Muri silicon karbide imwe yo gukura kwa kristu, ubwikorezi bwumwuka wumubiri nuburyo bugezweho bwinganda. Kuburyo bwo gukura bwa PVT,ifu ya silicon karbideifite uruhare runini mubikorwa byo gukura. Ibipimo byose byaifu ya silicon karbidebigira ingaruka ku buryo butaziguye ubwiza bwo gukura kwa kristu imwe hamwe n'amashanyarazi. Mubikorwa byinganda byubu, bikunze gukoreshwaifu ya silicon karbidesynthesis inzira nuburyo bwo gukwirakwiza ubushyuhe bwo hejuru bwo hejuru.
Uburyo bwo kwikwirakwiza ubushyuhe bwo hejuru bukoresha ubushyuhe bwo hejuru kugirango butange reaction yubushyuhe bwambere kugirango itangire imiti, hanyuma ikoreshe ubushyuhe bwayo bwa chimique kugirango ibintu bitarakorwa bikomeze kurangiza imiti. Ariko, kubera ko imiti yimiti ya Si na C irekura ubushyuhe buke, izindi reaction zigomba kongerwaho kugirango zigumane reaction. Kubwibyo, intiti nyinshi zasabye ko habaho uburyo bwiza bwo kwimenyekanisha bwogukwirakwiza uburyo bushingiye kuri sisitemu, bushyira ahagaragara. Uburyo bwo kwiyamamaza bworoshye biroroshye kubishyira mubikorwa, kandi ibipimo bitandukanye bya synthesis biroroshye kugenzura neza. Synthesis nini yujuje ibyifuzo byinganda.
Nko mu 1999, Bridgeport yakoresheje uburyo bwo gukwirakwiza ubushyuhe bwo hejuru bwo guhuza ubushyuheIfu ya SiC, ariko yakoresheje ethoxysilane na fenol resin nkibikoresho fatizo, byari bihenze. Gao Pan nabandi bakoresheje ifu ya Si-isuku nini na C ifu nkibikoresho fatizo kugirango bahuzeIfu ya SiCnubushyuhe bwo hejuru cyane muburyo bwa argon. Ning Lina yateguye ibice-bininiIfu ya SiCna synthesis ya kabiri.
Itanura rishyushye rya induction ryashyutswe ryakozwe n'Ikigo cya kabiri cy'Ubushakashatsi mu Bushinwa Ikoranabuhanga rya Tekinoloji Itsinda ry’Ubushinwa rivanga ifu ya silicon hamwe nifu ya karubone ku kigero runaka cya stoichiometric ikabishyira muri grafite ikomeye. Uwitekaigishushanyo mboneraishyirwa mu itanura rishyushye rigereranya ubushyuhe bwo gushyushya, kandi ihinduka ryubushyuhe rikoreshwa muguhuza no guhindura icyiciro cyo hasi yubushyuhe hamwe nubushyuhe bwo hejuru bwa silicon karbide. Kubera ko ubushyuhe bwa β-SiC synthesis reaction mucyiciro cy'ubushyuhe buke buri munsi yubushyuhe bwo guhindagurika kwa Si, synthesis ya β-SiC munsi yumuvu mwinshi irashobora kwemeza ko ikwirakwiza. Uburyo bwo kumenyekanisha gaze ya argon, hydrogen na HCl muri synthesis ya α-SiC birinda kuboraIfu ya SiCmurwego rwo hejuru-ubushyuhe, kandi irashobora kugabanya neza azote iri muri poro ya α-SiC.
Shandong Tianyue yateguye itanura rya synthesis, akoresheje gaze ya silane nkibikoresho fatizo bya silikoni nifu ya karubone nkibikoresho fatizo bya karubone. Ingano ya gaze y'ibikoresho fatizo yatangijwe yahinduwe hakoreshejwe uburyo bubiri bwa synthesis, kandi ingano ya nyuma ya silicon karbide ingano yari hagati ya 50 na 5 000 um.
