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Filimi za nanoscale grafiti (NGFs) ni ibikoresho bikomeye bishobora gukorwa hakoreshejwe umwuka wa chemical catalytic, ariko haracyari ibibazo ku bijyanye no koroshya kwimura no gukoresha imiterere y'ubuso n'uburyo imiterere y'ubuso igira ingaruka ku ikoreshwa ryabyo mu bikoresho bishya. Aha turatangaza ikura rya NGF ku mpande zombi za polycrystalline nickel foil (ubuso bwa 55 cm2, ubunini bwa 100 nm) no kwimura kwayo nta polymer (imbere n'inyuma, ubuso bugera kuri 6 cm2). Bitewe n'imiterere ya catalyst foil, filimi ebyiri za karuboni zitandukanye mu miterere yazo n'ibindi biranga (nk'ubushyuhe bw'ubuso). Tugaragaza ko NGF zifite inyuma igoye cyane zikwiriye gupimwa NO2, mu gihe NGF zoroshye kandi zitwara neza ku ruhande rw'imbere (2000 S/cm2, ubushobozi bwo kwirinda sheet - 50 ohms/m2) zishobora kuba amashanyarazi afatika, umuyoboro cyangwa electrode y'ingirabuzima fatizo z'izuba (kubera ko zohereza 62% by'urumuri rugaragara). Muri rusange, uburyo bwasobanuwe bwo gukura no gutwara ibintu bushobora gufasha mu gushyira mu bikorwa NGF nk'uburyo bwo gukoresha ikoranabuhanga mu ikoranabuhanga aho graphene na graphite filime z'ubugari bwa micron zitakwiriye.
Graphite ni ibikoresho bikoreshwa cyane mu nganda. By’umwihariko, graphite ifite imiterere yo kuba ifite ubucucike buke kandi ifite ubushobozi bwo gutwara ubushyuhe n’amashanyarazi mu kirere, kandi irahamye cyane mu bidukikije bikomeye by’ubushyuhe n’ibinyabutabire1,2. Graphite ya Flake ni ibikoresho bizwi cyane byo gutangira ubushakashatsi kuri graphine3. Iyo itunganyijwe mu mafirime yoroheje, ishobora gukoreshwa mu buryo butandukanye, harimo n’ibikoresho bishyushya ibikoresho by’ikoranabuhanga nka telefoni zigendanwa4,5,6,7, nk’ibikoresho bikora muri sensor8,9,10 no mu kurinda amashanyarazi kubangamira 11. 12 na firime zo gukoresha lithography mu mirasire ya ultraviolet ikabije13,14, zikora imiyoboro mu turemangingo tw’izuba15,16. Kuri izi porogaramu zose, byaba ari inyungu ikomeye niba ahantu hanini ha firime za graphite (NGFs) zifite ubunini bugenzurwa muri nanoscale <100 nm hashobora gukorwa no gutwarwa byoroshye.
Filimi za grafiti zikorwa hakoreshejwe uburyo butandukanye. Mu rubanza rumwe, gushyiramo no kwagura hanyuma hagakurikiraho gusohora ifu byakoreshejwe kugira ngo hakorwe uduce twa grafiti 10,11,17. Uduce tugomba gukomeza gutunganywamo filime z'ubugari bukenewe, kandi akenshi bifata iminsi myinshi kugira ngo hakorwe impapuro za grafiti zikomeye. Ubundi buryo ni ugutangirana n'uduce tw'ibanze dushobora gushushanywa. Mu nganda, impapuro za polimeri zishyirwamo karuboni (kuri 1000–1500 °C) hanyuma zigashyirwamo graphiti (kuri 2800–3200 °C) kugira ngo hakorwe ibikoresho bifite imiterere myiza. Nubwo ubwiza bw'izi filime ari bwinshi, ingufu zikoreshwa ni 1,18,19 kandi ubugari buke bugarukira kuri mikoroni nke 1,18,19,20.
Uburyo bwo gusohora umwuka w’ubushyuhe bwa shimi (CVD) buzwi cyane mu gukora filime za graphene na ultrathine grafiti (<10 nm) zifite imiterere myiza kandi zihendutse 21,22,23,24,25,26,27. Ariko, ugereranije n’ubwiyongere bwa filime za graphene na ultrathine grafiti28, gukura no/cyangwa ikoreshwa rya NGF mu buso bunini hakoreshejwe CVD ntibikunze kwitabwaho cyane11,13,29,30,31,32,33.
Filimi za graphene na graphite zatewe muri CVD akenshi zigomba kwimurirwa ku bikoresho bikora34. Uku kwimurirwa kwa firime ntoya kugizwe n'uburyo bubiri bw'ingenzi35: (1) kwimurirwa ku buryo budakoresha icyuma gishyushye36,37 na (2) kwimurirwa kwa shimi hakoreshejwe icyuma gishyushye (substrate ishyigikiwe)14,34,38. Buri buryo bufite ibyiza n'ibibi bimwe na bimwe kandi bugomba gutoranywa bitewe n'ikoreshwa ryabwo, nk'uko byasobanuwe ahandi35,39. Ku firimi za graphene/graphite zakuwe ku bikoresho bishyushye, kwimurirwa hakoreshejwe uburyo bwa shimi bushyushye (muri bwo polymethyl methacrylate (PMMA) niyo nkunga ikoreshwa cyane) ni yo ikomeza kuba amahitamo ya mbere13,30,34,38,40,41,42. Wewe n'abandi. Byavuzwe ko nta polimeri yakoreshejwe mu kwimurirwa kwa NGF (ingano y'icyitegererezo ingana na cm2 4)25,43, ariko nta bisobanuro byatanzwe ku bijyanye no kugumana icyitegererezo cyangwa uburyo gikoreshwa mu kwimurirwa; Uburyo bwo gukoresha polymers bukoresha polymers bugizwe n'intambwe nyinshi, harimo no gukoresha no gukuraho urwego rwa polymers rusanzwe30,38,40,41,42. Ubu buryo bufite ingaruka mbi: urugero, ibisigazwa bya polymer bishobora guhindura imiterere ya firime yakuze38. Gutunganya by'inyongera bishobora gukuraho polime zisigaye, ariko izi ntambwe z'inyongera zongera ikiguzi n'igihe cyo gukora firime38,40. Mu gihe cyo gukura kwa CVD, urwego rwa graphene rushyirwa ku ruhande rw'imbere rwa firime ya catalyst (uruhande rureba umuvuduko w'umwuka), ndetse no ku ruhande rw'inyuma rwayo. Ariko, iyi ya nyuma ifatwa nk'imyanda kandi ishobora gukurwaho vuba na plasma yoroshye38,41. Kongera gukoresha iyi firime bishobora gufasha kongera umusaruro, nubwo yaba ifite ubuziranenge buke ugereranyije na firime ya karuboni.
