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Potential Ivvs.Gelbasedre US010644304B2 ( 12 ) United States Patent ( 10 ) Patent No.: US 10,644,304 B2 Ein - Eli et al. (45 ) Date of Patent : May 5 , 2020 (54 ) METHOD FOR PASSIVE METAL (58 ) Field of Classification Search ACTIVATION AND USES THEREOF ??? C25D 5/54 ; C25D 3/665 ; C25D 5/34 ; ( 71) Applicant: Technion Research & Development HO1M 4/134 ; HOTM 4/366 ; HO1M 4/628 ; Foundation Limited , Haifa ( IL ) (Continued ) ( 72 ) Inventors : Yair Ein - Eli , Haifa ( IL ) ; Danny (56 ) References Cited Gelman , Haifa ( IL ) ; Boris Shvartsev , Haifa ( IL ) ; Alexander Kraytsberg , U.S. PATENT DOCUMENTS Yokneam ( IL ) 3,635,765 A 1/1972 Greenberg 3,650,834 A 3/1972 Buzzelli ( 73 ) Assignee : Technion Research & Development Foundation Limited , Haifa ( IL ) (Continued ) ( * ) Notice : Subject to any disclaimer , the term of this FOREIGN PATENT DOCUMENTS patent is extended or adjusted under 35 CN 1408031 4/2003 U.S.C. 154 ( b ) by 56 days . EP 1983078 10/2008 (21 ) Appl. No .: 15 /300,359 ( Continued ) ( 22 ) PCT Filed : Mar. 31 , 2015 OTHER PUBLICATIONS (86 ) PCT No .: PCT/ IL2015 /050350 Hagiwara et al. in ( Acidic 1 - ethyl - 3 -methylimidazoliuum fluoride: a new room temperature ionic liquid in Journal of Fluorine Chem $ 371 (c ) ( 1 ), istry vol . 99 ( 1999 ) p . 1-3 ; ( Year: 1999 ). * (2 ) Date : Sep. 29 , 2016 (Continued ) (87 ) PCT Pub . No .: WO2015 / 151099 Primary Examiner — Jonathan G Jelsma PCT Pub . Date : Oct. 8 , 2015 Assistant Examiner Omar M Kekia (65 ) Prior Publication Data (57 ) ABSTRACT US 2017/0179464 A1 Jun . 22 , 2017 Disclosed is a method for activating a surface of metals , Related U.S. Application Data such as self- passivated metals , and of metal -oxide dissolu tion , effected using a fluoroanion -containing composition . (60 ) Provisional application No.61 / 972,481, filed on Mar. Also disclosed is an electrochemical cell utilizing an alu 31, 2014 . minum -containing anode material and a fluoroanion - con taining electrolyte , characterized by high efficiency , low (51 ) Int. Ci. corrosion , and optionally mechanical or electrochemical HOIM 4/04 (2006.01 ) rechargeability . Also disclosed is a process for fusing (weld HOIM 4/134 ( 2010.01 ) ing , soldering etc.) a self- passivated metal at relatively low ( Continued ) temperature and ambient atmosphere , and a method for ( 52 ) U.S. CI. electrodepositing a metal on a self- passivated metal using CPC HOLM 4/044 ( 2013.01 ) ; B23K 35/3605 metal- oxide source . (2013.01 ) ; B23K 35/383 ( 2013.01) ; ( Continued ) 6 Claims, 15 Drawing Sheets PotentialIVvs.gelbasedRE - SS 50 % *** 89 838-88-88 88-9 *** -1.2 US 10,644,304 B2 Page 2 (51 ) Int. Ci. Translation dated Aug. 19 , 2018 of Notification of Office Action and HOIM 4/36 ( 2006.01 ) Search Report dated Jul . 20 , 2018 from the State Intellectual HOIM 4/46 ( 2006.01 ) Property Office of the People's Republic of China Re. Application HOIM 4/62 ( 2006.01 ) No. 201580024001.2 . ( 19 Pages ) . HOIM 10/054 ( 2010.01 ) Supplementary European Search Report and the European Search C250 3/66 ( 2006.01 ) Opinion dated Aug. 10 , 2017 From the European Patent Office Re. HOIM 12/08 ( 2006.01 ) Application No. 15773010.2 . ( 9 Pages) . B23K 35/36 ( 2006.01 ) Tsuda et al . “ A Highly Conductive Composite Electrolyte Consist C25D 5/54 ( 2006.01 ) ing of Polymer and Room Temperature