5112722, 153 PM 44P2003054821A -Purficaton, allgnment, and quasi-rystalization of carbon nanotube - Google Patents Patents g Purification, alignment, and quasi-crystallization of carbon nanotube Aboot PROBLEM TO BE SOLVED: To provide thod of purifying and ali sare tubes(CNT) eosenaseys sin patie snge layer carbon nanotubes (SWNT). and to provide carbon nanotube quash 7 pubtahed unexamined patent application “Shel peut oy SOLON Hon eapontng Nad tn Shien tte pat aspect oon 9 ch trea sented eon ogo onde rece een mens ‘hen Wo actrees Oe npg gree Invent: Koko Ke, Hist Kabr, cho Teste SEH, tuo Yara Us, Masala, xe Worle aplictions ‘Appleton JP20012454808 events 2001-08-13 Aspleton ls by Say Cap = stat 2012407-11 pletion grantee 2or297-11. Pubes of sPasv2en082 Ine: Patent tations 2), ce by (6, Lepalevers Smtr Societe, Ponty se Related Rpheatons Exel ins: spacer Obl Dos ious claims (66) ide Dependent = ranlate rom Japanese {cisine 1 rong sot contin carbon nancies Produtng an ai tretent tre by petorming aire on he aot sample Canin decstng. nd ‘suspen te aid teatneat ure Generating a acdvemoved precipitate by eruging decanting. an teauspecng the wodvemovrg pecptatet orm @cabon narotbe corcetvae and eveporig the carbon rarctubecancentate Armetiod of punifing en algnng carbon rarstubes, which comprises produ alone crben narowbe quesersil. 2. The method of ela further omprsng exvacig the quascytaloremove hgh yerogensted carbon te exacting stp boing permed ater ‘he evaporina sen. The method described 2 The ratios of chim 2, wernt erating stp compranssosieating te uasoystal 4 Natiad acca to cli 2, ‘haacteraed inthe erating stn compass ung wate ae sven The folowing gnaal mthod where the extractant hes an N soup Method scoring oem 2B RryeRreaNih he OLR, Rye rel HO H Ngo Mae Hah the forma, n= 114), gHene nt frm = 1104 Nein Mya HrusCH aa AN (CHa Ie elected rom te fou earsitng of 8 The method usta comeies ar anesing sap of temovrg urcionl groupe Bonde the arb narattes the anealing sap ‘The muthod of daim2, 7. he matbad of clan 6, herent aed step compra eng the quasirysal.8A mad econ to claim 1, characterizedin th a eep of earyig out an ace refx compiesnsodueng concerted ie edna sald oot 8. The method of ln & whan te concerted We ace ae concervaton of about 70% 10 The step of caning ut the ae eux comprises about etka secorcng to clam cmrecerzed in tat tie caied mt 310° Cor about 10 outs. 11, Thematod of lai 7, wherein eld tp of perorning an airs furor comprises paforing ay ee eft t about 170°C forabout ‘hours 72. The mth ter compres coal the aed reatmant treo oom erga Ne ‘The method of da | ure emariinghe sep af well De soo, wheres the ste of welling priormed pire he step ol peorming acs ref 4 The step wetigcomariees aig the too wth a olen of DMF and pute wae, ‘The method according telat 13.15. Thermethod of cain 4 wherein the wating step comoiss mang the sot wth asluon of OMF and pure waterin 1:1 eo 16. The process of eran decartg and esuspencing the ac eatment mite comprises cnfugng he ald veeent mare at abot 5000 rp fo about 2 nutes. The ‘method acceding 01.17 Themethod fla t wherein the steps of contin decanting ane resuspending the 20 eatment mire ile decaring by innate superstar. Method. 18. The tod of am 17, wherein the stp of daring by dang the superatant comprises fusing aed row, ht rown or esos spernatantThemethed desribes. 9. Temettod of ei Ileana tes of ceniiing, decanting and reaapenng the ais eatment mire campriges hiupssipaterts.google.compatentJP2009054821Alen ane5112122, 153 PM 44P2003054821A -Purficaton, allgnment, and quasi-rystalization of carbon nanotube - Google Patents ‘renupening np water 20 Therethod flan. wheteln he steps of ening deeaning, rdresuspending the aed estment mitre aerepeated 3 tines. 2, The ep of cotiugng decanting ad resupercng he areted mite ae repeat nt a black superar ppeas ae cent elec spent beng an scdeemoved prepate The method accord to lain 1, characterized in tat 2. The meod of cm 2, fue among aang he lack sypeatant 23. The ste of ‘centring, eating ard resuepending the aciremoves preps compres centiigg te acd-eroved eet at aout S00 tpn or abou 29 minute, 2, The meted of dam 22.24. The tp of certfugna, carting ad resuspending he aeldtenovesprsptae corres resuspending the acldtemoved precip ln pure Water. 