Aha, turatangaza uburyo INGF yakuze mu buryo bwa wafer ifite imiterere myiza ku rupapuro rwa nikeli rwa polycrystalline na CVD. Hasuzumwe uburyo ubuso bw'imbere n'inyuma bw'urupapuro bugira ingaruka ku miterere n'imiterere ya NGF. Tugaragaza kandi ko NGF ihendutse kandi idahumanya ibidukikije iva ku mpande zombi z'urupapuro rwa nikeli ijya ku duce duto tw'imikorere myinshi, kandi tukerekana uburyo filime z'imbere n'inyuma zikwiriye gukoreshwa mu buryo butandukanye.
Ibice bikurikira biganira ku bunini butandukanye bwa filime ya grafiti bitewe n'umubare w'ibice bya graphene byashyizwemo: (i) graphene y'urwego rumwe (SLG, urwego 1), (ii) graphene y'urwego ruto (FLG, < urwego 10), (iii) graphene y'urwego rwinshi (MLG, urwego 10-30) na (iv) NGF (~ urwego 300). Ubunini bwa nyuma ni bwo bukunze kugaragara nk'ijanisha ry'ubuso (hafi 97% by'ubuso kuri 100 µm2)30. Niyo mpamvu filime yose yitwa gusa NGF.
Udupapuro twa nikeli twa polycrystalline dukoreshwa mu gukora filime za graphene na grafiti dufite imiterere itandukanye bitewe n'uko twakozwe ndetse no gutunganya nyuma. Duherutse gutangaza inyigo yo kunoza inzira yo gukura ya NGF30. Tugaragaza ko ibipimo by'imikorere nk'igihe cyo guteranya n'umuvuduko w'icyumba mu gihe cyo gukura bigira uruhare runini mu kubona NGF z'ubugari bungana. Aha, twakomeje gusuzuma ikura rya NGF ku buso bwa polished (FS) n'ubuso bw'inyuma butaraseswa (BS) bwa nikeli (Ishusho ya 1a). Ubwoko butatu bw'ibipimo bya FS na BS bwasuzumwe, byavuzwe mu mbonerahamwe ya 1. Iyo urebye neza, ikura rya NGF ku mpande zombi za nikeli (NiAG) rishobora kugaragara bitewe n'ihinduka ry'ibara rya substrate ya Ni nyinshi kuva ku ibara ry'umweru rya feza ridasanzwe kugeza ku ibara ry'umukara ritameze neza (Ishusho ya 1a); ibipimo bya mikorosikopi byemejwe (Ishusho ya 1b, c). Ishusho isanzwe ya Raman ya FS-NGF yagaragaye mu gace keza kandi igaragazwa n'utwambi dutukura, ubururu n'umuhondo muri Ishusho ya 1b igaragazwa muri Ishusho ya 1c. Imisongero ya Raman ya grafiti G (1683 cm−1) na 2D (2696 cm−1) yemeza ikura rya NGF ifite ubushyuhe bwinshi (Ishusho ya 1c, Imbonerahamwe ya SI1). Muri filime yose, hagaragaye ubwinshi bwa spectra ya Raman ifite igipimo cy'ubukana (I2D/IG) ~0.3, mu gihe spectra ya Raman ifite I2D/IG = 0.8 idakunze kugaragara. Kuba nta misongero ifite inenge (D = 1350 cm-1) muri filime yose bigaragaza ireme ryinshi ry'ikura rya NGF. Ibisubizo nk'ibya Raman byabonetse ku gipimo cya BS-NGF (Ishusho ya SI1 a na b, Imbonerahamwe ya SI1).
Kugereranya NiAG FS- na BS-NGF: (a) Ifoto y'icyitegererezo gisanzwe cya NGF (NiAG) kigaragaza gukura kwa NGF ku gipimo cya wafer (55 cm2) n'ingero za foil za BS- na FS-Ni, (b) Amashusho ya FS-NGF / Ni yabonetse hakoreshejwe mikorosikopi y'urumuri, (c) spectra isanzwe ya Raman yafashwe ahantu hatandukanye muri panel b, (d, f) Amashusho ya SEM ku bwinshi butandukanye kuri FS-NGF / Ni, (e, g) Amashusho ya SEM ku bwiza butandukanye Amashami ya BS -NGF / Ni. Akambi k'ubururu kerekana agace ka FLG, akambi k'umuhondo kerekana agace ka MLG (hafi y'agace ka FLG), akambi k'umutuku kerekana agace ka NGF, naho akambi k'umutuku kerekana aho kagonga.
Kubera ko gukura biterwa n'ubugari bw'igice cya mbere cy'ubutaka, ingano ya kristu, icyerekezo, n'imbibi z'ingano, kugera ku kugenzura neza ubugari bwa NGF ku bice binini biracyari imbogamizi20,34,44. Ubu bushakashatsi bwakoresheje ibikubiye twasohoye mbere30. Ubu buryo butanga akarere keza kari hagati ya 0.1 na 3% kuri 100 µm230. Mu bice bikurikira, turagaragaza ibisubizo by'ubwoko bwombi bw'uturere. Amashusho ya SEM yo gukuza cyane agaragaza ko hari ahantu henshi hatandukanye ku mpande zombi (Ishusho ya 1f, g), bigaragaza ko hari uturere twa FLG na MLG30,45. Ibi kandi byemejwe no gukwirakwiza Raman (Ishusho ya 1c) n'ibyavuye muri TEM (byaganiriweho nyuma mu gice cyitwa "FS-NGF: imiterere n'imiterere"). Uduce twa FLG na MLG twagaragaye ku bipimo bya FS- na BS-NGF / Ni (imbere n'inyuma bya NGF byahinzwe kuri Ni) bishobora kuba byarakuriye ku binyampeke binini bya Ni (111) byakozwe mu gihe cyo gufunga 22,30,45. Ku mpande zombi hagaragaye gupfunyika (Ishusho ya 1b, yashyizweho ikimenyetso cy'imyambi y'umuhengeri). Iyi mipfunyika ikunze kuboneka muri graphene na graphite byatewe na CVD bitewe n'itandukaniro rinini mu gipimo cy'ubushyuhe hagati ya graphite na nickel substrate30,38.
