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The National Ha Ett Luciditate THE NATIONALUS009780386B2 HA ETT LUCIDITATE (12 ) United States Patent ( 10 ) Patent No. : US 9 ,780 , 386 B2 Kwon et al. ( 45) Date of Patent : Oct . 3 , 2017 ( 54 ) COMPOSITE FOR LITHIUM AIR BATTERY, (2013 . 01 ) ; C01P 2004/ 04 ( 2013 . 01) ; COIP METHOD OF PREPARING THE 2004 /64 ( 2013. 01 ) ; COIP 2004 /86 ( 2013 .01 ) ; COMPOSITE , AND LITHIUM AIR BATTERY COIP 2006 / 16 ( 2013 . 01 ) ; EMPLOYING POSITIVE ELECTRODE ( Continued ) INCLUDING THE COMPOSITE (58 ) Field of Classification Search @(71 ) Applicant: Samsung Electronics Co ., Ltd ., CPC .. HO1M 4 / 9091; HOTM 4 / 8605 ; HO1M 12/ 08 Suwon - si , Gyeonggi- do (KR ) See application file for complete search history . @( 72 ) Inventors : Soonchul Kwon , Hwaseong -si (KR ) ; Dongjin Ham , Hwaseong- si (KR ) ; ( 56 ) References Cited Victor Roev , Suwon - si (KR ) ; Dongmin U . S . PATENT DOCUMENTS Im , Seoul (KR ) 6 ,355 , 377 B1 3 /2002 Sheem et al. @( 73 ) Assignee : SAMSUNG ELECTRONICS CO ., 7 ,282 ,295 B2 10 / 2007 Visco et al . LTD ., Gyeonggi- Do (KR ) (Continued ) ( * ) Notice : Subject to any disclaimer, the term of this FOREIGN PATENT DOCUMENTS patent is extended or adjusted under 35 EP 1806805 A3 7 / 2007 U . S . C . 154 ( b ) by 33 days . EP 2717366 A1 4 /2014 ( 21 ) Appl. No .: 14 /818 , 665 ( Continued ) (22 ) Filed : Aug. 5 , 2015 OTHER PUBLICATIONS Korean Office Action for Korean Patent Application No . 10 - 2015 (65 ) Prior Publication Data 0067600 dated Jun . 7 , 2016 . US 2016 /0043408 A1 Feb . 11 , 2016 ( Continued ) ( 30 ) Foreign Application Priority Data Primary Examiner - Jane Rhee Aug . 8 , 2014 (KR ) .. .. .. .. 10 - 2014 -0102625 May 14 , 2015 (KR ) .. .. .. .. .. .. .. .. 10 - 2015 -0067600 ( 74 ) Attorney , Agent, or Firm — Cantor Colburn LLP (51 ) Int. CI. (57 ) ABSTRACT HOIM 4 /90 (2006 .01 ) HOIM 12 / 08 ( 2006 . 01 ) A composite for a lithium air battery , wherein the composite COIB 21 / 082 ( 2006 .01 ) is represented by Formula 1 : C04B 35 /58 ( 2006 .01 ) HOIM 4 /86 ( 2006 .01 ) MC N (1 - x ) Formula 1 (52 ) U . S . CI. wherein M in Formula 1 is at least one selected from a CPC .. HOIM 4 /9091 ( 2013 .01 ) ; C01B 21/ 0828 metal element and a metalloid element, and 0 < x < 1 . ( 2013 .01 ) ; C04B 35 /58007 (2013 . 01 ) ; C04B 35 /58021 (2013 .01 ) ; HOIM 12 /08 ( 2013 .01 ) ; C01P 2002 / 72 ( 2013. 01 ) ; C01P 2004 / 03 26 Claims, 29 Drawing Sheets POSITIVE ELECTRODE TERMINAL - NEGATIVE t22 ELECTRODE - E21 - TERMINAL - 19 L - - - - - - - - - - - - - - - - - - not- - - - - 23 US 9 ,780 ,386 B2 Page 2 (52 ) U .S . Cl. 2014 /0234733 A1 8 /2014 Roev et al. CPC . .. C04B 2235 /424 ( 2013 .01 ) ; HOIM 4 / 8605 2015 /0079485 Al 3 /2015 Choi et al. ( 2013 .01 ) ; YO2E 60 / 128 (2013 . 01 ) 2016 /0043408 A1 2 /2016 Kwon et al . (56 ) References Cited FOREIGN PATENT DOCUMENTS U . S . PATENT DOCUMENTS JP 2001256977 A 9 / 2001 KR 1020030056544 A 7 / 2003 7 , 691 , 536 B2 . 4 / 2010 Johnson KR 1020070109118 A 11/ 2007 7 , 767 , 345 B2 . 