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20170001252.Pdf 11111111111111111111111111111111111111111111111111111111111111111111111111 (12) United States Patent (io) Patent No.: US 9,543,575 B2 Yushin et al. (45) Date of Patent: Jan. 10, 2017 (54) SILICON-BASED ANODE AND METHOD HOLM 411395 (2010.01) FOR MANUFACTURING THE SAME HOLM 4136 (2006.01) HOLM 4138 (2006.01) (75) Inventors: Gleb Nikolayevich Yushin, Atlanta, (52) U.S. Cl. GA (US); Igor Luzinov, Clemson, SC CPC ......... H01M 411395 (2013.01); HOLM 410404 (US); Bogdan Zdyrko, Clemson, SC (2013.01); HOLM 41366 (2013.01); HOLM (US); Alexandre Magasinski, Atlanta, 41386 (2013.01); HOLM 41625 (2013.01); GA (US) Y02E 601122 (2013.01); Y02P 70154 (2015.11) (73) Assignees: Georgia Tech Research Corporation, (58) Field of Classification Search Atlanta, GA (US); Clemson University, USPC ............. 429/217, 218.1; 252/182.1; 423/324 Clemson, SC (US) See application file for complete search history. (*) Notice: Subject to any disclaimer, the term of this (56) References Cited patent is extended or adjusted under 35 U.S. PATENT DOCUMENTS U.S.C. 154(b) by 754 days. 7,592,095 132 * 9/2009 Lee et al....................... 429/118 (21) Appl. No.: 13/510,038 2003/0198870 Al 10/2003 Wariishi et al. 2007/0048609 Al * 3/2007 Ueda ..................... HO IM 4/134 (22) PCT Filed: Nov. 16, 2010 429/218.1 2007/0122700 Al* 5/2007 Miyachi et al. ........... 429/218.1 (86) PCT No.: PCT/US2010/056876 * cited by examiner § 371 (c)(1), (2), (4) Date: Jun. 6, 2012 Primary Examiner Daniel Gatewood (74) Attorney, Agent, or Firm Muncy, Geissler, Olds & (87) PCT Pub. No.: WO2011/060433 Lowe, PC PCT Pub. Date: May 19, 2011 (57) ABSTRACT (65) Prior Publication Data A silicon-based anode comprising silicon, a carbon coating that coats the surface of the silicon, a polyvinyl acid that US 2012/0244391 Al Sep. 27, 2012 binds to at least a portion of the silicon, and vinylene carbonate that seals the interface between the silicon and the Related U.S. Application Data polyvinyl acid. Because of its properties, polyvinyl acid (60) Provisional application No. 61/261,520, filed on Nov. binders offer improved anode stability, tunable properties, 16, 2009. and many other attractive attributes for silicon-based anodes, which enable the anode to withstand silicon cycles (51) Int. Cl. of expansion and contraction during charging and discharg- HOLM 4162 (2006.01) ing. HOLM 4188 (2006.01) HOLM 4104 (2006.01) 11 Claims, 15 Drawing Sheets { 6; 0 U.S. Patent Jan. 10, 2017 Sheet 1 of 15 US 9,543,575 B2 100 1c 110 5 1 FIG■ U.S. Patent Jan. 10, 2017 Sheet 2 of 15 US 9,543,575 B2 Suspend Sitirmn Particies in So~vent to Create wpensm 2i 5w scats; suspension 205 210 smicata smpension 2"5 AW' nylano Carbonate to ` uspe ion 220 onicate Swperlworl :2.25 Comm an Awde Current. Coi~ec~ur With the Suspem ion 23£ Dry Anode Coating by Heating 255 U.S. Patent Jan. 10, 2017 Sheet 3 of 15 US 9,543,575 B2 -Suspend Silicon Parlic~er> in Solvent to Create Suspension 200- onicate Sw pension 20 Add Polyvinyl Acid t uspens- iiot.,§ 210 onicate suspension 215 -W are Awde Cuaent Collector With the &M.. en i n 240 Dry Anode Coating by Heating 245 Spray A€ o-de With Vinyle e CarbomMe-Cantaining Solvent 250 Evapotale Solvent. 255 FIG. 2 U.S. Patent Jan. 10, 2017 Sheet 4 of 15 US 9,543,575 B2 1600 14€1CI 1200 oo 41'5 200 5 1 2 3 4 5 5 7 8 9 10 1112 1314 15 16 17 18 19 25 FIG. 3 U.S. Patent Jan. 10, 2017 Sheet 5 of 15 US 9,543,575 B2 Oide number IG'. 4 U.S. Patent Jan. 10, 2017 Sheet 6 of 15 US 9,543,575 B2 FIG. U.S. Patent Jan. 10, 2017 Sheet 7 of 15 US 9,543,575 B2 100 800 600 M IKC 400 s~. MM 0 1 2 3 4 5 6 i 8 9 1-0 1' 1 12 13 11. 16 16 17 Cycb number SIG. U.S. Patent Jan. 10, 2017 Sheet 8 of 15 US 9,543,575 B2 im 1.02 Hg 11 0 wil Time, sec U.S. Patent Jan. 10, 2017 Sheet 9 of 15 US 9,543,575 B2 FIG. 8 si w 85-95 0 am 0 BEMMMMIF Art-WIC U.S. Patent Jan. 10, 2017 Sheet 10 of 15 US 9,543,575 B2 it X-ray energy, eV FIG. 11 U.S. Patent Jan. 10, 2017 Sheet 11 of 15 US 9,543,575 B2 E SM P11O U.S. Patent Jan. 10, 2017 Sheet 12 of 15 US 9,543,575 B2 PAA DEC wet PVDF 8 4 0 1 2 3 4 5 6 7 8 9 10 1 I dry 1 # U. 1 il 21 1 2 3 4 5 6 7 8 11 Young's modulus,arbitrary units FIG. 14 U.S. Patent Jan. 10, 2017 Sheet 13 of 15 US 9,543,575 B2 m d U. LL 0, U} VII j} f atl -rt -- -- - -- _'F""" 0 '0 . -#O ' f A q OftllO .' aft O v .n Z m U.S. Patent Jan. 10, 2017 Sheet 14 of 15 US 9,543,575 B2 ...:,. :{ ,....._ L,0.0 -T - ~k :. - = 1 5000 W..:... r 400 y .wgo 3£-o , 50 FIG. 1 2000. .70 -coated 1000 P,0120 01 2.50 4 6 8 10 12 14 16 18 Cycle number 50. ,.. ,.....100 4000- w >1 C-Coated 0z2000. -70 +:: R ' 1000 50 $$ : Na-CMC, W 20 YV~ } 26 8 1 14 1 6 1 ~. Cycle 5000, 1 oo M ~~++•~~~•~ t Ann 4000": 95 80 FIG. 16c 2000. C-coated -70 -94 1000. 