Ishusho ya AFM yemeje ko icyitegererezo cya FS-NGF cyari gito ugereranyije n'icyitegererezo cya BS-NGF (Ishusho ya SI1) (Ishusho ya SI2). Agaciro k'ubukana bw'imizi (RMS) bwa FS-NGF/Ni (Ishusho ya SI2c) na BS-NGF/Ni (Ishusho ya SI2d) ni 82 na 200 nm, uko bikurikirana (bipimwe ku buso bwa 20 × 20 μm2). Ubukana bwinshi bushobora kumvikana hashingiwe ku isesengura ry'ubuso bwa foil ya nickel (NiAR) mu gihe yakiriwe (Ishusho ya SI3). Amashusho ya SEM ya FS na BS-NiAR agaragara mu Mashusho ya SI3a–d, agaragaza imiterere itandukanye y'ubuso: foil ya FS-Ni ikoze neza ifite uduce duto twa nano- na micron, mu gihe foil ya BS-Ni idafite ikoze neza igaragaza urwego rwo gukora nk'uduce dufite imbaraga nyinshi. n'igabanuka. Amashusho yo hasi kandi yo hejuru ya foil ya nickel ikozwe (NiA) agaragara mu Mashusho ya SI3e–h. Muri izi shusho, dushobora kubona ko hari uduce twinshi twa nikeli dufite ingano ya mikoroni ku mpande zombi z'urupapuro rwa nikeli (Ishusho ya SI3e–h). Uduce duto dushobora kugira icyerekezo cya Ni (111), nk'uko byatangajwe mbere30,46. Hari itandukaniro rinini mu miterere ya nikeli hagati ya FS-NiA na BS-NiA. Ubukana bwinshi bwa BS-NGF/Ni buterwa n'ubuso butarasukurwa bwa BS-NiAR, ubuso bwabwo bugakomeza kuba bubi cyane ndetse na nyuma yo gukururwa (Ishusho ya SI3). Ubu bwoko bw'imiterere y'ubuso mbere y'uko inzira yo gukura butuma ubukana bwa graphene na graphite films bugenzurwa. Tugomba kumenya ko substrate ya mbere yavuguruwe mu gihe cyo gukura kwa graphene, byagabanyije gato ingano y'utubuto kandi byongera ubukana bw'ubuso bwa substrate ugereranije na annealed foil na catalyst film22.
Gutunganya neza ubukana bw'ubuso bw'ibumba, igihe cyo gutera (ingano y'ibinyampeke) 30,47 no kugenzura kurekura 43 bizafasha kugabanya ubukana bw'ubunini bwa NGF mu gace kayo kugeza kuri µm2 cyangwa nm2 (ni ukuvuga ihindagurika ry'ubunini bwa nanometero nke). Kugira ngo hagenzurwe ubukana bw'ubuso bw'ibumba, uburyo nko gusiga electrolytic foil ya nickel bushobora gusuzumwa48. Ibumba rya nickel ryavuwe mbere rishobora gufatirwa ku bushyuhe buri hasi (<900 °C) 46 n'igihe (
Uburyo bwo kohereza imiti itose idafite polymer kuri NGF ihingwa kuri nikeli: (a) Imbonerahamwe y'imigendekere y'ibikorwa (reba Ishusho ya SI4 kugira ngo umenye byinshi), (b) Ifoto ya digitale ya NGF yatandukanye nyuma yo gushushanya Ni (ibipimo 2), (c) Urugero rwo kohereza FS - na BS-NGF kuri SiO2 / Si substrate, (d) kohereza FS-NGF kuri substrate ya polymer idasobanutse, (e) BS-NGF ivuye ku gipimo kimwe n'agace ka d (gagabanyijemo ibice bibiri), yoherezwa ku rupapuro rwa C rutwikiriwe na zahabu na Nafion (substrate ibonerana ihinduka, impande zifite inkingi zitukura).
Menya ko kohereza SLG hakoreshejwe uburyo bwo kohereza imiti itose bisaba igihe cyo gutunganya cyose kingana n'amasaha 20-24. Hamwe n'uburyo bwo kohereza budafite polymer bwagaragajwe hano (Ishusho ya SI4a), igihe cyose cyo kohereza NGF muri rusange kiragabanuka cyane (hafi amasaha 15). Ubu buryo bugizwe na: (Intambwe ya 1) Tegura umuti wo gukata hanyuma ushyiremo icyitegererezo (~iminota 10), hanyuma utegereze ijoro ryose kugira ngo ukate Ni (~iminota 7200), (Intambwe ya 2) Oza n'amazi yakuwemo iion (Intambwe ya 3). Bika mu mazi yakuwemo iion cyangwa wimure kuri substrate (iminota 20). Amazi yafatiwe hagati ya NGF na matrix y'ingano akurwaho hakoreshejwe uburyo bwo kohereza imiyoboro y'amazi (ukoresheje impapuro zipfuka)38, hanyuma ibitonyanga by'amazi bisigaye bikurwaho no kuma karemano (hafi iminota 30), hanyuma icyitegererezo cyumye mu gihe cy'iminota 10 mu ifuru idafite umwuka (10-1 mbar) kuri 50-90 °C (iminota 60)38.
Graphite izwiho kwihanganira amazi n'umwuka ku bushyuhe buri hejuru cyane (≥ 200 °C) 50,51,52. Twapimye ingero dukoresheje Raman spectroscopy, SEM, na XRD nyuma yo kubika mu mazi yakuwemo iayoni ku bushyuhe bw'icyumba no mu macupa afunze mu gihe cy'iminsi mike kugeza ku mwaka umwe (Ishusho ya SI4). Nta kwangirika kugaragara kwabyo. Ishusho ya 2c igaragaza FS-NGF na BS-NGF bihagaze mu mazi yakuwemo iayoni. Twabifashe kuri substrate ya SiO2 (300 nm) / Si, nk'uko bigaragara mu ntangiriro y'Ishusho ya 2c. Byongeye kandi, nk'uko bigaragara ku Ishusho ya 2d, e, NGF ikomeza ishobora kwimurirwa mu bice bitandukanye nka polymers (Thermabright polyamide yo muri Nexolve na Nafion) n'impapuro za karuboni zitwikiriwe na zahabu. FS-NGF yoroshye kuyishyira ku gice cy'ingenzi (Ishusho ya 2c, d). Ariko, ingero za BS-NGF zirengeje 3 cm2 zari zikomeye kuzifata iyo zijugunywe mu mazi yose. Ubusanzwe, iyo bitangiye kwibira mu mazi, bitewe no kuyafata nabi rimwe na rimwe acikamo ibice bibiri cyangwa bitatu (Ishusho ya 2e). Muri rusange, twashoboye kugera ku ihererekanya ridafite polymer rya PS- na BS-NGF (ihererekanya rihoraho ridafite NGF/Ni/NGF kuri cm2 6) ku bipimo bigera kuri cm2 6 na 3 mu buso, uko bikurikirana. Ibice binini cyangwa bito bisigaye bishobora (kugaragara byoroshye mu gisubizo cyo gushushanya cyangwa amazi yakuwemo ioni) ku butaka bwifuzwa (~1 mm2, Ishusho ya SI4b, reba icyitegererezo cyimurirwa mu muyoboro w'umuringa nkuko biri muri "FS-NGF: Imiterere n'Imiterere (byaganiriweho) munsi ya "Imiterere n'Imiterere") cyangwa bikabikwa kugira ngo bikoreshwe mu gihe kizaza (Ishusho ya SI4). Dushingiye kuri iki gipimo, twemeza ko NGF ishobora kugaruzwa mu musaruro wa 98-99% (nyuma yo gukura kugira ngo ihererekanywe).
