519722, 7:14 PM 4920045314424 - Method for producing stable suspension and powder of single carbon nanotubes - Google Patents Patents JP-2000531492-4 Method for producing stable suspension and powder of single carbon nanotubes Abstract tarlte om Japanese P20! suspension ct such eben ranotubes cortege dpered eeserily duel tube vig "edspetsedto form a sable suspension Trenaotes canbe used neces, pita Imvetor = SLAF an Le Images (2) by Wordwde eptentons | 2001 & 2002 sBAUEFWOGA 2008 US sppleaonJP2002576156k events @ Classifications ae ey 1» 012720/00 Nancecnalgy for mater or surface scence eg nanocomposite 2002.09.25 Prony PTAL202/000297 2007.52.97 Appcaton arte roorses7 Pu Ine: Patent ction (2). ety (68), apa even Siar socunect Pony an alte Apaestons xamal inks: Esc, loa Dossier, cuss aims 22) ide Depencont ~ srnaeted om Japan -Aretosfor producing an aqueous suspension of aon rates, comping ating. an aqueous meium. water olble polymer mater before or afer the ation of ‘hecathon notes, etd dispersing the nanotubes eseray one ote The above mathe compan separnghnto bes. The metodo lam whee th pole! t hycopilepabmerofathernsturslor tte arin A poces for rong uenlngle ty catbonraraunes cami rosea an aqueous suspension of ton raretuses acco lm ai removing Wate rm sal suspension & The metodo la 3, whet reovng ie wate conptises evapora, ophizig or tet. 5 Thamethe seearang ec, heen the concen of he ry pohmerastederbon nanatbes nthe surpansan spo GS by weigh Theat of ny of cine 1105 where mesa o ayer to carbon nenounes inthe range of 206-2, The meted accorsng oan one of clams to 6 ween he polar aed rom pobescchager adplyestidee, Tha metiog accrsngte anya of chins 1196 whan the pare awatenelbl sitet sora The meth acodngto my oe receding ate, wren thepohme comes qu eae, cage, pec pelyalctuane cl alge ald eean ard devate thes 9. Temebod aco 6 ‘hin @ wherinheplmerea hare poker habe suspension of citkor moles Fociced azodngo ay one eins 10 0. The powder eran rene, were th ponder cortans a pole med wi the cuban neotbes 13. The powder of cla 2 whee the pars sont ob the bon napatbe. Use of bon Tarotnes scavenge clan 17 012 fordepostig cabo neice arequtes pen on 3 a apport Use of carbon nantes aeoreng carn 1 or 2 388 {erie or growg sen tl or yd mati slice and earbonnaneutes. Ue ofthe carbon nanolbes according to cin 1 or Yas inrcig ape fora poor mata 17 Use of efor narctues acorn o lar 6 whean the palmer math isan alstome 13. Use of acabon nanotube accoréngto am 11 or 2aga candice connecter betwee wo elec dees 1. The te aecathpta clam 18 wren. ae of ol of the dees te hatodeconic devices Use fa eaten rartube ‘Sccorting och 1 or 12 esi voling the formation ofan yee 2, Us according eae 2, heron he een pening 21, Use asadng ta el 20, wherein te eciqueie wea, Description trait fo Japanese ecmcael) (ooo) ‘he present ie retest exfoliation cf crbon naretubes ad to a mead fer prosucing a stable aqueous suspension of con raratubes. The preset verton Dring costs thn ayer, mele machines and ithe produto of conooae, [oackgounse hitpssipaterts.google.comfpatorlJP2004531442Aen?0qJP-2004831442-A a0519722, 7:14 PM 4920045314424 - Method for producing stable suspension and powder of single carbon nanotubes - Google Patents tooo) Caren anctunes, other inthe frm of she aaled nanotubes (NT) orn the fom of mutha parctubes (MNT) hav typical ameter of ew arate std alegthofup io ten of micro Polat eade leven ibs present ts excelent mechanical an decal oper ha Yaugs module oreach TPs MS Dresehaus ot Science of Flerns ane Carbon Mantis, eacemi ret, ie, NewYork. 