28 Themathed of clam 2 25. he maton serarng te clom 2, cnerecnized inthe tps of cerning Sean an rauependng the aieremoves pects ae repeats times 26 The sen of contin. decanting ane resuspending he aeromaved preepate comprare doaning by dang a ack superatany, whichis = ‘won narotbe corcetate wher the caronnanalubeconeentte 2, The method of lain 22, wherein comprise fest voe. 27, The method bin 2, farther compiig the step of thckeig the carbon rantube concent “Tne method accadng to 6.28. he etching step comprises adding the fst vole ofthe carbon nantubeconcnrateta = - No. 28, he mod of le 27, compsng redoing toe eecnd value tetis 2.29, Themed of lam 27, rer con ube wieanined pate epleatn 9 Furtecentfugia the seven 0350 form sediment, washing he secimert wth pure wate nT part by volume of th carbon nanotube concen ated resuspension $0 35 to produce a careenratea resuspension, Resurpenag he sedenin vores of wae cninfuing he sediment wsnng he sedimen, 20, Methaesecorng to cli 29, chrtctorzdin Wa the sep of resuepending the sade cated 04 before the evaporation step 31. Tha rrthas of chi 25, further, comping extatng he qusicrystal arrow igh hyingeated carb, he acing sep Selb performed after he eaporang sep. The reo debe. 32. The ‘method of din 31, wherein the exvacng step compiz sonicatng he qusizrystal 3. The mathd of lain 31, wherein the exten sep compsse sig watt selvert 34-The folowing genera steps wher tie exvacon step comps ous ‘characterizedin nett comerses sing a clvnt ofthe forma etd accorcng to clam 31: Rae te fol. RANE Rls HO Nine Mean the orn 1), yan fn frm, = 1204 Nie Noa HrCHTaNTa AN CHCl ee Ie selected rom te grou constng of. 38. The matiod fea 31, further coor an annealing of emoeng funnel tous tached the earon nanotube, he annealing ste boing perfoma ater te erect ste, 36, The method of lim 35, wberrntheanresg step comieshestag the essere 3. The eveparston sep is out 700 Tor and about § Tor Process acorgt hi, charctrieain that itis eared out t 0°. 38. The method f chim where the eafonrarotuses ae singlal earn antes 28, Proving so contig the aon raratubeseubjecirg he soto an accra produce an arested miatrremoving a om theater to poduce sn acigvemoved precise Generating ast carbonnanlubeconcnraes Iu by centiluping the aisremovedprecpiate at sped of 2200 pm or mare tremore patales lage tan 20 nm Produc. erituing the concenate to produce a peste, alec he eile, nd resuspending the precpaten eid ge a et ‘ume of second oarbon nanotube concentrate. 2, edn the second carbon nanlube cocerrte to produce an algned cafe nanotube eusiysal method at bung ena shin carbon nanctbes,camorsng veparstng ate rate of /hosrto Ie! hour 40. The maton lem 3, iter omprsirg lacing the carbon ranotaeeunslerstlin an eector end performing extraction wth s kent to raravempuries 9-The method according 91, The method of lain 40, wherein sald exacting stp comrisespesfrming extract with water a sole. 42. The step of pefoming sis Iie paricalaly characterize ata it eampisescayng ou he extaton wth Slt athe genealfomule “Te method ofa 40 wher Ry Rage. the FOU, Ry, Ryo Rp LO HN ge Ma 104 yan nt formal +110 Nein NaH oan AN (CHM In selcea ram he top eating of 3. The method af clam 39, where the steno prov soot comprzes provid soa carping siglewale eatbon rarotes ‘The step of pefoming a are comprigs subjecting he sat to ef a bout 110°C or about 1Dhows, ed the refuxig ashe 170°C fr abot TO hates rode an ecdtestes mire 4. Te mathod acordgto cam 2, characte aha 4, The tps of roving ad om the eld Westnet te nude: central ‘he acd estan mitre to produce a supernatant an sediment orton rening the supernatant hau: te sediment portion 42, Themethod of clan 39, compris washing the presiptat wth water an resuspeding the sediment orton nwatero produce te sclé-emved presto. 46. The method of im 45, frther comprising ‘peaing te step of remove he ai om he acid ventana ni the sapeatan ud urs black, 47, The ech stp comprises adn th rst volume cf the ‘aon arabe corcetatetothefratvoime, 10 No.40The mated of ln 2, ning redcing tox econ volume hat 20.48 Further comping he sep of sting ssi concentra ai step of ting sid concent beg afte sald tp of ertaugg aid concentrate and fad stp of elect sid recat $0. Method aoctdng a clam 39, characterized that Ms ‘arid out befor. 49. The metod of em 7 where the step of esuspening the prec need comprises resuspending a pero fhe prec in about pats of ‘the lu. The method acoring 10 38. $0. The metodo lam 3, urher comprising the step of annealing te carbon nanotube quasrysial.s1. The method of eam 50, eran the tp of aneaing he carbon nanotube quasirysal comprises heating the carbon rartube quaioystal “The method deserbadin 52. The evaporation steps aout 100 Tora about § Tor 49. Method accor toc 29, characterized in ta ti cared ou a <> forma than Shou 58 Asura of crbon nanotube bundles coupled ta each the ech of ‘ne pay of crbon nanotube bundles beng eanged aan engl of tnaton wih respect ah alghneat pial ess frm atBubon ana carton nate bun Quastanstl carbon nantes where the dstruton has aul wih all maximum of ks than 24" over alengh of ymlong he aged pital ex 54 The eaeon notte bundle Strbuton nae full wih stalf max oles than 70° ‘Aauassystal according clam S358. Thequasrystalaccerding te dain 88 wherein the carbon ranoube Bundle bon as full ith thal maximum of "t09” 5 The quays according im 2 wher ebch fhe pay of earbon anole bands ha a dameterin he range oF2 100m 57. The quay aesortng to ‘him 53 wheres eae of be paaliy of aran naraluse burl asa dameterin the range of 210 20m 8 Each of the pirally ofctbon nanotube Brees compres. 