Ingero zo kwimura zidafite polymer zasesenguwe mu buryo burambuye. Imiterere y'imiterere y'ubuso yabonetse kuri FS- na BS-NGF/SiO2/Si (Ishusho ya 2c) hakoreshejwe mikorosikopi y'urumuri (OM) n'amashusho ya SEM (Ishusho ya SI5 n'Ishusho ya 3) byagaragaje ko izi ngero zoherejwe zidafite mikorosikopi. Kwangirika kw'imiterere kugaragara nko kwangirika, imyobo, cyangwa ahantu hafunguye. Imirongo iri kuri NGF ikura (Ishusho ya 3b, d, yashyizweho ikimenyetso cy'imyambi y'umuhengeri) yagumye uko iri nyuma yo kwimurwa. FS- na BS-NGF zombi zigizwe n'uturere twa FLG (uturere tw'ubururu tugaragazwa n'imyambi y'ubururu mu Ishusho ya 3). Igitangaje ni uko bitandukanye n'uturere duke twangiritse dukunze kugaragara mu gihe cyo kwimura polymer ya filime za grafiti nto cyane, uturere twinshi twa FLG na MLG duhuza na NGF (twashyizweho ikimenyetso cy'imyambi y'ubururu mu Ishusho ya 3d) twoherejwe nta kwangirika cyangwa gucika (Ishusho ya 3d). 3). Ubuziranenge bwa mekanike bwemejwe cyane hakoreshejwe amashusho ya TEM na SEM ya NGF yimuwe ku miyoboro y'umuringa ya lace-carbon, nk'uko byavuzwe nyuma (“FS-NGF: Imiterere n'Imiterere”). BS-NGF/SiO2/Si yimuwe irakomeye kurusha FS-NGF/SiO2/Si ifite agaciro ka rms ka 140 nm na 17 nm, uko bikurikirana, nk'uko bigaragara ku Ishusho ya SI6a na b (20 × 20 μm2). Agaciro ka RMS ka NGF yimuwe ku gice cya SiO2/Si (RMS < 2 nm) kari hasi cyane (hafi inshuro 3) ugereranyije n'aka NGF yakuriye kuri Ni (Ishusho ya SI2), bigaragaza ko ubukana bw'inyongera bushobora kuba buhuye n'ubuso bwa Ni. Byongeye kandi, amashusho ya AFM yakozwe ku nkengero za FS- na BS-NGF/SiO2/Si yagaragaje ubunini bwa NGF bwa 100 na 80 nm, uko bikurikirana (Ishusho ya SI7). Ubunini buto bwa BS-NGF bushobora guterwa n'uko ubuso butahuye neza na gaze y'inyongera.
NGF (NiAG) yimuwe idafite polymer kuri SiO2/Si wafer (reba Ishusho ya 2c): (a,b) Amashusho ya SEM ya FS-NGF yimuwe: ubwinshi bwo hasi n'ubunini (bujyanye na kare y'icunga mu gice). Uduce dusanzwe) – a). (c,d) Amashusho ya SEM ya BS-NGF yimuwe: ubwinshi bwo hasi n'ubunini (bujyanye n'agace gasanzwe kagaragazwa na kare y'icunga mu gice c). (e, f) Amashusho ya AFM ya FS- na BS-NGF yimuwe. Umwambi w'ubururu ugaragaza agace ka FLG – itandukaniro ry'ubururu, umwambi wa cyan – itandukaniro ry'umukara rya MLG, umwambi utukura – itandukaniro ry'umukara rigaragaza agace ka NGF, umwambi wa magenta ugaragaza ipfundo.
Imiterere y'imiti ya FS- na BS-NGFs zakuze n'izimutse yasesenguwe hakoreshejwe X-ray photoelectron spectroscopy (XPS) (Ishusho ya 4). Isonga rito ryagaragaye muri spectra yapimwe (Ishusho ya 4a, b), ihuye na substrate ya Ni (850 eV) ya FS- na BS-NGFs zakuze (NiAG). Nta songa riri muri spectra yapimwe ya FS- na BS-NGF/SiO2/Si (Ishusho ya 4c; ibisubizo bisa kuri BS-NGF/SiO2/Si ntabwo byagaragajwe), bigaragaza ko nta cyandu cya Ni gisigaye nyuma yo kwimurwa. Ishusho ya 4d-f yerekana spectra ifite ubushobozi bwo hejuru bw'ingufu za C 1 s, O 1 s na Si 2p za FS-NGF/SiO2/Si. Ingufu zo gufatanya za C 1 s za grafiti ni 284.4 eV53.54. Imiterere y'imitwe ya grafiti muri rusange ifatwa nk'aho idahuje, nk'uko bigaragara ku Ishusho ya 4d54. Ishusho ya C1 s yo ku rwego rwo hejuru (Ishusho ya 4d) nayo yemeje ko habaho ihererekanya ry'amazi (ni ukuvuga ko nta bisigazwa bya polymer), ibyo bikaba bihuye n'ubushakashatsi bwabanje38. Ubugari bw'imirongo ya spectra ya C1 s y'icyitegererezo gishya (NiAG) na nyuma yo kwimura ni 0.55 na 0.62 eV, uko bikurikirana. Izi gaciro ziri hejuru y'iza SLG (0.49 eV kuri SLG kuri substrate ya SiO2)38. Ariko, izi gaciro ni ntoya ugereranije n'ubugari bw'imirongo bwavuzwe mbere ku bipimo bya graphene bya pyrolytic (~0.75 eV)53,54,55, bigaragaza ko nta hantu hafite inenge ha karuboni mu bikoresho bigezweho. Ishusho ya C1 s na O 1 s yo ku rwego rwo hasi nayo ibura amababa, bigatuma habura ishingiro ryo gukuraho peak deconvolution54. Hari uburebure bwa satelite ya π → π* hafi ya 291.1 eV, bukunze kugaragara mu bipimo bya grafiti. Ibimenyetso bya 103 eV na 532.5 eV muri spectra ya Si 2p na O 1 s (reba Ishusho ya 4e, f) bikomoka kuri substrate ya SiO2 56, uko bikurikirana. XPS ni tekiniki yoroshye kureba ubuso, bityo ibimenyetso bihuye na Ni na SiO2 byabonetse mbere na nyuma yo kohereza NGF, uko bikurikirana, bifatwa nk'aho bikomoka mu gace ka FLG. Ibisubizo nk'ibyo byagaragaye ku bipimo bya BS-NGF byimuwe (ntibyerekanye).
Ibisubizo bya NiAG XPS: (ac) Gusuzuma imiterere itandukanye ya atome ya FS-NGF/Ni, BS-NGF/Ni no kohereza FS-NGF/SiO2/Si, uko bikurikirana. (d–f) Spectra ifite ubushobozi bwo hejuru bw'urwego rw'ibanze C 1 s, O 1s na Si 2p by'icyitegererezo cya FS-NGF/SiO2/Si.
