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( 12 ) United States Patent US010129975B1 (12 ) United States Patent ( 10 ) Patent No. : US 10 , 129 ,975 B1 Tabor et al. ( 45 ) Date of Patent : Nov . 13 , 2018 ( 54 ) LIQUID METAL INTERFACES FOR ( 56 ) References Cited FLEXIBLE AND RECONFIGURABLE ELECTRONICS U . S . PATENT DOCUMENTS 5 , 980 , 776 A * 11/ 1999 Zakikhani .. A61K 6 / 0023 (71 ) Applicant: The United States of America , as 252 / 175 represented by the Secretary of the 2014 /0202531 Al * 7 / 2014 Oya .. .. .. H01B 1 / 22 Air Force , Washington , DC (US ) 136 /256 (72 ) Inventors: Christopher Tabor , Kettering, OH ( US ) ; Nahid Ilyas, Lexington Pk , MD OTHER PUBLICATIONS (US ) Hotchkiss , The Modification of Indium Tin Oxide with Phosphonic Acids: Mechanism of Binding, Tuning of Surface Properties, Accounts ( 73 ) Assignee : The United States of America as of Chemical Research , 2011 . represented by the Secretary of the Air Force , Washington , DC ( US ) (Continued ) Primary Examiner — Timothy Thompson ( * ) Notice : Subject to any disclaimer , the term of this Assistant Examiner — Charles Pizzuto patent is extended or adjusted under 35 (74 ) Attorney, Agent, or Firm — AFMCLO / JAZ ; Timothy U . S . C . 154 (b ) by 0 days . Barlow ( 21) Appl. No .: 15 /939 , 356 (57 ) ABSTRACT A reconfigurable electronic component comprising a chan ( 22 ) Filed : Mar. 29 , 2018 nel having first and second ends and outer walls defining a lumen ; a liquid phosphonic acid within the lumen ; and a Related U . S . Application Data liquid metal within the lumen . A first electrical contact at the (60 ) Provisional application No . 62 / 479 ,620 , filed on Mar . first end of the channel and a second electrical contact in 31 , 2017 communication with the lumen at the second end of the channel. A predetermined amount of a solvent and a liquid (51 ) Int. Ci. metal may be within the lumen , and the solvent may H05K 1 /02 ( 2006 .01 ) comprise ethanol . The liquid metal may be selected from the H05K 1 / 09 ( 2006 . 01 ) group consisting of eutectic gallium indium ( EGaIn ) and (Continued ) eutectic gallium - indium - tin alloys . The phosphonic acid ( 52 ) U . S . CI. may be selected from the group consisting of decylphos CPC .. .. .. H05K 170272 ( 2013. 01 ); H01B 7 / 0027 phonic acid (DPA ) , fluorobenzylphosphonic acid ( FPA ) , and ( 2013. 01 ) ; H05K 1 /028 ( 2013 .01 ) ; H05K 1/ 09 difluorobenzylphosphonic acid (DFPA ) . The first and second ( 2013 .01 ); C22C 30 /00 (2013 . 01 ) electrical contacts comprise copper. An overflow channel (58 ) Field of Classification Search and a reservoir for the liquid metal and phosphonic acid may CPC . .. .. HO5K 1/ 0272 ; HO5K 1 /028 ; HO5K 1 /09 ; be in fluid communication with the lumen . H01B 70027 10 Claims, 16 Drawing Sheets (Continued ) ( 16 of 16 Drawing Sheet( s ) Filed in Color ) XXX 09 WWWWWW M * 23 US 10 , 129 , 975 B1 Page 2 (51 ) Int. CI. HOIB 7 /00 ( 2006 . 01 ) C22C 30 /00 ( 2006 .01 ) ( 58 ) Field of Classification Search USPC . .. 