g., less than ten nanometer thickness) corro 5,817, 160 A 10/1998 Nagpal et al. Sion-resistant film, thereby rendering the metal Surfaces cor 5,866,652 A 2/1999 Hager et al. rosion-resistant. The corrosion-resistant film includes an at 5,939,197 A * 8/1999 Blohowiak et al. .......... 428/413 5,939,487 A 8, 1999 Kimura et al. least partially crosslinked amido-functionalized silanol com 5,969,075 A 10, 1999 Inoue ponent in combination with rare-earth metal oxide nanopar 5.998,523 A 12/1999 Grunbauer et al. ticles. The invention also relates to methods for producing 6,180,248 B1 1/2001 Basil et al. Such corrosion-resistant films. 6,228.904 B1 5, 2001 Yadav et al. 6,232,386 B1 5/2001 Vargo et al. 82 Claims, No Drawings US 7,507,480 B2 Page 2 OTHER PUBLICATIONS F. Mansfeld et al., “Corrosion Protection of High Copper Aluminium K. Aramaki, "The Inhibition Effects of Chromate-Free, Anion Inhibi Alloys by Surface Modification', British CorrosionJournal, vol. 29. tors on Corrosion of Zinc in Aerated 0.5 M NaCl, Corrosion Sci No. 3, pp. 194-200 (1994). ence, vol.43, pp. 591-604 (2001). F. Mansfeld et al., “Development of Stainless Aluminum”. J. F. Mansfeld et al., “Development of “Stainless' Aluminum Alloys by Electrochem. Soc., vol. 138, No. 12, pp. L74, L75 (1991). Surface Modification.” Materials Science and Engineering, vol. Y.C. Lu et al., “The Improvement of the Localized Corrosion Resis A198, pp. 51-61 (1995). tance of Stainless Steel by Cerium”. Corrosion Science, vol. 34, No. Y.C. Lu et al., "Chemical Treatment With Cerium to Improve the 11, pp. 1773-1785 (1993). Crevice Corrosion Resistance of Austenitic Stainless Steels', Corro F. Mansfeld et al., “Short Communication—Pitting and Surface sion Science, vol. 37, No. 1, pp. 145-155 (1995). Modification of SIC/AL”. Corrosion Science, vol. 27. No. 9, pp. A. Aballe et al., "CeCls and LaCl binary solutions as environment 997-1000 (1987). friendly corrosion inhibitors of AA5083 Al-Mg alloy in NaCl solu A.E. Hughes et al., “XPS and SEM Characterization of Hydrated tions”,Journal of Alloys and Compounds, vol. 323-324, pp. 855-858 Cerium Oxide Conversion Coatings'. Surface and Interface Analy (2001). X. Yu, et al., "Corrosion Behavior of Rare Earth Metal (REM) Con sis, vol. 23, pp. 540-550 (1995). version Coatings on Aluminum Alloy LY12. Materials Science & F. Mansfeld, "Surface Modification and Stainless Steels: GreenTech Engineering, vol. A284, pp. 56-63 (2000). nology for Corrosion Protection'. Surface and Coatings Technology, D.R. Arnott et al., "Cationic-Film-Forming Inhibitors for the Protec vol. 90, pp. 224-228 (1997). tion of the AA 7075 Aluminum Alloy Against Corrosion in Aqueous M.A. Arenas et al., “Cerium: A Suitable Green Corrosion Inhibitor Chloride Solution'. Corrosion Science, vol. 45, No. 1, pp. 12-18 for Tinplate'. Corrosion Science, vol. 44, pp. 511-520 (2002). (1989). X. Yu et al., “Electrochemical Study of the Corrosion Behavior OfCe S.M. Powell et al., “Use of the Scanning Reference Electrode Tech Sealing Of Anodized 2024 Aluminum Alloy'. Thin Solid Films, vol. nique for the Evaluation of Environmentally Friendly, Nonchromate 423, pp. 252-256 (2003). Corrosion Inhibitors'. Corrosion, vol. 55, No. 11, pp. 1040-1051 K. Aramaki. “Cerium(III) Chloride and Sodium Octylthiopropionate (1999). as an Effective Inhibitor Mixture for Zinc Corrosion in 0.5 M Nacil', C.B. Breslin, “Influence of Rare-Earth Metal Passivation Treatments Corrosion Science, vol. 44, pp. 1361-1374 (2002). on the Dissolution of Tin-Zinc Coatings'. Corrosion, vol. 54, No. 12, pp. 964-971 (1998). M. Balasubramanian et al., “An X-Ray Absorption Study of the Local B.R.W. Hinton, “The Corrosion Inhibition of Zinc with Cerous Chlo Structure of Cerium in Electrochemically Deposited Thin Films'. ride', Corrosion Science, vol. 29, No. 8, pp. 967-985 (1989). Thin Solid Films, vol. 347, pp. 178-183 (1999). B.R.W. Hinton et al., “The Inhibition of Aluminum Alloy Corrosion M. Dabala et al., “Cerium-Based Conversion Layers on Aluminum by Cerous Cations'. Metals Forum, vol.7. No. 4, pp. 211-217 (1984). Alloys'. Applied Surface Science, vol. 172, pp. 312-322 (2001). B.R.W. Hinton, “Corrosion Inhibition With Rare Earth Metal Salts', W. G. Fahrenholz et al., “Characterization of Cerium-Based Conver Journal of Alloys and Compounds, vol. 180, pp. 15-25 (1992). sion Coatings for Corrosion Protection of Aluminum Alloys'. Sur A.J. Aldykewicz, Jr. et al., “The Investigation of Cerium as a Cathodic face and Coatings Technology, vol. 155, pp. 208-213 (2002). Inhibitor for Aluminum-Copper Alloys'. J. Electrochem. Soc., vol. 142, No. 10, pp. 3342-3350 (1995). * cited by examiner US 7,507,480 B2 1. 2 CORROSION-RESISTANT METAL SURFACES embodiment, the rare-earth metal oxide nanoparticles are nanoparticles of cerium oxide or Samarium oxide. This invention was made with Government support under In a preferred embodiment, the at least partially contract number DE-AC02-98CH10886, awarded by the crosslinked amido-functionalized silanol component is com U.S. Department of Energy. The Government has certain 5 posed, minimally, of at least partially crosslinked versions of rights in the invention.
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