1 Kugenzura ibintu byifu ya synthesis
1.1 Ingaruka yubunini bwa powder kumikurire ya kristu
Ingano yubunini bwa silicon karbide ifu ifite uruhare runini kumikurire imwe rukumbi. Iterambere rya SiC imwe ya kirisiti yuburyo bwa PVT igerwaho cyane cyane muguhindura igipimo cya molarike ya silicon na karubone mugice cya gaze, naho igipimo cya molarike ya silicon na karubone mubice bya gaze ya gazi bifitanye isano nubunini bwa pisitori ya karubide ya silicon . Umuvuduko wuzuye hamwe na silicon-karubone igereranyo ya sisitemu yo gukura yiyongera hamwe no kugabanuka kwubunini bwibice. Iyo ingano yibice igabanutse kuva kuri mm 2-3 kugera kuri mm 0,06, igipimo cya silicon-karubone cyiyongera kuva kuri 1.3 kigera kuri 4.0. Iyo uduce duto duto kurwego runaka, umuvuduko wa Si igice cyiyongera, hanyuma hakorwa urwego rwa firime ya Si hejuru ya kirisiti ikura, bigatuma habaho gukura-gazi-amazi-akomeye, bigira ingaruka kuri polymorphism, inenge zumurongo hamwe nudusembwa twumurongo; muri kristu. Kubwibyo, ingano yubunini bwa silicon karbide yifu ya pisine igomba kugenzurwa neza.
Byongeye kandi, iyo ingano yifu yifu ya SiC ari ntoya, ifu ibora vuba, bigatuma gukura gukabije kwa kristu imwe ya SiC. Ku ruhande rumwe, mubushyuhe bwo hejuru bwubushyuhe bwa SiC imwe yo gukura kwa kirisiti, inzira ebyiri zo guhuza no kubora bikorwa icyarimwe. Ifu ya karibide ya silicon izabora kandi ikore karubone mugice cya gaze nicyiciro gikomeye nka Si, Si2C, SiC2, bikaviramo karubone ikomeye yifu ya polycristaline no gushiraho karubone muri kristu; kurundi ruhande, iyo igipimo cyo kubora cya poro cyihuta cyane, imiterere ya kristaliste ya SiC imwe ikuze ya kirisiti ikunda guhinduka, bigatuma bigorana kugenzura ubuziranenge bwa kristu imwe ikuze.
1.2 Ingaruka yifu ya kristu ifata kumikurire ya kristu
Gukura kwa SiC kristu imwe muburyo bwa PVT ni sublimation-recrystallisation yubushyuhe bwinshi. Imiterere ya kristu yibikoresho fatizo bya SiC igira uruhare runini mu mikurire ya kristu. Muburyo bwo guhuza ifu, icyiciro cyo hasi yubushyuhe bwo hasi (β-SiC) hamwe nububiko bwa cubic selile yingirabuzimafatizo hamwe nicyiciro cyo hejuru cyubushyuhe bwo hejuru (α-SiC) hamwe nuburinganire bwa mpande esheshatu zingirabuzimafatizo bizakorwa cyane cyane . Hariho uburyo bwinshi bwa silicon karbide ya kirisiti hamwe nubushyuhe buke bwo kugenzura ubushyuhe. Kurugero, 3C-SiC izahinduka muri silikoni ya silicon karbide polymorph, ni ukuvuga 4H / 6H-SiC, mubushyuhe buri hejuru ya 1900 ° C.
Mugihe kimwe cyo gukura kwa kirisiti imwe, iyo powder-SiC ifu ikoreshwa mugukura kristu, igipimo cya silikoni-karubone iruta 5.5, mugihe iyo ifu ya α-SiC ikoreshwa muguhinga kristu, igipimo cya silikoni-karubone ni 1.2. Iyo ubushyuhe buzamutse, icyiciro cyinzibacyuho kibaho mubikomeye. Muri iki gihe, igipimo cya mara mu cyiciro cya gaze kiba kinini, kikaba kidafasha gukura kwa kirisiti. Byongeye kandi, ibindi byuka bya gaze ya gaze, harimo karubone, silikoni, na dioxyde de silicon, byabyara byoroshye mugihe cyinzibacyuho. Kubaho kwimyanda itera kristu kubyara microtubes nubusa. Kubwibyo, ifu ya kirisiti igomba kugenzurwa neza.