1996) a 10° Aer anons acter deny of andl excl ‘tara statity (Selene 2617998) 1744, WA dear ta) (ooo) Nenotbes tendo clump however most esate erm sa well separated ube of eer SWAT ar MNT Carbon rentubesare cure atthe cece of ‘teal an experiment woe (8 Tanz tal, Nature 96 (1987) 474 EW Wong eta, Saance 277 (1987) 1971. tooo) “he exceptional mechanical ropa of carbon nanotubes have aac high pes fort us a refrcing filers noma matics to frm igheih stronpmesoconpostes. To achieve these exzectstos. good mecaniceleaping betwee the pave! met ands nanotubes, epely sess nse ate (0005) ‘second ren of reserch expected fr carbon ances, speci SWNT, mle electors Her, SWNT wl pate ieee: thay wl sare a ace components nranoszed devices sot es eater varltr and elezvon-nitig sources, Aerabve, hy cou are a molec Wes comectng varus tooo) However ecropances re often foundation thasetal predcions ad experimental sbserved proper of crbonnancuses,Tereatonithathe erson arouses tendo eytallae in fopes hat become eagle io anetwor Vande Wal rteracos betes the we bes alg ham ancconseuenty bundle ‘temo a etal petit can ona 10-50 tes (Live al, Sere 89 (1998) ) 1259) Theatre ofthe rope exeabntyghee Het annie Xp ‘eater diagram Diller aggregtion eee of eon nitrites ave ben founda flectbo the lca nd mecariabhavr (Sai tl. Py. Re. {on a4 (20009) saplomerned ops are bt an do net vb expect aera propa sch a lemon ney, even wher wel aed tooo) ecetworkharocuesonnaneive hansg an onenaton evened Mater (200) 579, such a FP). Oe ofthe novel approaches a baedon he ‘ress of dene ered aay of exon neclbes ona sid suport nome of the pubished stun each eta ope rae thn aig ube, The ligne rope shows per properes compared what woud be expected om 2 wall saad ube. Theres alo ard for sufacoteatmerthat wi prove beter (eooe Recent 2 pstaytesieagment post fo carbon nanotubes was described Vig ea (8. Vg a, Scree 290 (200) 1291. Inte metog as proccss SWNT are pest aque salon of te onc satan! sagum dee sft (808) 3 concn es low 36 035% by Woh Te csr repeisthenrecondentedina shear flow eo fee and bona of webbed rope DISCLOSURE OF THE RWENTION [Problems tobe aoe he vent) (ooo) work noniualope nt ope in rte bes Aeeordng, oe abet oh preset neon sf pres mats for prodsing a tne naveoce ieprsin of vida npteted con rartubes. tet ecto he preset en ata provi wallespa'sed aon nanotube ny form tise a6 store ad han, anc ready rus m2 wide vary of eppeatins ed techloges nus electrons ae materi enateetng tobe Yet another nec of [seas fr Sling the Peles) looto) {Summary oftenvertion) ‘Thu reer ition vie forth xfoltion of cron ances ne te mon fw wears pera oan aque nei foc afte oe ‘adn ofthe carbon nantes thereby separating he eafoonrartubes nto esertallyincvdual ube thal are @sperse And producing a sable aqueus ‘spendin of crhon ranches. The poimeteder eno te carton ies andere th the tog frees betwen te tue, preventing fe epepaton red ‘cancer stale polecote bon naptube suspension tat ean b euch ae SS weigh pret or more. Enables th formato of Poa cose bes reparation ofthe suspension water-soluble pone, ete ythete or aura nwhih ese the weght ato payer earn narcubes Inthe ange 0S {020 leprefoe. oor ‘Therese iertion als proviesndidul wet eparte ator rartubes in powder fom hal can be easly epee orm sable suspeon This form Issimgeto handle nd alone quck and easy roducton ofa suspen havng is wellseprted, o-applonetted bess the eae olume an ence abon. ‘hs fem ofrantibe is convenient or slags, handng. nd medat use, The vention farther eles tha ue of pabmescostes angle non rants eeweris ring coags hn yes molec machines, and De maruacive of composts (oor) ‘The above and ther ete and advastages fhe prevent veriton wi be ete understood wit ference tothe oso state embodiments and wi reference oth accompanying cawige toois) (Dota desrtion of te vention) ‘herent ientrs nave dove al sme pone compounds lw ete teductan of sabe equous suspensions of vida carbon naotbes tht lenvig ay arose aos te nero ise stored. bareon his