5 A.quasiytl scoring te lm 5, characterizedin hat tha length nthe rarge 1 mto 10m 9. The usslerystlacorsgtchim 53, hten echo he ay of eatbon nanotube bunds hs fnghinthe range of 10 pte 1 em, 60. Furth, 401 ym #16 100, ‘4 Acusiystal aceon to ci 3, characte in tal cmp a volune nthe range G cm <*>, 61 Furth 0.001 yn #0 Tem Ma he orn 54 Avolume cnaisting orange of 10 5. «i SI, wher the quis forms curved poon 64 Each ofthe etn nanotube bundle compriees play of eaten ranctibes, each fhe eabon sapoties having kes 2 100 01001, 6. Having alength inte range um. Tre quslrystal secorang ote 3.65. A yérogn storage med comprsing th qascrytal ofthe carbon nanotube acoréng tary one of cams 83064 and hyarogen ‘edue inthe quascrytal 6, Te hyérogen storage eum according claim 68 wherein te hyroge is stored between at last woo the pray of crbennantibe anaes hiupssipaterts.google.compatentJP2009054821Alen ane5112122, 153 PM 43P2003054921A - Purification, allnment, and quasi-rystalization of carbon nanotube - Google Patents Deseription naa rom parent Detaled Descriptio fh nvntion (0001) ‘TECHNICAL FLO OF THE INVENTION a TECHNICAL FIELOOF THE INVENTION The pesentinvertin fats oa mead for uring and etgnig carbon nanotubes (CT wren canbe singe wale carbon rancubes(SWNTE), muted carbon nanctbes (MNT) athe ke More specially te preset inverion eep- ‘eran aed dense hich one used as a hyrogen storage mediom ora an electrode of aysroge fl oa, [Arti erpurhing an aging SWNT to anv voli effet qusiyaale Furthermore the patent invention alates carton nantuse quays race bythe meios (0002) 2 escrpton ofthe Rleted At b. elated Art When sytesze using ac lsharge or ase abate, CNTs and mare special SWNT, ae CN Ins commonly ccomosrie by other earoonacenus tere a exalts Used fr | growth Purlemlon of CNT nd SWNT i exrraly porat for sre instil paposee Moreover even ar beag pres, SHNTe ate uly Sud i aardom, high enanghs state. Haver fr ame applleaons, slgned [SWNTe are expecta tha a supariopevlermance to at of entangled SHAT, Terfors,abymen of SUNTsi lo vry parent er scene aia purposes SWNT mage by are cechrge sntese [Anumter of mathads have been deelped forthe putin of bu few of hem can be easy sealed up. See for name the fllonng artes: et a Ad A Toi et a Nae, vlume 383,679. Page, 196; Ton etal, Phys. Che 8 103,1974 3997-7 Objet App Suet Se 657 nesta, Sr Met 103,2480,1 rn. 112.35,199;8. 5h ‘vay eal chem. Phys. Let, 2 192,420,199; Band oto Appl Phys. Val 87, 29,1998 ‘ear 6. 5. Duesberg etal Age Py 2.457.117, 1998 5.0 setg etal, Syn Met Vlume 13,2484 1958, Holger etal, Ap Lys. A70vlomes, 88 pope, 2000. Japanese Patent ai-Open No, 1120809 by Th any methods have als ben developed forth pureaton of SWNT thesized by laser slaton Hower the soot produce by ars charges Coniering that WNT gully psy, atx composition ete. ate lee rom hose of at shez aerate methods have Been develope opty SWNT syptheaze by lee alaton, at these methods have een developed Net apoiabe 0 WNT ‘Sncetherateaf soc gerration by ar dacharge smc faster than heat of sol generation by laser blatin he Appa een fcusng on ltd att ‘methods fr stat too y te dchage ing, Foloweg he main tee to renoverrost cubon img, be published priclon meth an be clase to teurypes, Aion ret saparatn; trometry end ald onto. ‘Te frst ype of SWAT eing proces ia odin, Tay and oes ae SWNTe produced ate dacuge whe he row mari seal efued wh watt before coxdston, Repos tat xan be pre by xdaton in ar For exams K. Tet al, Net 388, ol 57,196; ot eal, Py 4: ven 8 101, 1974, 1987 Year Tob tl gp Sut Se (857,145, 1995 and KS. Japanese Patent Lad-pen No, 10120408 by Toi et ‘See ale sue 1998. This meted ia simple and econacl proces, but rt now thas ony Been succes scaleap as netbeen done, maybeand matisS ‘Tis probaby because t's tic oxize and remove te ararpous carbon by acrtain method before damaging te WNT. Aslghtyimeroved tod eter {orem reszons or atedon ga oxdata, nas alo See scent forsmallsamplevlumes. A Hous, ‘ym Mat, 103, 2480 pages, ‘corn, 172,p.35 198, Furthermore, for ume ata groups he esl lady the abovemethod could ot be eroded, B. Saino eal, Chen. Ph ye Late 282 £2,189 hance ese manage re Lvlable tn mal amounts of raw sot 100mg. Prt ot ‘The second ype of SWNT purieatin proces is dect sepaation Sand etal ea aoealed ae-step SWN, ‘The procedure forthe T pieaon process is anounced The Bardow process ivoiescetrtugig or mirofheng the aw stn aguous soliton the presence of aeatene soca §.8 ae ta op. Phys 8, Volume 7.17 Seepage 71998, The method is exremely snp and saighfrwar Homeve: the problem wih i proses i tha the product bined roto safacory hiupssipaterts.google.compatentJP2009054821Alen ane5112122, 153 PM 43P2003054921A - Purification, allnment, and quasi-rystalization of carbon nanotube - Google Patents pure Requces adnan by i xan ard als Vesa is over life scale. the cate ofr Sie, eles i partly [Seu because