Ubwiza rusange bwa kristu za NGF zahinduwe bwapimwe hakoreshejwe X-ray diffraction (XRD). Imiterere isanzwe ya XRD (Ishusho ya SI8) ya FS- na BS-NGF/SiO2/Si zahinduwe igaragaza ko hari imisozi miremire ya diffraction (0 0 0 2) na (0 0 0 4) kuri 26.6° na 54.7°, bisa na grafiti. . Ibi byemeza ubwiza bwa NGF buri hejuru kandi bihuye n'intera iri hagati ya d = 0.335 nm, ikomeza gukurikizwa nyuma y'intambwe yo kwimura. Ubukana bw'umurambararo wa diffraction (0 0 0 2) bungana n'inshuro 30 z'umurambararo wa diffraction (0 0 0 4), bigaragaza ko ikirere cya kristu cya NGF gihuye neza n'ubuso bw'icyitegererezo.
Dukurikije ibyavuye muri SEM, Raman spectroscopy, XPS na XRD, ireme rya BS-NGF/Ni ryagaragaye ko ari rimwe n’irya FS-NGF/Ni, nubwo ubukana bwa rms bwaryo bwari hejuru gato (Ishusho ya SI2, SI5) na SI7).
SLG zifite urwego rushyigikira polymer rugera kuri 200 nm z'ubugari zishobora kureremba hejuru y'amazi. Iyi gahunda ikunze gukoreshwa mu buryo bwo kohereza imiti itose ifashijwe na polymer22,38. Graphene na grafiti ni hydrophobic (inguni 80–90°) 57. Byatangajwe ko ubuso bw'ingufu bushoboka bwa graphene na FLG ari ndende cyane, bufite ingufu nke (~1 kJ/mol) ku ngendo z'amazi ku mpande58. Ariko, ingufu zibazwe z'amazi na graphene n'urwego rutatu rwa graphene ziri hafi − 13 na − 15 kJ/mol,58, bigaragaza ko imikoranire y'amazi na NGF (urugero hafi 300) iri hasi ugereranije na graphene. Iyi ishobora kuba imwe mu mpamvu zituma NGF ihagaze ku rundi ruhande iguma ku rundi ruhande ku rundi ruhande rw'amazi, mu gihe graphene ihagaze ku rundi ruhande (igenda mu mazi) iragenda yizunguruka ikameneka. Iyo NGF yinjijwe mu mazi yose (ibisubizo ni bimwe kuri NGF igoye kandi igororotse), impande zayo ziragonda (Ishusho ya SI4). Mu gihe cyo kwibira mu mazi yose, byitezwe ko ingufu za NGF n'amazi zikubye hafi kabiri (ugereranije na NGF ireremba) kandi ko impande za NGF zizunguruka kugira ngo zigumane inguni yo hejuru yo gukoraho (hydrophobicity). Twizera ko ingamba zishobora guterwa kugira ngo hirindwe ko impande za NGF zinjiramo zizunguruka. Uburyo bumwe ni ugukoresha imiti ivanze kugira ngo ihindure uburyo graphite film itose59 ikora.
Kwimura SLG mu bwoko butandukanye bw'ibice by'ingufu binyuze mu nzira zo kohereza imiti ivanze n'amazi byavuzwe mbere. Muri rusange byemewe ko imbaraga nke za van der Waals ziri hagati ya graphene/grafiti na substrates (yaba substrates zikomeye nka SiO2/Si38,41,46,60, SiC38, Au42, Si pillars22 na lacy carbon films30, 34 cyangwa substrates zoroshye nka polyimide 37). Aha dutekereza ko imikoranire y'ubwoko bumwe ari yo yiganje. Nta kwangirika cyangwa gushwanyagurika kwa NGF kuri substrates zimwe na zimwe zagaragajwe hano mu gihe cyo gukoresha ikoranabuhanga (mu gihe cyo kugena ibintu biri mu kirere cyangwa mu gihe cyo kubika) (urugero, Ishusho ya 2, SI7 na SI9). Byongeye kandi, ntabwo twabonye peak ya SiC muri XPS C 1 s spectrum y'urwego rw'ibanze rw'icyitegererezo cya NGF/SiO2/Si (Ishusho ya 4). Ibi bisubizo bigaragaza ko nta mibanire ya shimi iri hagati ya NGF na substrate igamije.
Mu gice cyabanje, “Kwimura FS- na BS-NGF nta polimeri bitanga,” twerekanye ko NGF ishobora gukura no kwimura impande zombi za nickel foil. Izi FS-NGF na BS-NGF ntabwo zimeze kimwe mu bijyanye n’ubuso bugoye, byatumye dushakisha uburyo bukwiye bwo gukoresha buri bwoko.
Dukurikije uburyo FS-NGF igaragara neza kandi isunika neza, twize imiterere yayo, imiterere y’amatara n’amashanyarazi mu buryo burambuye. Imiterere n’imiterere ya FS-NGF idafite polymer transfer byagaragajwe no gupima electron mikroskopi (TEM) no gusesengura imiterere ya electron diffraction (SAED) yatoranijwe. Ibisubizo bihuye bigaragara ku Ishusho ya 5. Gupima TEM mu buryo buke byagaragaje ko hari uturere twa NGF na FLG dufite imiterere itandukanye ya electron contrast, ni ukuvuga uduce twijimye kandi tugaragara cyane (Ishusho ya 5a). Muri rusange, iyi filime igaragaza ubuziranenge bwiza bwa mekanike n’ubudahangarwa hagati y’uduce dutandukanye twa NGF na FLG, hamwe n’aho duhurira neza kandi nta kwangirika cyangwa gucika, ibyo kandi byemejwe na SEM (Ishusho ya 3) n’ubushakashatsi bwa TEM bwo hejuru (Ishusho ya 5c-e). By’umwihariko, ku Ishusho ya 5d yerekana imiterere y’ikiraro ku gice cyayo kinini (ahantu hagaragazwa n’akambi k’umukara kadomo ku Ishusho ya 5d), karangwa n’ishusho y’impandeshatu kandi kagizwe n’urwego rwa graphene rufite ubugari bwa 51. Imiterere ifite intera iri hagati ya 0.33 ± 0.01 nm irushaho kugabanuka ikagera ku byiciro byinshi bya graphene mu gace gato cyane (iherezo ry'umwambi w'umukara ukomeye mu Ishusho ya 5 d).
Ishusho ya TEM y'icyitegererezo cya NiAG idafite polymer ku muyoboro w'umuringa wa lacy wa karuboni: (a, b) Amashusho ya TEM yo gukura make harimo n'uturere twa NGF na FLG, (ce) Amashusho yo gukura cyane y'uturere dutandukanye muri panel-a na panel-b ni imyambi ifite ibara rimwe. Imyambi y'icyatsi kibisi muri panel a na c yerekana ahantu hazengurutse hangiritse mu gihe cyo guhuza imirasire. (f–i) Muri panel a kugeza kuri c, imiterere ya SAED mu turere dutandukanye igaragazwa n'uruziga rw'ubururu, cyan, orange, n'umutuku, uko bikurikirana.