Molten Fluorohydrogenates ” , HOIM 4/1395 ( 2010.01 ) Solid State Ionics, XP004370988 , 149 (3-4 ) : 295-298 , Aug. 2 , 2002 . C25D 5/34 ( 2006.01) Notification of Office Action and Search Report dated Jul. 20 , 2018 B23K 35/38 ( 2006.01 ) From the State Intellectual Property Office of the People's Republic HOIM 4/66 ( 2006.01) of China Re. Application No. 201580024001.2 . ( 13 Pages ) . HOIM 10/0569 ( 2010.01) Communication Pursuant to Article 94 ( 3 ) EPC dated Mar. 21 , 2018 HOIM 4/02 from the European Patent Office Re. Application No. 15773010.2 . ( 2006.01 ) ( 5 Pages ). HOIM 4/50 ( 2010.01) Armand et al. “ Ionic -Liquid Materials for the Electrochemical (52 ) U.S. CI. Challenges of the Future ” , Nature Materials , 8 : 621-629 , Aug. 2009 . CPC C25D 3/665 ( 2013.01 ) ; C25D 5/34 Berrettoni et al. “ A Cyclic Voltammetric Study of the Electrochemi ( 2013.01) ; C25D 5/54 ( 2013.01 ) ; HOTM 4/134 cal Behavior of NiS2 in Molten NaCl Saturated NaAlC14 Melts ” , (2013.01 ) ; HOTM 4/1395 (2013.01 ) ; HOLM Journal of the Electrochemical Society , 140 ( 4 ) : 969-973 , Apr. 1993 . 4/366 (2013.01 ) ; HOTM 4/463 ( 2013.01 ) ; Bockstie et al. " Control of Al Corrosion in Caustic Solutions” , HOTM 4/628 (2013.01 ) ; HOTM 4/661 Journal of the Electrochemical Society , 110 ( 4 ) : 267-271, Apr. 1963 . ( 2013.01 ) ; HOIM 10/054 ( 2013.01) ; HOLM Doche et al. “ Electrochemical Behaviour of Aluminium in Concen 10/0569 (2013.01 ) ; HOIM 12/08 ( 2013.01) ; trated NaOH Solutions” , Corrosion Science , 41 ( 4 ) : 805-826 , 1999 . HOIM 4/502 (2013.01 ) ; HOLM 2004/027 Egan et al. “ Developments in Electrode Materials and Electrolytes for Aluminium - Air Batteries ” , Journal of Power Sources , p . 1-18 , ( 2013.01 ) ; HOIM 2300/0045 ( 2013.01 ) ; YO2E 2013 . 60/128 ( 2013.01) Gelman et al . “ Aluminium - Air Battery Based on an Ionic Liquid (58 ) Field of Classification Search Electrolyte ” , Journal of Materials Chemistry A , 2 ( 47 ) : 20237 CPC HO1M 10/054 ; HO1M 2004/027 ; HOLM 20242 , 2014 . 4/044 ; HO1M 12/08 ; HOTM 4/1395 ; Holleck “ The Reduction of Chlorine on Carbon in AIC13 - KC1 HO1M 4/502 ; HO1M 4/463 ; HO1M 4/661; NaCl Melts ” , Journal of the Electrochemical Society , 119( 9 ): 1158 1161 , Sep. 1972 . HOLM 10/0569; HOTM 2300/0045 ; B23K Jiang et al. “ Electrodeposition of Aluminium From Ionic Liquids: 35/3605 ; YO2E 60/128 Part I — Electrodeposition and Surface Morphology of Aluminium USPC 429/200 From Aluminium Chloride ( A1C13 ) -1- Ethyl- 3 -Methylimidazolium See application file for complete search history . Chloride ( [ EMIm ]CI ) Ionic Liquids” , Surface & Coatings Technol ogy, 201 : 1-9 , 2006 . ( 56 ) References Cited Knutz et al . “Mechanism of Reaction in NaAlC14 Molten Salt Batteries With Nickel Felt Cathodes and Aluminium Anodes . I. U.S. PATENT DOCUMENTS Modeling of the Battery Properties at Thermodynamic Equilib 4,619,716 A 10/1986 Suzuki et al . rium ” , Journal of the Electrochemical Society, 140 ( 12 ): 3374-3379 , 4,643,241 A 2/1987 Yonekura et al. Dec. 19963 . 8,715,853 B1 5/2014 Vajo et al . Knutz et al. “ Mechanism of Reaction in NaAlC14 Molten Salt 2011/0262816 A1 * 10/2011 Amatucci HOLM 8/0606 Batteries With Nickel Felt Cathodes and Aluminium Anodes . II . 429/336 Experimental Results and Comparison With Model Calculations” , 2012/0082904 A1 4/2012 Brown et al . Journal of the Eletrochemical Society , 140 ( 12 ): 3380- 3390 , Dec. 2012/0082905 A1 4/2012 Brown et al . 