carbon prices ca eal Bock he mire: making rubeequn iatonextamel tft “The tir typeof SWNT pula proces I chraratography. Duesberg and ther ar SW _Ammetia of sire erlsion choreography hasbeen developed to spate NT frm ater eabon pares. Ths method wa aiid to sth sutectnt-spanded scr eciented sot GS, Duesberg etl Ap Phy $457,117, 19965. sary etal, Sy. Met Vlume 13,2488 1995 Hongr tal, Ap | ys 70,59, 2000, ying ts method, SWAT having high purty and unfrm gt an be obtained. However. the ited cliv frantbes an the ‘rablty to eae up we mir dawbacks ofthe method bled examined pate appleaton ‘The fourth ype oF SWAT penton paces side cxdstion Tha als refx poeadie was fst oped bythe Rie groupto puny soe le Forex, Leta Sees, 2801 253, 199% and Liv etal APL Py, A, 29,1996 Since thn many ther researchers have caine 70 wo 0 vol pute SWNT by ae dachatge srhecs by using erent eacon tres tempers, ed concenveong, nd postiteatment ecnigues suceeded, For example, “1 hen eta, Sane, 262, 9.95 1998; Vacar et al, Sy. Me 1 309,248,198: 89), Alsahm etal, Elerochinea ‘esa 45,451,200: ‘ketal, Cth, 38,1723, 200, "eared, Lu ta Chen. Py. Lat 1826365, 2000. Regarding the post:reetment ofthe cle rex slr themestaracive ecnique stems tobe he cose flan techique which can salve the ‘logan pote nth ne fitrtonprcess. Using his workup several rams of SWNT reater than 90% purecan be ebtaned in awe. However he labore _rosssfow ration system andthe ge volume of ter soon contshing siztactate-nece than 20000 mes te arcu a soot tobe purest ‘See Scene, 22 page 95,1998. adaon addtional pufeton by oxidation wth song al taton and vaca caenaton lrequed. Therefore, the method ‘exremely complatd to scale up, outleseme, ad takes ive a wel as manpower Pure SA ebainedby ofthe sboremetieds sae usvalyburcled end entangle extremely andomly Therefore a eddion othe purfcaton method desorbed above, nadtonl alignment tpi requte. Ferman apaliatins, such as hase used inte mechanical an lean insti algns SWNT are expects to outperform te perfomance ofrendomly entangle SWNTe Such excelent efomarce ie SW Duetotnenigh degre of wsatay of NT Aged pe er hyerogen storage \WNTe may provide addtoal aaron tesin he rt pace Between the rarotubes and buns, and thus may provide alate age amber fet thet ‘cas ener at adsorption ses ise he nantes. ‘Several acsques have been developed lr aging SWNT: Thsetectiquas cn be cid into fut pes nas CVD growth mecha atetching: magnet stetchng and eapscciation D tecnologia to SWAT gow on Se, Far exo M, Teas et al, Nate 2366 521997, Creng eta A ol. Phys. Let, Volume 72, page 3282.1 598: R Frank etal, A. eter Vol 12. 890, 7000, This etnies staghtorwars an straightfarwas naling SWNTe and may Sit app ction napa devices, However is notes ‘tat alned SWNTe repos by ths ecg af goodon in catsn anal areas andre ually unalnes Moreover the packing degre of liza SWNT is 0 “The seconde of SWNT lapment method = SHN Sot rw sot contain T ana pole comooses contain SATE ate dawn Fe exargh CHK, Phy sche, 16,2454, 200; ‘And A Haggenmual etl, Phys. hem. Let 39,218, 2000 SN for peer compostes [Aerts hav en mae to use ifort acacia strengths fr andthe palyrar mati. The SWNT-PMMA corpo rl rocesing metos wa aloes ‘sued on sin mactaricl drbwing mechanism Please refrto be same book though ths composite develops = igh degree of mechaieal tng the SWNT content of thee aes uly low “That ee ten TOR-th hows that SWNT i a the punt of eyetalltin [Athi ype of SWNT abgnmet meting outa song plane magoei eld-25 Tes wh ilring the rantube / Tito suspension. 1338.9. 14.2001 sing such amatiod Wehr era ‘We seceeded inobaring a thin lm of WNT. This thin fm exhibits use optical properties an fers antral cleavage plane paleo te magnetic ele However the msrstuctr of he thin fim ths prodoedhas net yet ben deraneated, utherars,suretants (Ion) have Been use wer he surface ae rary of SWNT SN elton ‘Tocrestearetatale state f Til hese surfactant are at completely washed they may have alage impact an he statin of he a prot. Futhermre ‘tute challange wah ete he poe of eng up the tan and alignment proces, bu sng extreme age magnetic els tat aren ey hiupssipaterts.google.compatentJP2009054821Alen ana5112122, 153 PM 44P2003054821A -Purficaton, allgnment, and quasi-rystalization of carbon nanotube - Google Patents ‘The fouth ype of SUNT algnrentmstod based on calf atsocinlon One research ru has diameter of0 1.12 p89, 2000 _Aer hamogenzaton, SWNT ca ef assoclte det the fomation of ome cf thecesuperbundles athe saver. trace wah te ald of vesoun suet androlonged sting. However he araur of is supe-sunle ctaned i very smal (nuchless than 1 mg tom a stata amount of rg. sne this superSundle forms ely at he aeslvent intros, Woreoe, the dene of agosto by Canna si abe eh rem for provement Infurter tts using ths type ofalgnmant meth, fine "etal SHIN matetl-bving& with of 0.2 mum and alengb of 08 .muim-was observes by STM Aer lerng te SHIN collie suspension using the