1.3 Ingaruka zumwanda wifu kumikurire ya kristu
Ibirimo umwanda biri mu ifu ya SiC bigira ingaruka kuri nucleation ya spontaneous mugihe cyo gukura kwa kirisiti. Iyo hejuru yibirimo umwanda, ntibishoboka ko kristu ihinduka ubwayo. Kuri SiC, ibyingenzi byingenzi byanduye birimo B, Al, V, na Ni, bishobora gutangizwa nibikoresho byo gutunganya mugihe cyo gutunganya ifu ya silicon nifu ya karubone. Muri byo, B na Al nizo nyamukuru zidafite ingufu zingirakamaro zakira muri SiC, bigatuma kugabanuka kwa SiC kugabanuka. Ibindi byanduye byicyuma bizana ingufu nyinshi, bikavamo imashanyarazi idahindagurika ya sisitemu imwe ya kirisiti ya SiC mubushyuhe bwinshi, kandi ikagira ingaruka zikomeye kumiterere yumuriro wamashanyarazi yumutuku mwinshi wigice kimwe cya kirisiti, cyane cyane ukurwanya. Kubwibyo, ifu yuzuye ya silicon karbide ifu igomba guhurizwa hamwe bishoboka.
1.4 Ingaruka yibigize azote mu ifu kumikurire ya kristu
Urwego rwibintu bya azote rugena ubukana bwa substrate imwe. Inganda zikomeye zikeneye guhindura azote doping yibikoresho bya sintetike ukurikije uburyo bwo gukura kwa kristu ikuze mugihe cyo guhuza ifu. Igice kinini-cyera-kirisile silicon karbide imwe ya kristal substrate ni ibikoresho byizewe cyane mubikoresho bya elegitoroniki. Kugirango ukure-isuku-y-igice-imwe-imwe-imwe-ya-kristal substrate ifite imbaraga zo kurwanya cyane hamwe n’amashanyarazi meza cyane, ibikubiye muri azote nyamukuru yanduye muri substrate bigomba kugenzurwa kurwego rwo hasi. Imiyoboro imwe ya kristu isaba ibintu bya azote kugenzurwa cyane.
2 Tekinoroji yingenzi yo kugenzura ifu ya synthesis
Bitewe nuburyo butandukanye bwo gukoresha ibidukikije bya silicon karbide substrate, tekinoroji ya synthesis ya poro yo gukura nayo ifite inzira zitandukanye. Kuri N-ubwoko bwimyororokere imwe ya kristu yo gukura, irasukuye cyane kandi icyiciro kimwe kirakenewe; mugihe kimwe cya kabiri cyokwirinda ifu yo gukura, birasabwa kugenzura cyane ibirimo azote.
2.1 Kugenzura ingano yubunini
2.1.1 Ubushyuhe bwa Synthesis
Kugumana ubundi buryo bwimikorere idahindutse, ifu ya SiC yakozwe mubushyuhe bwa synthesis ya 1900 ℃, 2000 ℃, 2100 ℃, na 2200 ℃ byapimwe kandi birasesengurwa. Nkuko bigaragara ku gishushanyo cya 1, birashobora kugaragara ko ingano yingingo zingana na 250 ~ 600 mkm kuri 1900 and, naho ingano yingingo ikiyongera kugera kuri 600 ~ 850 mm kuri 2000 ℃, kandi ingano yingingo ihinduka cyane. Iyo ubushyuhe bukomeje kwiyongera kugera kuri 2100 ℃, ingano yifu ya SiC ni 850 ~ 2360 mm, kandi kwiyongera bikunda kuba byoroheje. Ingano ya SiC kuri 2200 ℃ irahagaze kuri 2360 mm. Ubwiyongere bwubushyuhe bwa synthesis kuva 1900 ℃ bugira ingaruka nziza mubunini bwa SiC. Iyo ubushyuhe bwa synthesis bukomeje kwiyongera kuva 2100 ℃, ingano yingingo ntigihinduka cyane. Kubwibyo, iyo synthesis yubushyuhe yashyizwe kuri 2100 ℃, ingano nini yingirakamaro irashobora guhuzwa mugukoresha ingufu nke.