Imiterere y'urushundura mu Ishusho ya 5c igaragaza (ifite akambi gatukura) icyerekezo gihagaze cy'imirongo ya grafiti, bishobora guterwa no kurema imigozi ku gice cya filime (ifite akambi gatukura mu Ishusho ya 5c) bitewe n'umuvuduko mwinshi w'ubushyuhe 30,61,62. Mu gihe TEM ifite ubushobozi bwo hejuru, izi nanofolds 30 zigaragaza icyerekezo gitandukanye cya kristalografiya n'igice cya NGF; imiterere y'ibanze ya grafiti ireba hafi mu buryo buhagaze, aho kuba mu buryo butambitse nk'igice cya filime (ifite akambi gatukura mu Ishusho ya 5c). Mu buryo nk'ubwo, akarere ka FLG rimwe na rimwe kagaragaza imigozi igororotse n'imitobe (ifite akambi k'ubururu), bigaragara ku gipimo cyo hasi n'igiciriritse mu Ishusho ya 5b, 5e, uko bikurikirana. Imigozi igaragara mu Ishusho ya 5e yemeza ko hari imiterere ibiri na itatu ya grafiti mu gice cya FLG (intera ya interplanar 0.33 ± 0.01 nm), ihuye neza n'ibyavuye mu bushakashatsi bwacu bwa mbere30. Byongeye kandi, amashusho ya SEM yafashwe ya NGF idafite polymer yimuwe ku miyoboro y'umuringa hamwe na firime za lacy carbon (nyuma yo gupima TEM yo hejuru) agaragara ku Ishusho ya SI9. Agace ka FLG gahagaze neza (karangwa n'umwambi w'ubururu) n'agace kamenetse ku Ishusho ya SI9f. Umwambi w'ubururu (ku nkengero za NGF yimuwe) werekanwe nkana kugira ngo werekane ko agace ka FLG gashobora kurwanya inzira yo kwimura nta polymer. Muri make, aya mashusho yemeza ko NGF ihagaze igice (harimo n'agace ka FLG) igumana ubuziranenge bwa mekanike ndetse no nyuma yo gufata no gushyira mu mwanya w'umwuka mwinshi mu gihe cyo gupima TEM na SEM (Ishusho ya SI9).
Bitewe n'ubugari bwiza bwa NGF (reba Ishusho ya 5a), ntabwo bigoye kwerekeza uduce duto ku murongo wa [0001] kugira ngo usesengure imiterere ya SAED. Bitewe n'ubugari bw'aho filime iherereye n'aho iherereye, uturere twinshi dushimishije (ingingo 12) twagaragaye kugira ngo hakorwe inyigo ku gukwirakwiza electron. Mu Ishusho ya 5a–c, utu duce tune dusanzwe tugaragara kandi twashyizweho ikimenyetso cy'uruziga rw'amabara (ubururu, cyan, orange, n'umutuku byanditseho code). Ishusho ya 2 na 3 ku buryo bwa SAED. Ishusho ya 5f na g byakuwe mu gace ka FLG kagaragajwe mu Ishusho ya 5 na 5. Nkuko bigaragara mu Ishusho ya 5b na c, uko bikurikirana. Bifite imiterere ya hexagonal isa na graphene igoretse63. By'umwihariko, Ishusho ya 5f igaragaza imiterere itatu ifite icyerekezo kimwe cy'umurongo wa [0001] zone, izungurutswa na 10° na 20°, nk'uko bigaragazwa no kudahuza kw'impande z'amabara atatu ya reflections (10-10). Mu buryo nk'ubwo, Ishusho ya 5g igaragaza imiterere ibiri ya hexagonal ifite impande esheshatu izungurukaho dogere 20. Amatsinda abiri cyangwa atatu y'imiterere ya hexagonal mu gace ka FLG ashobora guturuka ku byiciro bitatu bya graphene biri mu ndege cyangwa hanze ya plane 33 bizunguruka ugereranije. Mu buryo bunyuranye, imiterere ya electron diffraction iri ku Ishusho ya 5h, i (ihuye n'akarere ka NGF kagaragajwe ku Ishusho ya 5a) igaragaza imiterere imwe [0001] ifite ubukana bwa diffraction buri hejuru muri rusange, ijyanye n'ubunini bw'ibikoresho. Izi moderi za SAED zihuye n'imiterere ya grafiti ikomeye n'icyerekezo cyo hagati kurusha FLG, nk'uko byagaragajwe ku gipimo cya 64. Imiterere y'imiterere ya crystalline ya NGF yagaragaje kubaho kwa crystallites ebyiri cyangwa eshatu za superimposed grafiti (cyangwa graphene). Ikintu cy'ingenzi cyane mu karere ka FLG ni uko crystallites zifite urwego runaka rwo kunyuranya hagati cyangwa hanze ya plane. Uduce twa grafiti/ibice bifite inguni zo kuzenguruka mu kirere za 17°, 22° na 25° byavuzwe mbere kuri NGF yahinzwe kuri filime za Ni 64. Agaciro k'inguni yo kuzenguruka kagaragaye muri ubu bushakashatsi gahuye n'inguni zo kuzenguruka zabonetse mbere (±1°) kuri graphene ya BLG63 igoramye.
Imiterere y'amashanyarazi ya NGF/SiO2/Si yapimwe kuri 300 K ku buso bwa 10×3 mm2. Agaciro k'ubwinshi bw'amashanyarazi atwara electron, kugenda no gutwara electron ni 1.6 × 1020 cm-3, 220 cm2 V-1 C-1 na 2000 S-cm-1, uko bikurikirana. Agaciro k'ubwinshi bw'amashanyarazi atwara electron na conductivity ya NGF yacu kameze nk'aka grafiti karemano2 kandi kari hejuru y'aka grafiti ya pyrolytic iboneka ku isoko (ikorwa kuri 3000 °C)29. Agaciro k'ubwinshi bw'amashanyarazi atwara electron kagaragaye kari hejuru y'akavuzwe vuba aha (7.25 × 10 cm-3) ku mashusho ya grafiti afite ubunini bwa micron yateguwe hakoreshejwe impapuro za polyimide zifite ubushyuhe bwinshi (3200 °C) 20.
Twanakoze ibipimo by’urumuri rwa UV rugaragara kuri FS-NGF yimuwe muri quartz substrates (Ishusho ya 6). Ishusho yavuyemo igaragaza ko urumuri rwa 62% rudahinduka ruri hagati ya 350–800 nm, bigaragaza ko NGF ibonerana ku mucyo ugaragara. Mu by’ukuri, izina "KAUST" riboneka mu ifoto y’ikoranabuhanga y’icyitegererezo kiri ku Ishusho ya 6b. Nubwo imiterere ya nanocrystalline ya NGF itandukanye n’iya SLG, umubare w’ibice ushobora kugereranywa hakoreshejwe itegeko rya 2.3% by’igihombo cyo kwanduza kuri buri gice cy’inyongera65. Dukurikije iyi sano, umubare w’ibice bya graphene bifite igihombo cyo kwanduza 38% ni 21. NGF yakuze igizwe ahanini n’ibice 300 bya graphene, ni ukuvuga ubugari bwa nm 100 (Ishusho ya 1, SI5 na SI7). Kubwibyo, dutekereza ko urumuri rw’amatara rwagaragaye ruhuye n’uturere twa FLG na MLG, kuko bikwirakwizwa muri filime yose (Ishusho ya 1, 3, 5 na 6c). Uretse amakuru yavuzwe haruguru, ubushobozi bwo gutwara ibintu no gukorera mu mucyo nabyo byemeza ubwiza bwo hejuru bwa NGF yimuwe.