expen nang ven ne fies) hata pales fbi capil paar. = sorbed on He ropes io induce aebound, Th repulin preven the tes For agganeraingalwg exflton he cbr rartube adrmationa a “usprson conning welleeprae polerconte rl ees loot) “he watereakle poland th aroduced powder ofrantubes nlsng the ayo burled ops aera wih Water or aqueous sluin nay order THe ones then sclestd of rite amie eutngin a bekinktke suspension. Ths suspension cotaing the separated peymercoated ube ead oe Interest uepein e tble rmon loos) Supra wehave fone tat he suspension obtained canbe rad alnewn manner nde pon obtaned canbe upto Sy wl orm) par water or coi een. Has ben fund tobe ely epee tthe dated polymer cote caton tube concerti seling ng revi canbe used ft the respersion. The eouing suspension also saber anh, The yng an the rerovalof water om the suspension of crhon nanotubes can casi ‘reparation optical cetieton and ita, toore, htpssipaterts.google.comfpatortJP2004531442Aen? 2n0519722, 7:14 PM 4920045314424 - Method for producing stable suspension and powder of single carbon nanotubes - Google Patents ‘The polymer nt inthe present veton pees yophiiplyme: ore preter a charged polymer feber tra or yeti cig and te weight ato of id palmer carbon nanotubes is 1 Ris nthe range of 020. he olyere selecte For plsercarisesané plete. The poe cen be a wate salle sible palmer oor Ine prefered enbosinen of invention he puytr comprise loots tne refered enone gm wabic(GA) is Snore in denice water io sconentaionf 19% ad the apredaved eben ubing ited io nconcerston (of 3% fotoned by soneation eroam tempers. The sancti tne preferably om $20 mines. loore, ‘Na ter stern dont cause te ropes to seperce to nvidaltube, rd conten he negate resus fe i’ a, athave the persingefect on cense ‘epeementoned stove. Litte orn zaton hassles een our the preset rerio (FG. 3} and ter reearchers (8. Vig etal, Sere 290 (2000) 39), (ter pes of surat, exept 0s, evn mmonum cli (CTAC dedeeyninethylanmnoiun boride (TAB) pertaebyereoxotyee dodecyl ‘thar (2, entra plete oie 10000) Was chacadt ves concentrations Noe ofthese maleated aac depres of arouses sq.esus sauon, nd aver he bs of then under conan whee CA resutedina SOK cape fare carbon narlute, twas ol even sossie ‘oslablze te 0.35% (elt ecetin wate suspension fhe bale (ooz0) node et the agategaton tate ofthe aon naotubesin the perso te crbn be conte with GA was abject to Kray eeatig measurement. The ‘ypesl pes saractrng the inestune pking inthe eanufacre SENT rope dsgpenred wth he palymercoatedeaaon eg accord othe prece Irverton (8 I.) The concoct of ie stable persion was vestigated using eryegei nanan electron microscopy ayoqene TEM) Cyoperic TEM images showed wal spared tubes 02 im lamers F. 4), Sch ubes canbe clay cere suspension Bch before ad fr gad ‘esunpenste These obeereans emonaute hat CA aGseton eauedin complete dtupon of We ubedo‘ubeineactan ite aystaioe ope. Adon ‘odes of adseptansrvied byl mensurerert ry SWNT ponder Tis ry SUM poner la shows character pre duno th earn arian of rec 6 50), (oor ‘ecodngy. he presen nvenon voles aig watrsolble pojarc mati tan aqueous meu efor te ato atom nantes hereby ‘seprnig the raraibe io seein eucalaber Gapeeed. The prose ever eeso 3 ethad fo poduce an aqueous surponean which aon rapsuses ate Saperse Furthermore, the tert venton rite ea metodo producing unentared ey ean nantes company Eapersingnantunes ‘an aquoussluion ofthe paar and erg the asperson, looza) “he pest iron ke reso te uso aon nantes na suspended or pore tte may appt hare senor by ene carbon tubes required (ova) ‘Based oe above nrg, the preset evento ls fr etn he pope fa sre ue ard comparing Ito foetal predictors em apace paint ot vents ety produce srl dry powder a wel separated ple spacer a bong equred in separsog asl tube from