2.1.2 Igihe cyo guhuza
Ibindi bikorwa byimikorere ntibigihinduka, kandi igihe cyo guhuza cyashyizwe kuri 4 h, 8 h, na 12 h. Isesengura ryakozwe rya SiC ifu yerekana isesengura ryerekanwe mubishusho 2. Byagaragaye ko igihe cyo guhuza kigira ingaruka zikomeye kubunini bwa SiC. Iyo igihe cyo guhuza ni 4 h, ingano yingingo ikwirakwizwa cyane kuri 200 mkm; iyo synthesis igihe ni 8 h, ingano yubukorikori yiyongera cyane, ikwirakwizwa cyane kuri 1 000 μ m; mugihe synthesis ikomeje kwiyongera, ingano yingingo yiyongera cyane, ikwirakwizwa hafi 2 000 mm.
2.1.3 Ingaruka yubunini bwibikoresho fatizo
Mugihe uruganda rukora ibikoresho bya silikoni yo murugo rugenda rutera imbere buhoro buhoro, ubuziranenge bwibikoresho bya silikoni nabwo burarushaho kunozwa. Kugeza ubu, ibikoresho bya silikoni bikoreshwa muri synthesis bigabanijwe cyane muri silicon granular na silicon ya puderi, nkuko bigaragara ku gishushanyo cya 3.
Ibikoresho bitandukanye bya silicon byakoreshejwe mugukora ubushakashatsi bwa silicon karbide. Kugereranya ibicuruzwa bya sintetike bigaragara mu gishushanyo cya 4. Isesengura ryerekana ko iyo ukoresheje ibikoresho bibisi bya silicon, umubare munini wibintu bya Si biboneka mubicuruzwa. Nyuma yo guhagarika silicon kumeneka kunshuro ya kabiri, Si element mubicuruzwa bya sintetike iragabanuka cyane, ariko iracyahari. Hanyuma, ifu ya silicon ikoreshwa muguhindura, kandi SiC yonyine irahari mubicuruzwa. Ibi ni ukubera ko mubikorwa byo gukora, silikoni nini nini ikenera kubanza gukorerwa reaction ya synthesis, kandi karbide ya silicon ikomatanyirizwa hejuru, ikabuza ifu yimbere ya Si gukomeza guhuza ifu ya C. Kubwibyo, niba guhagarika silikoni ikoreshwa nkibikoresho fatizo, igomba guhonyorwa hanyuma igakorerwa inzira ya kabiri kugirango ibone ifu ya karubide ya silikoni kugirango ikure neza.
2.2 Ifu ya kirisiti igenzura
2.2.1 Ingaruka yubushyuhe bwa synthesis
Kugumana ubundi buryo bwimikorere idahindutse, ubushyuhe bwa synthesis ni 1500 ℃, 1700 ℃, 1900 ℃, na 2100 and, kandi ifu ya SiC yakozwe iratorwa kandi igasesengurwa. Nkuko bigaragara ku gishushanyo cya 5, β-SiC ni umuhondo wubutaka, naho α-SiC yoroshye mu ibara. Iyo witegereje ibara na morphologie yifu ya synthesize, birashobora kwemezwa ko ibicuruzwa bivanze ari β-SiC mubushyuhe bwa 1500 ℃ na 1700 ℃. Kuri 1900 ℃, ibara riba ryoroheje, kandi ibice bitandatu bigaragarira, byerekana ko nyuma yuko ubushyuhe buzamutse bukagera kuri 1900 ℃, inzibacyuho ibaho, kandi igice cya β-SiC gihinduka α-SiC; iyo ubushyuhe bukomeje kuzamuka kugera kuri 2100 ℃, usanga ibice bigize synthesize bibonerana, kandi α-SiC byahinduwe.