srectant SDS, te SWNT materl Was ebarned 2 @ sol eneppedor 30.2 bm pre size fer mek ea ‘carbo, 1728.2 See year 00. However Unis © bled examined pate appleaton -As canbe zoe fom the foregoing these methods ar compe and produce SNNT “yea” srcture tht ae emalin size an poo aed (oo) Problems tobe Soe bythe vertone Problems Saved the resent vertan One obec f the preset invention |e to provide amethoc for pun ang along (NTS Nore sect, one purposes Isto poise tod for pring sndagning CNTs hate saldup wh ihe ficieney anbeer apachy ‘Another objet ofthe vention sto purty ang align CNTs based on solution chemist whch allows the mtadto be eel saleups ra aes he CNT ro qssenstls, Move specfely i arene obacive to make hgh alors large CNT gusta, turer objectives lon ‘Yet another object of te presertnvertin ite high dere oflage estan’ seucure fe, quas-eetl nasil, aly seledp, nd corolble mane, a compare rlted art methods. To prone the SWNTE algedth each ote. (0021) (Mears for Saving the Potter dn tere achieve te above ar ote jets, the present iventon provides © Prove is ametbod fr oustyng nd along CNTs, which comprises peodicing a eancentated NT slzin and slowly evapratg he slo By slowly ‘evaprating the ONT concerts, © The vn oer Wane tren ofthe Ns roves sfc efor the CNTstoslelion. The ower he eeaporton of he CNT concent the longer th al lgpneat er ofthe CNTs £0 haa west gned qtsenytal cn be gtneraed Thais, the quaserytlis ers ans contains few ers that deviate rom the aed ‘Fauabcyslal ae weld ad relat dene and hus havea igh volume eiceny which makes the vel for aplatons such as hyogenetoage or ycrogen fe cellecuodes SWNTe, MWNTo ee cap be sede the CMTE af the methos. is aplable to CNTs syed by any ret auch a le ablation Fue nro achieve he above aida objets, a mstod far puting and aging ‘eon naotubes is proved incu: prov soc contain cafbon nanotubes and subjecting te soc sample to an aleve Feming en acistateg minwe by cettupig. decarting, and resuspending te aeléreated mature to form an see reraved precpte cenrfuging, daring, and Produongacrbon ‘anole concentrate by esuspnng an evaporating the eabanraroubeconcetne st an eapartion rte of 200 boro 1 er hata pads lon “atonnanatbe qunsestle, Te achive he above another ote, thre further provided ametod of purifying and alin carbon nanotubes comprising powdng oot contig the carbon nanatbes acid refizing of he sot Generating an aiéreated mir removing an aid om te aidreated mire to produce an aciéeroved prec ‘cong the created recat a speed of 2000 rm orig Proauinga feat canonnantubeconerrte by removig prices aera On Cneeniating the fst arb nnolabe concent produce a concstae, ‘enttugng the cancentate to produce a precptate Then ‘colectng te presptate ed esvnendng the precipite a ud topoduce afr volume of second cfban nanotube concent and te second to rasiee gre ceson nanotube quasieysale,Eveporat the carbon ranctbe concentrate arate of 200 ml Rout er hout Furnes: otdr to achieve the above and ote objects, aaron sarotube gusset proved whch includes pitty of earn nanotbe bude Bonde 0 ‘echother.adtbuton ofeach of he platy of carbon rartube bundles. Are ranged at an angle of rclnation wth respecte the aller prinopal send the _Serbon of arn anotbe buds ha fl wth al sir ofl han 24° ove ath fm alg tb abgnmen panel ae Peter ti ful wit at halt macmunless than 10°, mae preferably nthe range 3209 (0028) ‘The above and ler objet and adratags of he presen venton wl bec mre appre by deseing in etl the prefered enenplary embodies ofthe ‘resent vention wh refrence tothe aceompanyig érening, utying ad abing CNT The CNT ray be ay eatbon nancube suchas SHAT or MINT Inthe ution spe se ated umber onthe se fhe flow chart whl onthe ght ide the removed pei ae shawn In abox with dashes ox. The maa ow a higghed nthe mid of the ow char highihted bythe sald box Fee raw materi oot cotaining the deed caton nanctubes i colecte, Tis aw soo canbe made yay known method suchas a eecharge and et lation. Ths emaodieat fhe ventions slaor-chemsty based and th emgeratue ir, qual pury and mex compaction ofthe deste eeron anonaes erate Tat sn anotbe-ontanng soot canbe ved In Exe seen rer bel ths ot conte SWNTs anes cased‘ panty tr ag te SWNT nto cust, Second n stp 51 the sete subjected to aide reuxtoremovermtal parce (om feshcatayet) and amorphous carbon. Durng the aise re process the soot mite wth the acide ensure that he metal particles and amerphous carb nthe soot andthe eld hae acharce fem a sliton, Before the sets hiupssipaterts.google.compatentJP2009054821Alen siz5112122, 153 PM 44P2003054821A -Purficaton, allgnment, and quasi-rystalization of carbon nanotube - Google Patents "bjected to acdc ei, epecil ia svong tidied in the sede refute sone a alent sa ogi any aaoeatalet contained inthe 00 when ‘mined with 24 Kimay be esa be wet ith rire of water ad wae. The produc al his tape the aid Weaten ise “Tira oder trove rt oly the seat als the metal an aarphos