1993 . 2012/0164541 A1 * 6/2012 Darolles HOTM 6/164 Kuboki et al. “ Lithium - Air Batteries Using Hydrophobic Room 429/326 Temperature Ionic Liquid Electrolyte ” , Journal of Power Sources , 2015/0093659 Al * 4/2015 Gonzalez HOM 12/08 146 : 766-769 , 2005 . 429/405 Li et al. “ Aluminium as Anode for Energy Storage and Conversion : A Review ” , Journal of Power Sources , 110 : 1-10 , 2002 . FOREIGN PATENT DOCUMENTS Licht et al . “ The Effect of Water on the Anodic Dissolution of Aluminium in Non - Aqueous Electrolytes ” , Electrochemistry Com JP 2006-198512 8/2006 munications , 2 : 329-333 , 2000 . JP 2010-146800 7/2010 Lin et al . “ An Ultrafast Rechargeable Aluminium - Ion Battery ” , JP 2014-032914 2/2014 Nature , p . 1-16 , 2015 . WO WO 01/66827 9/2001 Mikeska et al. “ Corrosion of Alumina in Aqueous Hydrofluoric WO WO 2015/151099 10/2015 Acid ” , Journal of the American Ceramic Society, 82 ( 12 ): 3561 3566 , 1999 . OTHER PUBLICATIONS Shvartsev et al . “ Reference Electrode Assembly and Its Use in the Study of Fluorohydrogenate Ionic Liquid Silicon Electrochemis English language machine translation of Joboji Toru JP 2010 try ” , Physical Chemistry Chemical Physics, 15 (41 ) : 17837-17845 , 146800 ( A ) —Jul. 1 , 2010 “ Air Battery ” ( Year : 2010) . * Nov. 7 , 2013 . Communication Pursuant to Article 94( 3 ) EPC dated Aug. 17 , 2018 Wang et al. " Corrosion and Electrochemical Behaviors of Pure From the European Patent Office Re. Application No. 15773010.2 . Aluminium in Novel KOH -Ionic Liquid -Water Solutions” , Materi ( 4 Pages) . als and Corrosion , 60 ( 12 ) : 977-981 , 2009 . Chen et al . “ Electrochemical Study of Copper in a Basic 1 - Ethyl Weaving et al. “ Experimental Studies of Transition Metal Chloride 3 -Methylimidazolium Tetrafluoroborate Room Temperature Molten Electrodes in Undivided Cells Using Molten NaAlCl4 Electrolyte ” , Salt ” , Electrochimica Acta 45 ( 3 ) : 441-450 , Oct. 15 , 1999 . Journal of Power Sources, 36 : 537-546 , 1991 . US 10,644,304 B2 Page 3 ( 56 ) References Cited OTHER PUBLICATIONS Zaromb " The Use and Behavior of Aluminium Anodes in Alkaline Primary Batteries” , Journal of the Electrochemical Society, 109 ( 12 ) : 1125-1130 , Dec. 1962 . Zaromb et al . “ Aluminium -Consuming Fluidized - Bed Anodes ” , Journal of the Electrochemical Society , 137 (6 ) : 1851-1856 , Jun . 1990 . Zaromb et al. “ Feasibility of Electrolyte Regeneration in Al Bat teries” , Journal of the Electrochemical Society , 109( 12 ) : 1191-1192 , Dec. 1962 . Zein El Abedin et al. “ Electrodeposition ofNano- and Microcrystal line Aluminium in Three Different Air and Water Stable Ionic Liquids ” , ChemPhysChem , 7 : 1535-1543 , 2006 . Zhao et al . “ Review : Electrodeposition of Aluminium From Nonaque ous Organic Electrolytic Systems and Room Temperature Molten Salts ” , Electrochimica Acta , 42 ( 1 ) : 3-13 , 1997 . Communication Pursuant to Article 94 ( 3 ) EPC dated Feb. 12 , 2019 From the European Patent Office Re . Application No. 15773010.2 . ( 7 Pages ) . Result of Consultation dated Feb. 1 , 2019 From the European Patent Office Re . Application No. 15773010.2 . ( 3 Pages ). Notification of Office Action and Search Report dated Mar. 14 , 2019 From the State Intellectual Property Office of the People's Republic of China Re .
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