2.2.2 Ingaruka yigihe cya synthesis
Ibindi bikorwa byimikorere ntibigihinduka, kandi igihe cyo guhuza cyashyizwe kuri 4h, 8h, na 12h. Ifu ya SiC yakozwe ikorwa kandi igasesengurwa na diffractometero (XRD). Ibisubizo byerekanwe ku gishushanyo cya 6. Igihe cyo guhuza kigira ingaruka runaka kubicuruzwa byashizwemo nifu ya SiC. Iyo igihe cyo guhuza ni 4 h na 8 h, ibicuruzwa byubukorikori ni 6H-SiC; iyo synthesis igihe ni 12 h, 15R-SiC igaragara mubicuruzwa.
2.2.3 Ingaruka yikigereranyo cyibikoresho fatizo
Izindi nzira ntizihinduka, isesengura ryibintu bya silicon-karubone birasesengurwa, kandi ibipimo ni 1.00, 1.05, 1.10 na 1.15 kubushakashatsi bwa synthesis. Ibisubizo byerekanwe ku gishushanyo 7.
Duhereye kuri XRD, birashobora kugaragara ko mugihe igipimo cya silicon-karubone irenze 1.05, Si irenze igaragara mubicuruzwa, kandi iyo igipimo cya silicon-karubone kiri munsi ya 1.05, C irenze igaragara. Iyo igipimo cya silicon-karubone ari 1.05, karubone yubusa mubicuruzwa bya sintetike iba ikuweho, kandi nta silikoni yubusa igaragara. Kubwibyo, ingano yikigereranyo cya silicon-karubone igomba kuba 1.05 kugirango ihuze neza-SiC.
2.3 Igenzura rya azote nkeya muri poro
2.3.1 Ibikoresho fatizo bya sintetike
Ibikoresho fatizo bikoreshwa muri ubu bushakashatsi ni ifu ya karubone isukuye cyane hamwe nifu ya silicon nziza cyane hamwe na diametre yo hagati ya 20 mm. Bitewe nubunini bwazo buto hamwe nubuso bunini bwihariye, biroroshye kwinjiza N2 mukirere. Mugihe cyo guhuza ifu, izazanwa muburyo bwa kristu yifu. Kugirango imikurire ya N-kristu yo mu bwoko bwa kristu, doping itaringaniye ya N2 mu ifu iganisha ku kurwanya kuringaniza kristu ndetse no guhinduka muburyo bwa kristu. Azote irimo ifu ya synthesize nyuma ya hydrogène yatangijwe ni mike cyane. Ni ukubera ko ingano ya molekile ya hydrogène ari nto. Iyo N2 yamamajwe mu ifu ya karubone nifu ya silikoni ishyushye kandi ikangirika hejuru, H2 ikwirakwira rwose mu cyuho kiri hagati yifu nubunini bwayo buto, igasimbuza umwanya wa N2, na N2 igahunga ikaboneka mugihe cyimyuka, kugera ku ntego yo gukuraho ibirimo azote.
2.3.2
Mugihe cyo guhuza ifu ya karubide ya silicon, kubera ko radiyo ya atome ya karubone na atome ya azote isa, azote izasimbuza imyanya ya karubone muri karubide ya silicon, bityo bikongerwamo azote. Ubu buryo bwikigereranyo bukoresha uburyo bwo kumenyekanisha H2, na H2 ikora hamwe nibintu bya karubone na silikoni muri synthesis ikomeye kugirango bibyare imyuka ya C2H2, C2H, na SiH. Ibintu bya karubone byiyongera binyuze mu kohereza gaze, bityo bikagabanya imyanya ya karubone. Intego yo gukuraho azote iragerwaho.