earn ares the aie resent murs, he a reatment mtr i subjected 0 Iahuld be auficent to rerove parle above 200m. General «speed of 200 rpm or mores sable Tire ino cela ng atti uct to replat parsebove 20 im. More special ale centage aisle mister sep I, tht areddl-bowa et supernatant above the Seamer. Thirds supematat qu certains acts, metals and amorphous con whe the sediment cota ie desed exon narctabes The edlsh ‘brown superatartisthe rained decanted, kovng sediment. Next ths secmerts washed wih ure water andresuspended, Then necessary step 826 ‘aried oit again unl he supmatnt quis lax fer carnfugton Aer cenrkagtion when the superatan tars bce the siperstan ora he fom Fourth the blak upematant cortanng he aiéemovedprecptate ram stp 82s subjected to centrifugation decantation, and resuspension instep $3. More pectic se0 S| ‘he tack superman contig the scented recite fom 2s decanted trove the desied blck supernatant. The lack supematant here compe the desired carbon santubes and waersalube carton hile the sedan compres Aenoparile wt ize above 20 nm (crbn perl and of metal coated wh ‘ator. The dceted slr thn wash ith ater a eauspended Te retuspension then cntsfuged agin. Thi proce tapes at nea ntl te ecient thoroughly removes anda bok spernatanterar, Ah ete bck soln decerteg, tts, poured ove cancerrted and then allowed 0 sete for several hours otha deste caon nanotubes are precited, urn the etng process, sme ofthe carbon nanotubes aggregate fromthe bundle Aer edimetatan,topoduc sediment. ‘When the solitons errfuge again he precntte now contain th desredearon nanotubes The precttes ar then washed wehpurewatertorerave ary esta eopures and entapeed in wate, This resvapension sa carbon panchbe concent Fith instep 4 the carbon nate concerted quits ted are ar subjectt lan reatment fora shrine and when hi irish, geile 10 a snd 50°C. The goat pil sd etaperaon, The slaw the evaporation fhe catban nanotube ence the longer the egret tne of the ‘caf notes ia apt Te evaporation ine should be eutlcntto alow te carbon nantubes a seal tothe dented isa az, To obtain te dened ize of ‘won nanote qussestls wh ahi degree of lore evaporation tes inthe range of 200m hour to Ier/ hur are tered. Thee he generated pressure and terperature canbe changed as long 2 the evaporation erate, ‘Sahn step 85 te aged ype cabo Nanotube concentrated sold quasieystale are ure puriedbyexracton Tobedone More in dt about hgh hydrogenated earon Algoment pe ceo remove alluch rest mpurien \Utasoncgeneted soe for Bonn rantibeenched sold quotas tracts stage, a Sante xvactoreg 264 “ung al. cher Mee 12 volumes, 2 p. 718000, "Yousan Atti stags, the rch brown slo From the ssovenentsnd aligned carson naclube-eiched sald quays ‘Separated butin th cate the sabton es han 209m f wate ‘Contain sokbie carbon parle, Soren containg N roupetha in general Feary eee salve nthe formula, Fy AyaghndR “renal HOH, Hye Ne Haste formal 0 £14), Gey heren = 14). a ro Mirnyi Al (Cryer Is ereneyffeciven renewing hyogerted impure, there Als water or moths sorts ade othe abovementioned gourcontaning ake Fina instep She quaicystalecontanng etn nanataes avin funtion roupsaresubated to a heal annealing sep in xderto rear the uncon! rouge The oduct of the aqnalng steps x sarge a puri ard aligned carbon ranotbes, or quays Tha hesting ue hs ana sep must Delage ‘rough oremove the furconal group a eauortl ine, but not high eraugh osarage he desired carbon ranotbesn the euasieystal Theta gee. ‘We temperate irate aneaing te ca be shvtaned or te lrpeate is owered, the arnealg tine canbe lengthened “The questa shown eirged in FIGS, 2-4. Qasizysal mean tht is mates reserbles a crys but does nol havea prec pro si frown in the ofthe preserve, General esta super to quater but externa eu obtain ysl wth sulcely ge SHAT, Theclore the prenent vento ereerts ama vance ovardethe goal of eyetllzton Furthermore, quaseytalamayhave advantages oft cystalsin certalo els such ‘ashytogen storage. That for example, quaserytalemey prove aitnelhycrogen assertion sts, andeletvel simple charmesto rete these ses ‘The quaseystl produced by he meted ofthe pesat overtone ‘NTs each avog a aster inthe range oft 10m Ireleng abunde ot. More preferably te burde of CNTs each hae aameterinthe range 210 201m. The ameter ofthe bundle censtiung he quastystal can ‘beaded by contig ta evaprmton te fhe CNT ences. That i th loner evaporation tna hati, the slomee tba vaporton at's) he lege ‘he arte ofthe CNT bundle contiuing ne quasiyta becomes, The quasirystal lc vais inlnat depending onthe evaporation rt and te lrgth of CNTin the nial soot. Gea the longer he CNTE inthe saring soothe longer tha qusloystal Aan longer eepraon tines produce longer qusiopsala sin tha coe of lamer. Qveckrysals ruced byte above tho rts ‘ntherange of pmto-0em, ad pretertiyintherange of 10 unto 1 en, Tomake such a quaseytlthelengh af the CNT in the ile! prelrablin the rage of 100 ta 10 