174 / 9 R See application file for complete search history. (56 ) References Cited OTHER PUBLICATIONS So , Ionic Current Rectification in Soft -Matter Diodes with Liquid Metal Electrodes , Advanced Functional Materials , 2012 , 22 , 625 631 . Xu , Effect of oxidation on the mechanical properties of liquid gallium and eutectic gallium - indium , Physics of Fluids, 2012 , 24 . Dickey , Eutectic gallium - indium ( EGaln ) : A Liquid Metal Allow formation of stable structures in microchannels at room tempera ture , Adv . Funct. Mater ., 2008 . Ladd , 3D printing of free standing liquid metal structures , Adv . Mater . 2013 , 25 . Cademartiri , Electrical resistance of AgTS - S ( CH2) n - 1CH3 // Ga203 / EGaln Tunneling Junctions , J . Phys . Chem C , 2012 , 116 . Li, A galinstan -based inkjet printing system for highly stretchable electronics with self -healing capability , Lab . Chip , 2016 , 16 . Paniagua , Phosphonic Acids for Interfacial Engineering of Trans parent Conductive Oxides , Cm . Rev ., 2016 , 116 . * cited by examiner U . S . Patent Nov . 13, 2018 Sheet 1 of 16 US 10 , 129, 975 B1 Egaln-OxPA FIG.10 *** * * wwwwwwwww FIG.1B 20T environment,ambientandlowoagaingrowthinonDPA Q FEATHEHEHE FIG.1A .10FIG U . S . Patent Nov . 13, 2018 Sheet 2 of 16 US 10 , 129, 975 B1 M w Withdrawalit Ethanol Withdrawal DPA-Ethanol Injection Ethanol Injection 2CFIG. 700um 500um um10031.5 700um 500um 100um D 9 . pos 1MHCIDodik 1mMDPA-Ethanol wwwwww Nextday. W. FIG.2B NextdayC .min10< Nextday MKM SAMMANN Nextday FIG.2A FlowDirection FlowDirection atent Nov . 13 , 2018 Sheet 3 of 16 US 10 , 129, 975 B1 ooooooongthereasonforcomoformos 472ev WF(eV) 1.004 4.36eV 4.20ey 1111 40:0 FPA EGaln GaOx BindingEnergy(CV) no worpen OH * * * * * * Air LE pogorooooooooooooooooooooooooooooooooooooooooooooooooooooo 9000003 FIG.3C ?????? Aa ??????OXOPA?? TipsProbe 1.72$01Qu/cm2 1.21$085Q/cm2 )b3B.FIG FIG.3A U . S . Patent Nov . 13, 2018 Sheet 4 of 16 US 10 , 129, 975 B1 Xxx FIG.4B w EgalnonGlass XXXXX w 20nm FIG.4A 12um WE UV-Ozonecleaned U . S . Patent Nov . 13, 2018 Sheet 5 of 16 US 10 , 129 ,975 B1 EGain Glass XXXXXXX FIG . 5A ** * LT WS HEZ XX 10111 * * 000000 EGaln Glass FIG . 5B U . S . Patent Nov . 13, 2018 Sheet 6 of 16 US 10 , 129 ,975 B1 EGaln Glass 30 ' s 1mM DPA w we FIG . 6A KU . Egaln Glass 130 $ ImMDPA FIG . 6B U . S . Patent Nov . 13, 2018 Sheet 7 of 16 US 10 , 129, 975 B1 20 nm EGain Glass 5 min ImM DPA Hii il FIG . 7A . : . ... ) . EGaln Glass 5 min im DPA 8 FIG . 7B U . S . Patent Nov . 13, 2018 Sheet 8 of 16 US 10 , 129 ,975 B1 EGaln Glass 5 min ImM DPA 30 s Ethanol Xxx * ** * www wwwwwwwwwww FIG . 8A 08 XXXXXX www X W Egaln Glass 5 min ImM DPA 30 3 Ethanol FIG . 8B atent Nov . 13 , 2018 Sheet 9 of 16 US 10 , 129, 975 B1 20 nm . Glass - Control XXXXXXXX Sin T?M ??? wa FIG . 9A PO 12 umW WW1000000 Glass - Control 5 min ImM DPA 30 % Ethanol ww FIG . 9B www U . S . Patent Nov . 13 , 2018 Sheet 10 of 16 US 10, 129 ,975 B1 105*1" 109#1° H,0 GLASSEGGIO-OPA . 1809 30$1mMDPA H2O 5min1mMDPA 17hrsEthanol 1081*FIG.10F 99*3FIG.10C .: . w H20 H20 10s1mMDPA SIEGin 5min1mMDPA 30sEthanol FIG.10B FIG.10E 27*3 106*1* H30 Hyo DPAmMmin15 FIG.10A FIG.10D U . S . Patent Nov . 13, 2018 Sheet 11 of 16 US 10 , 129 ,975 B1 11B holdingthe FIG.11C Tungsten dropLM mm AIRSDRAnalysis WASSA XPSAnalysis SingleRelectionATRDiamond crystal ImmersionofLMdrop 2100 200 insolvenusolution FIG.11A U . S . Patent Nov . 13 , 2018 Sheet 12 of 16 US 10, 129 ,975 B1 YkW . A . cis i wis www 30SDPA NativeOxide 111 FIG.12 U . S . Patent Nov . 