2.3.3 Gutunganya inyuma ya azote igenzura
Graphite ibamba ifite porotike nini irashobora gukoreshwa nkisoko yinyongera ya C kugirango ikure imyuka ya Si mubice bya gaze, kugabanya Si mubice bya gaze, bityo byongere C / Si. Muri icyo gihe, umusaraba wa grafite urashobora kandi kwitwara hamwe nikirere cya Si kugirango ubyare Si2C, SiC2 na SiC, ibyo bikaba bihwanye nikirere cya Si kizana C isoko ya grafite ingirakamaro mukirere gikura, ikongera igipimo cya C, kandi ikongera na karuboni-silikoni . Kubwibyo, igipimo cya karubone-silikoni gishobora kwiyongera ukoresheje umusaraba wa grafite ufite umubyimba munini, kugabanya imyanya ya karubone, no kugera ku ntego yo gukuraho azote.
3 Gusesengura no gushushanya uburyo bumwe bwo guhuza ifu ya kristu
3.1 Ihame nigishushanyo mbonera cya synthesis
Binyuze mu bushakashatsi bwuzuye bwavuzwe haruguru ku kugenzura ingano yubunini, imiterere ya kirisiti hamwe na azote yibigize ifu ya synthesis, birasabwa inzira ya synthesis. Ifu yera cyane C ifu ya Si nifu ya Si byatoranijwe, kandi biravanze neza kandi bishyirwa mubishushanyo mbonera bikurikije igipimo cya silicon-karubone ya 1.05. Intambwe zikorwa zigabanijwemo ibice bine:
1. Iyi nzira irashobora gukuraho ibintu bya azote hejuru yifu ya karubone nifu ya silicon.
) Iyi nzira irashobora gukuraho ibintu bya azote hejuru yifu ya karubone nifu ya silicon, kandi bigatwara azote mumashanyarazi.
3) Synthesis yuburyo bwubushyuhe buke, wimure kuri 5 × 10-4 Pa, hanyuma ushushe kuri 1350 ℃, komeza amasaha 12, hanyuma ushyireho hydrogène kugirango igitutu cya chambre kigere kuri 80 kPa, komeza isaha 1. Iyi nzira irashobora gukuraho azote ihindagurika mugihe cya synthesis.
4. Iyi nzira irangiza guhindura ifu ya silicon karbide ivuye kuri β-SiC ikagera kuri α-SiC ikanarangiza imikurire ya selile.
Hanyuma, tegereza ubushyuhe bwicyumba kugirango bukonje ubushyuhe bwicyumba, wuzuze umuvuduko wikirere, hanyuma ukuremo ifu.
3.2 Ifu yanyuma yo gutunganya
Ifu imaze guhuzwa nuburyo bwavuzwe haruguru, igomba gutunganywa kugirango ikureho karubone yubusa, silikoni nibindi byanduye byuma hanyuma ikagaragaza ubunini bwayo. Ubwa mbere, ifu ya synthesize ishyirwa mumashini yumupira kugirango ujanjagurwe, hanyuma ifu ya karubide ya silicon yajanjaguwe ishyirwa mu itanura rya muffle hanyuma ishyuha kugeza kuri 450 ° C na ogisijeni. Carbone yubusa muri poro ihindurwamo ubushyuhe kugirango habeho gaze karuboni ya dioxyde de gaze mucyumba, bityo ikageraho ikureho karubone yubusa. Ibikurikiraho, hategurwa amazi yo kwisukura acide ashyirwa mumashini isukura silicon karbide kugirango isukure kugirango ikureho karubone, silikoni hamwe nicyuma gisigara cyakozwe mugihe cyo guhuza. Nyuma yibyo, aside isigaye yozwa mumazi meza hanyuma ikuma. Ifu yumye irerekanwa muri ecran yinyeganyeza kugirango ingano yo gutoranya ingano yo gukura kwa kristu.
Igihe cyo kohereza: Kanama-08-2024