hiupssipaterts.google.compatentJP2009054821Alen ez5112722, 153 PM 432003054821 - Purification, algnment, and quasl-crytalization ofc bon nanotube - Google Patents ‘The volira of he quaserysalis selected according ois ee se ‘Yu can Thatisinthe case of hysiogen storage quasiesalare sores Suter btaing sual nergy deny volume othe steed Temuethave a eutable vue ut Napa From te vewpoit of knees, the male he qusiystal Is eayto sor hysogen nthe caer ofthe quae. Tharefr, trogen soreae| ‘The volar of ciasieysa for ein energy dena and na coniertions Iezapeds nth agree However in gerara he evaporation tne ong ‘The ong, he ger the volume of te qusiystalis. Ard ot “Te longer the NTA nthe soo te moe quart value ‘ng Vole of uesleystal produced by the present invention bled unexamined pate pian 10.001 yn™*To 1000 em "Nib he ange of ‘atlas nthe cae of ystogen storage, ie velume of guasieystal 0.09 1 um?™To 1 ont is preferably win th rage ‘Toprodue sich a refered volume, the startng oat selena Fortes he method ofthe present vention achieves igh degre of gpm of he CNT buns hat mae pte usslertal.CN [lgomen of Tunes wie desorbed wh eferece 0 FIGS. 1, 328 SEM photograph ofthe pure SWNT qunsirysal smo. 2 but wh he aligned ‘inp ans shaw in FE. FG i graph showing th buono urd inside te questa Te epee eights deste by the tl wid a hal maimum (FH of he dstebuton ofthe bundles siete quest. The derbuon of the bundle i etamnedbaseé on the wanton angle of ech ‘una from the alnmertman axis Xx shown nF. The anges Measured foreach bundle Te numberof bundles having tha ik angle with respec ta spei angle 3 counted. The sult ae shown nthe raph of FI 4 ‘nti the wai represents thei arte fhe Bune fom the main sxe of algnent whl the ya represents ach fhe specie cares sown or he xan [Aan angler along the aipimert an ofthe qasierystal 1p ‘ver veoreverts te numberof bundle, Wi eile ove smallWHM, because the eller the FWHM the ges the degree of alignment of the CNT bundles oun the qusiysta. Therefore, FWHM of 24” tess desl. FAH is preteblyless than 10” As canbe ste tom FICS. ane the qusiystalf the present vero hes 2G wih 2 FWHM of "3° Actives dirintion of NT bunds, Tati, th CT bene inte quae ofthe present iverson ae igh aligns th ea ater anshave a much haber ‘spre ofalanmen tan he degree of algnent achive bythe relied at _Athoug spect values ofalareent have been consid fo SWNT the same vale te btaned for oher NTE such as MWNTS. Slay, questa of ‘rove shapes oreo hang he same degre of alormantsan be achieved bythe mato ofthe nveton The shape of th askno which te carbon nanotube connate vepraed determines fo sme exten he over shape ofthe quis. Thats, asthe “bon nanabe coreeiae evaporates, the carbon nanlubes san wih etch oe arscotet onthe wal th Mk Therefore tan the Maske coves the ‘ton arabe quasierstal (lathe CNT oring he qual icuried inthe are shape asthe ask Therefore 2 mor lines assests dese the ‘evaporation sep ores must ues Mak wh alr nea tface, Sal diferent shapes of quas-eytale.e,Diferent ze of curvature on shapers ested complerettary shaped sk must be used othe eraperan step. Although he qusiysalmy be uve folowing the shape af the Mask. scutes serge that wl be near inne dese rlarey smal range (one) ‘apl Pureatin of SWNT Soot canting SWAT was ytheized by ate dachatge of acaontod cantaning 42 slams of Nand 1.0 atoms of ¥ The titan process or SHATcontining stots snl ta the process auned iF. 1 encept ha SWNT ar the esied CNT ne example. 25 rams ofthis sot was prepared et ming 1:7 sethylomaige(OMF) a pure water ina Mask, ‘Wet wih 10mlof he solvent mature Te soot and slvet mur was gouty sted inte ask Suc a weing proces is porta for enley, se soot may Ignite te nancstat contained th oot wen ia mined with cone tc cin the acre tage Aer wetbng. 250 mit concen ated nite aed (70%) was slowly slacein th ask to remove metals and aorphoesceron in he sample. The ask was then cached toa condenser conection acd absorber Ihe sen soakesin th aida the eed ot 110° € for 10 nore an then at 179°C for aneter Ohare The tine an terperatie ae net eral bt ‘he acd mast sont fom a slsion wh ham nthe soot andthe amorphous carbon Tal, ‘The higher te trperatre te shores the ne while longer ha i, the rth erature Now. he metre wae cole to room trp he exaust ne was removed a then cennfogaton was carrad atin a pls ibe 600 rpm for20 mint, “The tron tlespersttat was ten deca whl he wet pecptae was washed wth pe water and then esupendes a rmove the sed and rorhoe sede tale an high furctonal gauge were usualy ound. ler Wires cyeles af cetigatinecanation-esurpension deszrbedaboveafecetupai supetntant ted completely buck. The syperatant was close / ght own bel tuning Back Ate te supematan tured back was coleted by the process of decantation, resuspension and certftgtion under the ere rameters a above. thin cate he supenatat gud i a deed rata string lak ans IReontaned WNT and water slit eon. Ths proces is fepeated tes to obah a black Slur fa dented soluton whleteremaieg sediment contns ‘ewton parteles above 20 nm msi cabon coated metal te. was there. 