13 , 2018 Sheet 13 of 16 US 10 , 129, 975 B1 www ti . mm FIG.13A FIG.130FIG.13B FIG.13C atent Nov . 13 , 2018 Sheet 14 of 16 US 10, 129 ,975 B1 FIG . 14 5 um X www KORY WW www ** Www * ** * * WY U . S . Patent Nov . 13 , 2018 Sheet 15 of 16 US 10, 129 ,975 B1 FIG . 15 WA XXXXX 0888 Wwwsos Hyo CIDPA U . S . Patent Nov . 13 , 2018 Sheet 16 of 16 US 10, 129 ,975 B1 6CuEt- 112311211119111711151113 BE(EV) 3 . 2pGa 47 FIG.16D ) . u. a ( Intensity 1920 PABLO 0.5mm 16A.FIG FIG.16B FIG.16C US 10 , 129 , 975 B1 LIQUID METAL INTERFACES FOR Gallium aggressively alloys with every metal used in FLEXIBLE AND RECONFIGURABLE electronics , resulting in unwanted phase transitions , ELECTRONICS embrittlement of solid metal circuitry , and general lack of control of fluid location . Pursuant to 37 C . F . R . $ 1 .78 ( a ) ( 4 ) , this application claims 5 There is no known method of keeping the oxide and the benefit of and priority to prior filed Provisional Appli - allowing it to repeatably flow through channels while main cation Ser. No . 62/ 479 ,620 , filed 31 Mar . 2017 , which is taining a barrier between the liquid and solid metal states . expressly incorporated herein by reference . The main approach reported to date to circumvent the negative " sticky ” effects of the GaLMA fluids has been to RIGHTS OF THE GOVERNMENT 10 use strong acids or bases to continuously etch away the oxide skin . While these methods have resulted in temporary The invention described herein may be manufactured and removal of the “ sticky oxide ” problem , they have not yet led used by or for the Government of the United States for all to practical integration of GaLMAs into useful applications governmental purposes without the payment of any royalty for several reasons . In addition to introducing highly corro 15 sive materials , e . g . hydrochloric acid , into an otherwise FIELD OF THE INVENTION benign system , etching away the oxide forfeits all the beneficial attributes of GaLMAs detailed above . While The present invention relates generally to physically under normal circumstances the diffusion of gallium into reconfigurable electronics and , more particularly , to liquid solid metals is slow , an acidic or basic environment sub metal interfaces for flexible and reconfigurable electronics. 20 stantially accelerates this diffusion process . To prevent the diffusion of gallium into other solid metal contacts , barrier BACKGROUND OF THE INVENTION layers are needed , which may detrimentally introduce addi tional contact resistive losses and processing steps . Better Investment over the last decade to adapt electronic com rheological control of the liquid metals in microfluidic ponents from rigid constructs to agile and flexible architec - 25 channels and chemical stability at the liquid metal/ electrode tures is driven by the desire to create strain - tolerant and contacts is paramount to utilize these fluids to realize the reprogrammable systems such as wearable and reconfigu game- changing capabilities in reconfigurable and flexible rable electronics . Few materials have shown as much prom - electronics . ise to transform these diverse technology areas as room - Conductive traces in electronics have historically been temperature liquid metals .
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