8 / 2010 Imagawa et al . KR 100814817 B1 3 / 2008 8 , 129 , 050 B2 3 / 2012 Kim et al . KR 100926794 B1 11 / 2009 9 , 236 , 641 B2 1 / 2016 Shishikura KR 1020110138380 A 12 / 2011 2007 / 0231704 A1 10 / 2007 Inda KR 1020130050711 A 5 / 2013 2008 / 0070087 A1 3 / 2008 Johnson KR 1020140002628 A 1 / 2014 2010 / 0311852 Al 12 / 2010 Kang et al. KR 1020140006639 A 1 / 2014 2011 / 0059355 A1 3 / 2011 Zhang et al. KR 1020160018337 A 2 /2016 2011/ 0129739 A1 6 /2011 Nakanishi WO 2005044754 Al 2011 / 0223494 Al 9 / 2011 Feaver et al . 5 / 2005 2012 /0077084 A1 3 /2012 Christensen et al. 2012 / 0077095 Al 3 / 2012 Roumi et al. OTHER PUBLICATIONS 2012 / 0115048 A1 5 / 2012 Roev et al . 2012 / 0141889 A1 6 / 2012 Lee et al . Jang et al. , “ Li metal utilization in lithium air rechargeable batter 2012 /0276459 Al 11/ 2012 Im et al. 2013 /0108934 A1 5 / 2013 Lee et al . ies” , Journal of Power Sources , vol . 244 , 2013 , pp . 606 -609 . 2013/ 0112915 Al * 5 / 2013 Kim .. HOIM 4 /58 Kang et al ., “ A Facile Mechanism for Recharging Li202 in Li- 02 252 / 182 . 1 Baterries” , Chemistry of Materials , vol. 25 , 2013 , pp . 3328 -3336 . 2013 /0133923 A1 * 5 / 2013 Leis . .. .. .. .. HO1G 11/ 38 Ottakam Thotiyl et al ., “ A stable cathode for the aprotic Li- 02 174 / 126 . 2 battery ” , Nature Materials , vol. 12 , Nov. 2013 pp . 1050 - 1056 . 2013/ 0147439 A1 * 6 / 2013 Takahashi . .. .. HO1M 4 /667 Yuasa et al ., “ Discharge /charge characteristic of Li- air cells using 320 / 134 carbon - supported LaMn0 .6Fe0 .403 as an electrocatalyst” , Journal 2013 /0209348 Al * 8 / 2013 Ludvik CO1B 31 / 10 of Power Sources, 242 , 2013 , pp . 216 -221 . 423 /460 2013/ 0224609 AL 8 / 2013 Lee et al. Extended European Search Report for European Patent Application 2013 /0330639 Al 12 / 2013 Lee et al. No . 15179902 . 2 dated Jan . 18 , 2016 . 2014 /0011101 A11 / 2014 Ma et al. Yeh et al. , “ Direct formation of titanium carbonitrides by SHS in 2014 / 0093771 A1 4 /2014 Wang et al . nitrogen ” , Ceramics International , vol. 31 , 2005 , pp . 719 - 729 . 2014 /0113175 A1 * 4 / 2014 Zhang .. HO1M 4 /624 429 / 145 * cited by examiner U . S . Patent Oct. 3 , 2017 Sheet 1 of 29 US 9 ,780 , 386 B2 FIG . 1A POSITIVE ELECTRODE TERMINAL wwwwwww ? NEGATIVE myslimanima mengendara marunong ELECTRODE Ñ TERMINAL c og 23 U . S . Patent Oct. 3 , 2017 Sheet 2 of 29 US 9 ,780 , 386 B2 FIG . 1B ine e 130 140 120 myyty ondersteunendetandenendooronderhanadandidalamkeadaanberkenaa Hitradictiiitiiiiiii renginiai 1507 dat d iiiiiiiiiii iekinderkandungandankembang REARRER iiiiiiiiiiiiiiii RRRRRRRRRRRRRRRRRRRRRRRRRRRRRRRRRRRRRRRRRRRRRRRRRRRRRRRRRRRRRRRRRRRR U . S . Patent Oct. 3 , 2017 Sheet 3 of 29 US 9 ,780 ,386 B2 FIG . 2A SAI 200kV x200K SE 200mm FIG . 2B SAIT 30 .0 % V x200 % SESTEM 200nm * atent Oct. 3 , 2017 Sheet 4 of 29 US 9 ,780 ,386 B2 FIG . 20 SAIT 30. OKV x7QOK BESTEN FIG . 2D SAIT 30 .0KV x300K SE O ONER U . S . Patent Oct. 3 , 2017 Sheet 5 of 29 US 9 ,780 ,386 B2 FIG . 3A SAAT 20 . 0kV X250K SE FIG . 3B GAIT 30 . 0kV x250 EFSTEM 2008 n' S ' fu?Red PO' E ' LIOT jaays 9 JO 67 SA 6* 08L ‘ 98€ TO DIM DE 33 : : : : : : :: : : : : : : : : : : : : MODENYS 8000LX is 1 1 . 16 DIL & : : : : : : : : : : : : : : : : : : : : WU002 MODELS XLOSX 9 W918 . .wool . U . S . Patent Oct . 3 , 2017 Sheet 7 of 29 US 9 ,780 , 386 B2 FIG . 4A SAILOOK XOOK SE 100 FIG . 