(a) Igipimo cy’ihererekanya ry’imirasire igaragara nka UV, (b) ihererekanya risanzwe rya NGF kuri quartz hakoreshejwe icyitegererezo cy’icyitegererezo. (c) Igishushanyo cya NGF (agasanduku k’umukara) hamwe n’uturere twa FLG na MLG dukwirakwijwe ku buryo bungana twashyizweho ikimenyetso cy’umukara mu rugero rwose (reba Ishusho ya 1) (hafi 0.1–3% by’ubuso kuri 100 μm2). Imiterere idasanzwe n’ingano zayo ku gishushanyo ni ibyo kwerekana gusa kandi ntibihuye n’uduce nyatwo.
NGF ihumura yahinzwe na CVD yigeze kwimurirwa ku buso bwa silikoni budafite ibara kandi ikoreshwa mu turemangingo tw’izuba15,16. Uburyo bwo guhindura ingufu buvamo (PCE) ni 1.5%. Izi NGF zigira imirimo myinshi nko gushyiramo ibice bifatika, inzira zo gutwaramo umuriro, na electrode zibonerana15,16. Ariko, firime ya grafiti ntabwo ingana. Ni ngombwa kongera kunoza no kugenzura neza uburyo firime ihangana n’urumuri n’uburyo electrode ya grafiti inyuramo, kubera ko iyi miterere yombi igira uruhare runini mu kugena agaciro ka PCE k’uturemangingo tw’izuba15,16. Ubusanzwe, firime za grafiti zigira urumuri rugaragara ku kigero cya 97.7%, ariko zifite ubushobozi bwo guhangana n’urumuri rugaragara bwa 200–3000 ohms/sq.16. Ubuhanga bwo guhangana n’urumuri rwa firime za grafiti bushobora kugabanuka binyuze mu kongera umubare w’uturemangingo (guhinduranya inshuro nyinshi uturemangingo twa graphene) no gukoresha HNO3 (~30 Ohm/sq.)66. Ariko, iyi nzira bifata igihe kirekire kandi imiterere itandukanye yo kohereza ntabwo ihora ikora neza. NGF yacu y'imbere ifite imiterere nk'ubushobozi bwo gutwara amashanyarazi bwa 2000 S/cm, ubushobozi bwo kwirinda filime bwa 50 ohm/sq. na 62% by'ubuhanga, bigatuma iba ubundi buryo bwiza bwo gukoresha imiyoboro y'amashanyarazi cyangwa electrodes zo guhangana n'izuba mu turemangingo tw'izuba15,16.
Nubwo imiterere n'ubuso bwa BS-NGF bisa na FS-NGF, ubukana bwayo buratandukanye ("Iterambere rya FS- na BS-NGF"). Mbere, twakoreshaga grafiti ya filime 22 yoroheje cyane nk'icyuma gipima gaze. Kubwibyo, twagerageje uburyo bwo gukoresha BS-NGF mu mirimo yo kumenya gaze (Ishusho ya SI10). Ubwa mbere, ibice bya BS-NGF bifite ingano ya mm2 byimuriwe kuri chip ya sensor ya electrode interdigitating (Ishusho ya SI10a-c). Ibisobanuro birambuye ku gukora chip byari byaravuzwe mbere; ubuso bwayo bukora ni 9 mm267. Mu mashusho ya SEM (Ishusho ya SI10b na c), electrode ya zahabu iri munsi yayo igaragara neza binyuze muri NGF. Nanone, biragaragara ko ubwinshi bwa chip bungana bwagezweho ku ngero zose. Ibipimo bya sensor ya gaze bya gaze zitandukanye byanditswe (Ishusho ya SI10d) (Ishusho ya SI11) kandi igipimo cy'ibisubizo cyavuyemo kigaragara mu mashusho ya SI10g. Birashoboka ko hamwe n'indi myuka ibangamira irimo SO2 (200 ppm), H2 (2%), CH4 (200 ppm), CO2 (2%), H2S (200 ppm) na NH3 (200 ppm). Impamvu imwe ishoboka ni NO2. imiterere ya electrophilic ya gazi22,68. Iyo ishyizwe ku buso bwa graphene, igabanya uburyo electron zinjira mu buryo bugezweho na sisitemu. Kugereranya amakuru y'igihe cyo gusubiza cya sensor ya BS-NGF na sensor zasohotse mbere bigaragazwa muri Imbonerahamwe ya SI2. Uburyo bwo kongera gukoresha sensor za NGF hakoreshejwe plasma ya UV, plasma ya O3 cyangwa thermal (50–150°C) ku ngero zagaragaye birakomeje, byaba byiza hagakurikiraho gushyira mu bikorwa sisitemu zishyizwemo69.
Mu gihe cyo gukora CVD, gukura kwa graphene biba ku mpande zombi za catalyst substrate41. Ariko, BS-graphene ikunze gusohoka mu gihe cyo kwimura41. Muri ubu bushakashatsi, twerekanye ko gukura kwa NGF ku rwego rwo hejuru no kohereza NGF idafite polymer bishobora kugerwaho ku mpande zombi z'inkunga ya catalyst. BS-NGF ni nto (~80 nm) kurusha FS-NGF (~100 nm), kandi iri tandukaniro risobanurwa n'uko BS-Ni idahura neza n'umuvuduko wa gaze ibanziriza. Twasanze kandi ko ubukana bwa substrate ya NiAR bugira ingaruka ku bukana bwa NGF. Ibi byavuye mu bushakashatsi bigaragaza ko FS-NGF yakuze ishobora gukoreshwa nk'ibikoresho bibanziriza graphene (binyuze mu buryo bwo gusohora70) cyangwa nk'umuyoboro uyobora amashanyarazi mu turemangingo tw'izuba15,16. Mu buryo bunyuranye, BS-NGF izakoreshwa mu gupima gaze (Ishusho ya SI9) ndetse wenda no mu buryo bwo kubika ingufu71,72 aho ubukana bwayo bw'ubuso buzaba ingirakamaro.
Ukurikije ibivuzwe haruguru, ni ingirakamaro guhuza akazi kari gukorwa ubu na filime za grafiti zashyizwe ahagaragara mbere zahinzwe na CVD hamwe no gukoresha nickel foil. Nkuko bigaragara mu mbonerahamwe ya 2, igitutu kinini twakoresheje cyagabanyije igihe cyo gukora (igihe cyo gukura) ndetse no mu bushyuhe buri hasi (muri dogere selisiyusi 850–1300). Twageze kandi ku iterambere rinini kuruta uko bisanzwe, bigaragaza ko hashobora kwaguka. Hari ibindi bintu byo gusuzuma, bimwe muri byo twabishyize mu mbonerahamwe.