4 ~.+1.(„~,.-.yr,~ YF ~~`~~'l~• ~.i "W 0'1. V , C/20 0 2 4 6 8 10 12 14 16 18 2 ~. Cycle number U.S. Patent Jan. 10, 2017 Sheet 15 of 15 US 9,543,575 B2 .f ... 4 ..• nw o ?i?+~Y 5000-100slttis{. ~^~t'~Y'~?•fJJJ~.~$~nv..tit.s.. rrrsrrr 40€0 <€ r C/20 0 , 3000J .......... _ .....f2.,.. ................».:.-- _ ~ ~' " u~w~wrwwwr, € FIG. 17a 2000" 70 . 1000 60 PAA 050 1 20 30 40 50 60 70 80 90 1 Cycle number 5000 , v.~.1:4 `.NLi.S)...\4 ~. ttiSti iiroi YS.F 4000 k C/20 3000'. 80 FIG. 17b 02000 X 70 5 1000< 60 PAS -coated Si 05 0 10 20 30 40 50 60 70 80 00 100 Cycle number US 9,543,575 B2 2 SILICON-BASED ANODE AND METHOD sion can thereafter be sonicated and then baked at an FOR MANUFACTURING THE SAME elevated temperature, typically 100° C. or less. In another example, a process is disclosed for producing CROSS-REFERENCE TO RELATED a silicon based anode. Silicon particles are suspended in a APPLICATIONS 5 solvent, the solvent being water, or a water-alcohol mixture comprising an alcohol content in the range of 0.1-50 weight This application is the U.S. National Stage Entry under 35 percent of alcohol to water wherein the alcohol is ethanol in U.S.C. §371 of International Application No. PCT/US2010/ some examples. Added to the silicon-solvent suspension is 056876, filed on Nov. 16, 2010, which claims priority to a polyvinyl acid which binds to at least a portion of the U.S. Provisional Patent Application No. 61/261,520, filed on 10 silicon particles in the suspension creating an interface of Nov. 16, 2009, the disclosure of which is hereby incorpo- polyvinyl acid-silicon on at least a portion of the surface of rated by reference. at least a portion of the silicon particles. In some examples, vinylene carbonate is added to the suspension so that the STATEMENT REGARDING FEDERALLY 15 vinylene carbonate acts as a sealant to seal at least a portion SPONSORED RESEARCH of the silicon-polyvinyl acid interface. An anode current collector, which can be,for example, copper foil, conductive This invention was made with United States Government carbon paper/fabric, or copper-carbon composite paper), is support under Agreement No. NNC08CB0IC, awarded by then coated with the suspension and is heated until dry. In NASA. The Government has certain rights in this Invention. 20 addition, a carbon coating may be used to, among other things, to coat silicon particles, thus improving the perfor- BACKGROUND mance of the anode. In other examples, silicon particles are suspended in a 1. Field solvent. Added to the silicon-solvent suspension is a poly- The various embodiments relate generally to binders for 25 vinyl acid which binds to at least a portion of the silicon anodes in batteries. particles in the suspension creating an interface of polyvinyl 2. Description of Related Art acid-silicon on at least a portion of the surface of at least a Silicon-based, lithium-ion battery anodes offer advan- portion of the silicon particles. An anode current collector is tages over conventional graphite batteries, thus providing then coated with the silicon-polyvinyl acid suspension and advantages to battery operated devices such as electronics, 30 dried. The produced electrode is then sprayed with a electric and hybrid vehicles, portable instrumentation, medi- vinylene carbonate-containing solvent having a boiling cal equipment, and space applications. In addition, lithium- point lower than 162° C. (in some examples the solvent ion based batteries are more portable because of their having a boiling point lower than 91' C.). The solvent is then relative higher capacity in relation to other types of batteries 35 evaporated out.
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