4B SAT3000XSON CESTE n' S ' fu?Red PO' E ' LIOT J??US 8 JO 67 SA 6* 08L ‘ 98€ TO DIJ OP : : : : : : : : : :: : : : : : : : : : DIVS DE ANO X100LX aus : : : : : : :: : : EIXE T 19 WOO DIL VG TT T TTTTT . OSLIES SVO 2K % 20 : : : : : : : : . wwodeBWOCZ U . S . Patent Oct. 3 , 2017 Sheet 9 of 29 US 9 ,780 , 386 B2 FIG . 53 SAT 30 .01 XSSSTEIN 700sets FIG . 50 SAU 30 .0KVx1000R BESTEM $ 0 One U . S . Patent Oct. 3 , 2017 Sheet 10 of 29 US 9 ,780 , 386 B2 FIG . 6A 50 nm FIG . 6B U . S . Patent Oct. 3 , 2017 Sheet 11 of 29 US 9 ,780 , 386 B2 FIG . 7A : :: : : : : : : :: : : : : : : :: :: : : : : : : : : : :: : : : : : : : : : : : : :: : : : : : : : :: : :: : : : :: : : : : : :: : : :: : : : : : : : : : : : : :: : : :: : :: :: :: :: : : : :: : :: : : : : :: : : :: :: : : : : : :: : : :: : : : :: : :: : :: : :: : :: :: : : :: : : : :: : : : : : :: : :: : :: : : :: : : : : : :: : : : : : :8 : : : : : :: : : : : : : : : : : : 08 5 :13373797999303 : : a :. : 2293939393555555ESX99X999:797379199299393 :i 77777777777;: : . : . : : : : : : : : : : : : : : : : :: : 19:53335559 : : : : : : : : : : : : : : :: : : :: : :: : 11111111111111111 : :: : :: : :: : : : : : : : : : : :: : :: : : : : : : : :: : :: : :: : : : :: :: : : : :: c : :: : : : : : :: 37 237 : :: : : : : : : : :: : : : : : :: 225323UKE:: W : : 1353373 . 17 : 1:35 FIG . 7B : . 17 0 . 23 : :: : :: : : :: : : :: : : :: :: : : : : :: : : :: : :: : : : : :: : : : : :: : : :: : : : :: : : :: : : : : :: : : :: : :: :: : : :: :: : :: : : :: :: : EEEEE : :: :: : : :: :: : :: : : :: :: : : : :: : : : : :: : : : :: : : : : :: : :: : : :: : : : : :: : :: : : :: : : : : :: : : : :: : : : :: : : :: :: :: : : : : : : :: : : :: : :. :. :: : : :: : :: : : :: : : :: : : :: :: : :: : : : . : : : : : : : : : : : :: : : : : : : : 7:33 : : : : :: : :: :: :: : :: : : :: : : :: :: : : : : : : : : : : :: : : : : :: : : : :: :: : : :: :: : :: :: : : : : : : : :. : : : : : : : 3 : :: : :: :: : : : : : : : : :: : : : : : :. :: : : :: : : : :: : :: : : . : . : . : . : . : . : . : . : . : . : . : . : . : : 11. : . : . : . : . : . : . : . : . : . : . : . : . : . : . : : : : . : . : . : .: . : . : . : . : . : . : . : . : . : : : . : . : . : . : . : . : . : . : . : . : . : . : . : : : : . : . : . : . : . : . : . : . : . : . : . : . : . : . : : : : : : :: : : :: : : :: : : :: :: : : : : : : : : : :: : : :: : : : : : : : : : : : : : : : : : : : : : : : : : : : : . : . : . : . : . : . : . : . : . : . : . : . : . : . : . : . : . : . : : : :: : : :: : :: : :: : : : : : :: :: : : :: :: : : : : : : : : : : : :: : . : : : : :: : : : :: : : : : :: : : : : :: : : : : :: : : : : :: : : :: : : : : : :: : : :: : :: : :: : : :: : :: : : : :: : : : : :: : : . : . : . : . : . : . : . : . : : 5. :: : : :: :: : : : :: : : :: :: : : :: :: : : :: : : : 33: : : : : :: : : . : . : . : . : . : . : . : : : :: :: : : : : : : : : : : : 333333333333333333333333333333333333 :: : : :: : : : : Map data ww7333331:33 : :* MACM 300k . 327823223333333323395995555577777773329991797423EEEE U . S . Patent Oct. 3 , 2017 Sheet 12 of 29 US 9 ,780 , 386 B2 FIG . 70 Map data MARMOKHTOkyanus Lun FIG . 7D XXX Map data B MAC 2010 A300 . U . S . Patent- -Oct. 3 , 2017 Sheet 13 of 29 US 9 ,780 , 386 B2 FIG . 7E wwwwwwwwwwwwwwwwwwwwwwwwwwww 40 U
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