ae-syrtasze (ooze) ‘Theabityopredice suspension o powder ote aber ranlubs wit defined popes and conttled concerts ian advntage fib ny kw ‘echigue fr handing se astroutng ude and powers to conve carbon nanotubes te ary Albws 86 noduction othe ste nan fom ang amour hae ec ppleatnin ining coatgs th ayes ad molecular machine, loves) ‘She th poleradetedon the catban tbe sts a compat aia inrovenentin We aly af he terface between the rant ds mati an be cove. These ong-tan pomes can serve as achslon promoters hat ee othe fomaton of @hgh aches near between etude and he pote mati Ris wll rown ta tesa edhsie fer nea of ober saihtened interface on te rset 192-103. hich 8 out 10 tes greater ‘fan the ature eery fe ctbowentan plane. Thx none espe herent lets trong nigh adheaeintvaceetween the aon ie nd shepolyner meta (ooze) Ile well kno i the ld f mates scence ht composteraterals compris partles of ne component homogeneously dpesed centnuou hese, ‘oetcome the sbong adhesin between he parle. The polmezosted aban nanotubes aosodg othe rwenn canbe used rect the teducton ot ranscompostes suet excler sprit. Accor, he teaertnventan fare rateso the se of carbo anatbes nthe manufartire of roel ‘campostes. ene pltered enbodinert carb natubes serve a eharig opts te Done mats The pete polet mete nts embedmetie an (ove Inwas farther reeled atthe suspension ofcarbon nanotubes prosiced as cesred above showed the presence of ban neotbes wit lameter of 9m (FE {As desorbed above, sagle wales crbonaeotubes exit exvere exelent ele proper. The presen inven therefore dso lete tthe depesitn of opts ef mance poner or nao 2aerion a sent esto na estrone aay where ranstuns cen save a atocontacts Tepesetswenton ‘hus reletes to tieune of aeunpension ponder of bon nantes tomate a onductive const! betwee wo eect dees, oe of bath of wih ate rarcletone ovine (ooze ‘The peent ero alto pois 2 metho for depositing cba nanoibes ool uzpat ihe recued pate or ae tenlatforthegronth of lla crystals or ahyerid matron an eaten nancies eae othe se fa suspesion of ponder of notes (ooze ‘Theinvenan rer rae tothe we of suspension o: ponder of ctbon nnclubet ns teeviquelvohing he oman fa thinly. The ecniqueis prefer (ooo, “hemechani by hic te poner stables tenants seprin bases on he rieducon of repulsion between th asrbed poles oth ceeuotatc tdenvopicreulsone deo he conpostion ofthis mista wi ph aby case the itoduton a single metas o he padi of olmercoatd tutes has the mass preducton of ead nanotbesased adatves tbe usesin the fest. esas tn ayes molecu ‘machines enfored astetere and econ. Iean teove tro cbfales son he wy. Embodmere loom ‘um artic Samal coved npr waters 15 (elt eter) and 3% by wolght of eroded rartube ponder (rom Carles, Uverty of Ket, eng Keni USA Up lo, 2 mf Di ture was thet sonal far 20 inte. Ahomogencov person of SWNT ws based, This usps with hitpssipaterts.google.compatorlJP2004531442Aen?0q=JP-2004831442-A a0 bi, carapeenan pectin palyslctuanc tle ai chan and derivates tee.519722, 7:14 PM 4920045314424 - Method for producing stable suspension and powder of single carbon nanotubes - Google Patents Ink appearance was sored at ambit trpeatie and pty chee fo visa changes The dpataon eraineduncanged ater man, nthe rarest ete wnen certtged et #500 pm for 39 mas tonsa) rapt of 10 mL he suspension reparedaein Exaile 8 20m faced tout 7 grams of ine lek powder of pommarcoteeSHNT Tis powder es repersein 77 mt of pure water pean nkike homogeneous disperses pasion was Stabe. loos) ‘he fotoving sleionswara prepared) 2% GA (8) Sk GA () 5% SDS (0) 158 SOS (6) 5% CTAC an (F158 CTAC.Oinized water wa ua SDS anc GA were purchased om Suma end TAC wes puchase om Arh. 1D mL each soliton wes laced ha as be ado cach ube was atded Sa ofthe payne” ‘aed SUNT prepared an Exaile ar the