NGF nziza cyane ifite impande ebyiri yahinzwe kuri nickel foil hakoreshejwe CVD catalytic. Mu gukuraho substrates gakondo za polymer (nk'izikoreshwa muri CVD graphene), tubasha kwimura NGF (yahinzwe inyuma n'imbere ya nickel foil) mu buryo busukuye kandi budafite inenge mu buryo busanzwe. By'umwihariko, NGF irimo uturere twa FLG na MLG (ubusanzwe 0.1% kugeza 3% kuri 100 µm2) twubatswe neza muri filime nini. Planar TEM igaragaza ko utu turere tugizwe n'uduce tubiri cyangwa dutatu twa graphite/graphene (amakristale cyangwa urwego, uko bikurikirana), bimwe muri byo bifite itandukaniro rya 10–20°. Uturere twa FLG na MLG ni two dushinzwe ubwisanzure bwa FS-NGF ku rumuri rugaragara. Ku bijyanye n'impapuro z'inyuma, zishobora gutwarwa zifatanye n'impapuro z'imbere kandi, nk'uko bigaragara, zishobora kugira intego y'imikorere (urugero, mu gupima gaze). Ubu bushakashatsi ni ingirakamaro cyane mu kugabanya imyanda n'ibiciro mu mikorere ya CVD mu nganda.
Muri rusange, ubugari bw'impuzandengo bwa CVD NGF buri hagati y'impapuro za grafiti (zo hasi n'izifite ibyiciro byinshi) na grafiti y'inganda (micrometer). Imiterere yazo ishimishije, hamwe n'uburyo bworoshye twakoze bwo kuyikora no kuyitwara, bituma izi filime ziba nziza cyane mu bikorwa bisaba uburyo grafiti ikora, hatitawe ku mafaranga y'inganda zikoresha ingufu nyinshi.
Icupa rya nikeli rya 25 μm (ubuziranenge bwa 99.5%, Goodfellow) ryashyizwe muri reactor ya CVD y'ubucuruzi (Aixtron 4-inch BMPro). Sisitemu yasukuwe na argon hanyuma ijyanwa ku gitutu cy'ibanze cya 10-3 mbar. Hanyuma icupa rya nikeli ryashyizwe muri Ar/H2 (Nyuma yo gufunga icupa rya Ni mu minota 5, icupa ryashyizwe ku gitutu cya 500 mbar kuri 900 °C. NGF yashyizwe mu muvuduko wa CH4/H2 (100 cm3 buri imwe) mu minota 5. Icyitegererezo cyakonjeshejwe kugeza ku bushyuhe buri munsi ya 700 °C hakoreshejwe umuvuduko wa Ar (4000 cm3) kuri 40 °C/min. Ibisobanuro birambuye ku buryo bwo kunoza uburyo bwo gukura kwa NGF birasobanurwa ahandi30.
Imiterere y'ubuso bw'icyitegererezo yagaragajwe na SEM hakoreshejwe mikorosikopi ya Zeiss Merlin (1 kV, 50 pA). Ubukana bw'ubuso bw'icyitegererezo n'ubugari bwa NGF byapimwe hakoreshejwe AFM (Dimension Icon SPM, Bruker). Ibipimo bya TEM na SAED byakozwe hakoreshejwe mikorosikopi ya FEI Titan 80–300 Cubed ifite imbunda isohora urumuri rwinshi (300 kV), monochromator ya FEI Wien yo mu bwoko bwa monochromator na lens ya CEOS spherical aberration corrector kugira ngo haboneke ibisubizo bya nyuma. Ingero za NGF zoherejwe mu miyoboro y'umuringa ya carbon lacy coated kugira ngo hakorwe isuzuma rya TEM rigororotse kandi hasesengurwe imiterere ya SAED. Bityo, inyinshi mu ngero z'icyitegererezo zihagarara mu mwenge w'urukiramende rushyigikira. Ingero za NGF zoherejwe zasesenguwe na XRD. Imiterere y'urumuri rwa X-ray yabonetse hakoreshejwe ifu ya diffractometer (Brucker, D2 phase shifter ifite isoko ya Cu Kα, 1.5418 Å na detector ya LYNXEYE) hakoreshejwe isoko y'imirasire ya Cu ifite umurambararo w'ikimenyetso cya mm 3.
Ibipimo byinshi bya Raman byafashwe hakoreshejwe mikorosikopi ya confocal (Alpha 300 RA, WITeC). Laser ya 532 nm ifite imbaraga nke zo gushyushya (25%) yakoreshejwe kugira ngo hirindwe ingaruka ziterwa n'ubushyuhe. Spektroskopi ya X-ray photoelectron (XPS) yakozwe kuri spectrometer ya Kratos Axis Ultra hejuru y'ingero ya 300 × 700 μm2 hakoreshejwe imirasire ya monochromatic Al Kα (hν = 1486.6 eV) ku ngufu za 150 W. Spektroskopi ya resolution yabonetse ku ngufu za transmission za 160 eV na 20 eV, uko bikurikirana. Ingero za NGF zoherejwe kuri SiO2 zaciwemo ibice (3 × 10 mm2 buri kimwe) hakoreshejwe laser ya PLS6MW (1.06 μm) ytterbium fiber kuri 30 W. Impande z'umuringa (ubugari bwa 50 μm) zakozwe hakoreshejwe silver paste munsi ya mikorosikopi y'urumuri. Igerageza ry’amashanyarazi n’ingaruka za Hall ryakozwe kuri izi ngero kuri 300 K n’impinduka mu mbaraga za rukuruzi za ± 9 Tesla muri sisitemu yo gupima imiterere y’umubiri (PPMS EverCool-II, Quantum Design, USA). Spektara ya UV-vis yafashwe hakoreshejwe Lambda 950 UV-vis spectrophotometer iri mu bwoko bwa 350-800 nm NGF yimuwe muri substrates za quartz n’ingero za quartz.
Imashini ipima ubukana bw'imiti (interdigitated electrode chip) yashyizwe ku rubuga rwa circuit 73 rwacapwe ku giti cyayo, maze ubukana bukurwaho byihuse. Urubaho rwa circuit rwacapwe aho igikoresho giherereye ruhujwe n'aho bahuza ibyuma hanyuma rushyirwa mu cyumba cyo kumenya gazi 74. Ibipimo byo kurwanya byafashwe kuri voltage ya 1 V hamwe no gupima buri gihe kuva aho basukuye kugeza aho bahuriye na gazi hanyuma bongera gusukura. Uru ruganda rwabanje gusukurwa hakoreshejwe azote kuri cm3 200 mu gihe cy'isaha 1 kugira ngo hamenyekane ko izindi analyte zose zari mu cyumba zikurwamo, harimo n'ubushuhe. Imashini zipima buri kimwe cya kabiri zarekuwe buhoro buhoro mu cyumba ku muvuduko umwe wa cm3 200 binyuze mu gufunga silinda ya N2.
Verisiyo ivuguruye y'iyi nkuru yasohotse kandi ushobora kuyibona ukoresheje umurongo uri hejuru y'iyi nkuru.
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