1-21terefblack solution was obtaed "-2mbof lek stun e190 _Aterthckeningtheseluten, was alowed 1 sete for several burs. Thelonge the tne to sete this solton the beter forthe presiptatin of SWNT. In don, “several bundles of paegstes were formed cu hi rection process. The solsion then laced inatube for 5000, Iyoung a O rp or20 minutes moze SN ‘The T sediment ctied These SWNT presses were wathed vie with pre wae lo remevelmptes leg SUNT concerts) ‘Was uted wh tet 1 Mer andthe sons fr a short en, then resuspended inate. Then hie esuspenson(e- hiupssipaterts.google.compatentJP2009054821Alen m25112122, 153 PM 44P2003054821A -Purficaton, allgnment, and quasi-rystalization of carbon nanotube - Google Patents SWNT Algrenent and AtoralPrfeaton One Her of SWNT concentrate was eraported gery ove haurs—ing rotary evapora at 100 an 50": ny sha grades evaparaton process, ‘Webatgned SWNT precipitated rm the above sl Figure 24 -Aquaseyetal at sho in-2d wat produce. Th sow evaporation cases the SWNTS oes dt th hh van der Waal forces between the nanotubes. ‘The SWNT quaticystl wa the urbe puied S Putthe WNT quas-ysaio the tasani Soahetexractor Teremove residual imgurtes such 2s high ytogenated carbo, Perfor exracton process with water and oter solvents to remove became Salvrts contaning N groupe The goer fori Ree Ofte stern the or, age Rel HOH, NH bled unexamined patent ppleaton “wo Nite formul,= 1164, ‘tose foment 4), Ney. NHigHroe Myo ACOH ‘oar Selected rm Nie a drogen pu Iwas ene effective in removing nay, ne quasi were hese 0 250°C fr TO ours to emave excess fnstonal groups rom SWNT, ech 8 OH and NO 2. SWN pred othe nd Inthis earl, sot tom ae secharoe wae uso ae he start mater Hower this mtd 2 aoot canbe used staring material a lg ast contains WNT. Tats. the peiicaton and agent method ofthe recent iveton can be easy used on set made by we €athrge, sealant, and sol made wig ay cata he ctaot we dferent the sare diferent cide may beusedin he ae ret tage, Fue: nth embodiment re SANT coneentate soliton Was eded to S vaparte over une, Howeve such times nt grant and ison pelered. Tet. the evaporation fate must be ouficlentto aban en eget of SHINS wth sufetent rsa siz. geet te slower the evaporation rete ager he dlaetr rh an volume ofthe quasionystalhat forms. More specscal, 1 259 of scot cantnned in ero elute, whch s 200 lJ howto 1 Her erin the ease of pros selon tat x encatrates aon nanote schon Fvaparton ales nthe tine rangecan be used Tesora ar mera posto he present nveton tha the carbon ransube concentrates wed andthe raratues cane traces o each ter by storg van dr Waal fre ao tha the carbon ransubes have suena slain Tesoklon to only (0052) EFFECT OF THEINVENTION Advanta of th Inventn The present inverttanpovides a method of pring and aang carbon nanotubes int quasi ‘Se ths method irl chemist bases an eel sald pt hande age quite of ot eansning te see carbon notes Alo sine the ‘matod i sobticercherity based cn be uted with CNFcantanng soa made by anj method ach es we achargeo aration, Furthermore the method ean ‘euseorCNTe made wth vaso diferent class. Tats the usin of his had canbe ued fr CNTs wih various temperate ist, cues and mate congestion. Moteoe sae the method inelves mating ecard nanotube concent ndthen slowly evaporite selition, te method can oben lage quasicnystale of wellaloned cron nanotubes. “Te prevent nv ae avidetchiquee ach a slow process Therefore arelavely high aly carbon nanotube quasiysalcen be obtained ina shorertine than inthe 3 combutton, wich cases uneven cntlon and carbon nanotube damage nd micrefitation whichia a very Joe. \wiut departing tom the span sone ofthe present vention as diene lms balled that numerous modieations canbe made tothe method of uring and string CNTs acorn te present vention [suet description o drawings] FG. 1ie tema fow cart of te ptfeton ae gyn srceat of CNR where the pusication steps ae umbered and sted on he se ofthe cha, ule the bongo the ated bx onthe ght le of le cart have Been feroved, Species ae listed andthe ow of materiale Nghighed othe center fhe chart, ighated by te sa box 2d a snring electon ioscan (SEN) mags photograph of puted SWNT quis, FG aie a Saat te pail SWNT quasicryeain FC. 24 though ti an EM sheogrph tha a greet mae ai xshown the drawing FG. 4ie a raph showing he distribution of bundles within a quaserytal in wbich the mais howe the it angle of the bal frm th in i lige A, ile the yas shows each thee shown onthe ans The number of bundles a epee nglrover a qusiyeal wt of ri hen, [exptnaton of aymbete) 1 As (inl) 2x ane 3 ls 4 HH (fl wc tal min) conta tontsage (2s inentrntzusi amid 685 ssinagenashragawates Tok Soni tsi the corporation (72) nventorSefumi Ata 735 K-Shnapawa Shinagawa, Toyo Soni ie the “orporton Fem referee) 46045 CADD CC1D hiupssipaterts.google.compatentJP2009054821Alen ane