mitre was soit. The gs ace weretien sted mbt eerie wi cartira checked uly or anges. ne case of SDS an CTAC de sdiversepear thin mites thous, espe ther high concern. nthe ease of gun aabe the suspension Enbodimen¢ (oo ‘The asproduedrantibe ponder (rm Carole wes arazed using Pils #¥ey poner decree (KV 28 mA Wh Cu Ka fadaton waveengtd= 0154 1m) ne an rashte-nonciromate(PU-I0S0/ 70) an aracarzeby ray azar; hae he azaternpvectoring=4n/ hn, aise sonar ale FG. ashows the ope stucwe of SWNT to-dmetlonal ang tlce Wh latice constr Btw ab evdece of ultlae aghte abject content wth Tess tal (@ Thess eal, Sconce 273 (884) 489.1 shows a wdeangle ea apectum of FG," b saws a wide-ngle xy specrum ofa polecoated SWNT Depa ceseibec in Example The set shows he eflecon of he C/N cals usedin nanotube sytess I canbe seen thane eae rete sen In FE Tadsappearin Fe. basa reat aspereng he rope ect i ndvdal sgl crbon anette The twa Fekscorespending to graphs wouleect ‘hata cena amount tmutnatednapatubes were resetin the epoticed ponder Embedimert loos) “hemieeseop sta ofthe SUNT Asperon was rvstaatd ung eregeirnamicsin econ morscap evegene TEM) The perf Example? ws reapers deinzed water at 180m it 1, oe sto ofthis person was paced ona lace TEM gion FORMVAR ad vile in gui tan The sarc wa Imapedat-178¢ using» J 1200 TEM aqupped wh 2 Galan 826 ealsag tat rere testa afte cbc formed nt ln sha FG. shows» ‘Syopeic TEM image oe redapeteed navcube, Wepre bes of 2 rnin Gare ae ley vile (arows wih nF), Tek mal nnolbes can aloe observed aan wih). (ons) ‘Thess produced ranlube pander (tm Cle was raved caning econ mitosopy ISWAISCF, OL tang 254). Mcopaph fA sulted a reesvenannibe powder aw exible ropes in aml onete twos. The arow nats sng ope, (oosa ‘The powder of Caste 2 was computed wh GhtyFTR messirrent FIR spect of pallets made wih Kf pre GAs) 4 SWNT powder) wate measiedon¢ Nicole Protege 460 specromte FIG. 6 shows that GA aes to SHNTS, (oon Mocatns an vans ate posse ite avertion desorbed above a isttedn he exarphs. Tho preset veto canbe apple o the dparson of carton natin manufactured vous way naa fr varus aude pone The nates can bese a8 suspension of a3 powder The naatiber can de used as meee eves, telate for growing estes comporets of congoste mel npg, comings ha yes, alec aches, std ke Thus. is undestoos hat he vote eat be rated thervise hana peel dezebe iin h cape th appended ls [Bre desenton ofthe drags) loo) ‘BREF DESCRIPTION OF THE IGURESFIG1. fo) deangl xa specru of ope stuctve wt atwedmensioral bangle of asproduedcatbon arouses, ne) Ratio of 5% by wept gum abi (CA) 13% by weigh SWNT 1 shows waeanale ay spectum of = ponder odiced fom aaaliten having ‘he folowing fruit The eet shows ne refeton of eCo/ Nextt vee ne te of erbon ances, Fi 2ie SM mcragach of a sptete, a racied rote powder where he om heer angle pe FC. 3chows te eppewance of 0.05% (neh percent) SWNT dspersonnaferer aqueous soon afer 2 months (A) 2%GA (8) SEGA () S05 (0) 15% 505,(8 sucTae, (9K TAC Gis aeryogeie TEM ictogaph tad fom a depetsion of SWNT. The dspersin was pepaedby lepers ay once of coated cesbon nantes pare watr The powder was madeby ying an aqeeussluin of 15% GA ard 38 NT Arousal exe SWNT (SCa/ Nica (0) eatin came lace supgot (0) and mutate nencubes (). Fl Shows FTIR=poca (pre GA an) red SWNT ropa accra to HG, Samples wor prepared by mxngthealevant materia and Kan aratioat Patent Citations (12) - Pubtonnaber Pranydste Publetion Fay Te Fam rations saasesaoa tececnae 15741204 ——~FulPhotoFmCoLid Pree for paduing capes having wil of way mse saaseo7aa® wrzeza2 wwr4m203 yan ‘Aqueous method of mlroenoapsuatn ard capsules ssren62a" oa6o11e T896T149 Eastman Kodak main dement hang an dectealsconductve yet Cenpany hitpssipaterts.google.comfpatorlJP2004531442Aen?0q=JP-2004831442-A ano