I-Selenium, njengesixhobo esibalulekileyo se-semiconductor kunye nezinto eziluhlaza zoshishino, ukusebenza kwayo kuchaphazeleka ngokuthe ngqo bubunyulu bayo. Ngexesha lenkqubo yokucocwa kwe-vacuum distillation, ukungcola kwe-oksijini yenye yezinto eziphambili ezichaphazela ubunyulu be-selenium. Eli nqaku libonelela ngengxoxo eneenkcukacha ngeendlela ezahlukeneyo kunye neendlela zokunciphisa umxholo we-oksijini ngexesha lokucocwa kwe-selenium nge-vacuum distillation.

I. Ukunciphisa uMxholo weOksijini kwiSigaba sokuNyangwa kwezinto eziluhlaza

1. Ukucocwa kwangaphambili kwezinto ezisetyenziswa gwenxa

I-selenium eluhlaza idla ngokuqulatha ukungcola okwahlukeneyo, kuquka ii-oxide. Ngaphambi kokuba kungene kwinkqubo yokucocwa kwe-vacuum, kufuneka kusetyenziswe iindlela zokucoca ngeekhemikhali ukususa ii-oxides ezingaphezulu. Izisombululo zokucoca ezisetyenziswa rhoqo ziquka:

• Nciphisa isisombululo se-hydrochloric acid (uxinzelelo lwe-5-10%): Inyibilikisa ngempumelelo ii-oxides ezifana ne-SeO₂
• I-ethanol okanye i-acetone: Isetyenziselwa ukususa izinto ezingcolisayo eziphilayo
• Amanzi acocekileyo: Ukuhlamba okuninzi ukususa i-asidi eseleyo

Emva kokucoca, ukomisa kufuneka kwenziwe phantsi kwegesi engasebenziyo (umz., i-Ar okanye i-N₂) ukuze kuthintelwe ukuphinda kufakwe i-oxidation.

2. Unyango lwangaphambi kokunciphisa izinto eziluhlaza

Ukunciphisa unyango lwezinto ezikrwada ngaphambi kokuba kukhutshwe i-vacuum distillation kunokunciphisa kakhulu umxholo we-oksijini:

• Ukunciphisa i-hydrogen: Faka i-hydrogen ecocekileyo kakhulu (ubumsulwa ≥99.999%) kwi-200-300°C ukunciphisa i-SeO₂ kwi-elemental selenium
• Ukunciphisa iicarbohydrate: Xuba izinto eziluhlaza zeselenium kunye nomgubo wekhabhoni ococekileyo kakhulu uze ufudumale ukuya kuma-400-500°C phantsi kwe-vacuum okanye umoya ongasebenziyo, nto leyo ebangela ukuba kubekho impendulo C + SeO₂ → Se + CO₂
• Ukunciphisa i-sulfide: Iigesi ezifana ne-H₂S zinokunciphisa i-selenium oxides kumaqondo obushushu aphantsi.

II. Uyilo kunye nokuphuculwa kokusebenza kweNkqubo yokuCoca iVacuum

1. Ukukhethwa kunye noBume beNkqubo yoVutha

Indawo ene-vacuum eninzi ibalulekile ekunciphiseni umxholo we-oxygen:

• Sebenzisa ipompo yokusasaza kunye nendibaniselwano yepompo yoomatshini, apho i-vacuum ephezulu ifikelela ubuncinane kwi-10⁻⁴ Pa
• Inkqubo kufuneka ixhotyiswe ngesixhobo sokubamba esibandayo ukuthintela ukusasazeka komphunga weoyile emva.
• Zonke iziqhagamshelo kufuneka zisebenzise izitywino zesinyithi ukuze zingaphumi igesi kwizitywino zerabha
• Inkqubo kufuneka ikhuphe igesi eyaneleyo ekubhakeni (200-250°C, iiyure ezili-12-24)

2. Ulawulo oluchanekileyo lobushushu kunye noxinzelelo lwe-Distillation

Iindidi zeparameter zenkqubo ezifanelekileyo:

• Ubushushu bokunyibilikisa: Bulawulwa ngaphakathi koluhlu lwe-220-280°C (ngaphantsi kweqondo lokubila le-selenium eliyi-685°C)
• Uxinzelelo lwenkqubo: Lugcinwa phakathi kwe-1-10 Pa
• Izinga lokufudumeza: 5-10°C/min ukuze kuthintelwe ukufuma ngamandla kunye nokufakwa koqeqesho
• Ubushushu bendawo yokufuma: Igcinwa kwi-50-80°C ukuqinisekisa ukufuma okupheleleyo kweselenium

3. Itekhnoloji yokunyibilikisa ii-Multi-Stage Distillation

Ukucoca nge-multi-stage kunokunciphisa kancinci kancinci umthamo we-oksijini:

• Inqanaba lokuqala: Ukucocwa okurhabaxa ukuze kususwe uninzi lokungcola okuguquguqukayo
• Isigaba sesibini: Ulawulo oluchanekileyo lobushushu ukuze kuqokelelwe iqhekeza eliphambili
• Inqanaba lesithathu: Ukucoca okucothayo, okushushu kancinci ukuze kufunyanwe imveliso ecocekileyo kakhulu
  Amaqondo obushushu ahlukeneyo okufuma angasetyenziswa phakathi kwezigaba zokufuma okuqhekezayo

III. Amanyathelo eNkqubo yoNcedo

1. Itekhnoloji yoKhuseleko lweGesi engasebenziyo

Nangona isebenza phantsi kwe-vacuum, ukungeniswa ngokufanelekileyo kwegesi ecocekileyo kakhulu kunceda ukunciphisa umxholo we-oksijini:

• Emva kokuphuma kwinkqubo, gcwalisa nge-argon ecocekileyo kakhulu (ubumsulwa ≥99.9995%) ukuya kwi-1000 Pa
• Sebenzisa ukhuseleko lokuhamba kwegesi oluguqukayo, ngokuqhubekayo ufaka inani elincinci le-argon (10-20 sccm)
• Faka izicoci zegesi ezisebenzayo kakhulu kwiindawo zokungena zegesi ukuze ususe ioksijini eseleyo kunye nokufuma

2. Ukongezwa kwee-Oxygen Scavengers

Ukongeza izinto ezifanelekileyo zokususa ioksijini kwizinto eziluhlaza kunokunciphisa ngempumelelo umthamo weoksijini:

• Isinyithi seMagnesium: Ubudlelwane obuqinileyo kwioksijini, okwenza iMgO
• Umgubo we-aluminiyam: Ungasusa ioksijini nesalfure ngaxeshanye
• Iimetali zomhlaba ezingaqhelekanga: Ezifana ne-Y, i-La, njl., ezinemiphumo emihle yokususa ioksijini
  Ubungakanani bomxumi we-oxygen scavenger buqhele ukuba yi-0.1-0.5 wt% yezinto ezikrwada; ubuninzi obugqithisileyo bunokuchaphazela ubumsulwa beselenium

3. Itekhnoloji yokuhluza enyibilikisiweyo

Ukucoca i-selenium enyibilikisiweyo ngaphambi kokuba inyibilikiswe:

• Sebenzisa izihluzi ze-quartz okanye ze-ceramic ezinobukhulu beembobo eziyi-1-5 μm
• Lawula ubushushu bokucoca kwi-220-250°C
• Ingasusa amasuntswana e-oxide eqinileyo
• Izihluzi kufuneka zikhutshwe igesi kwangaphambili phantsi kwe-vacuum ephezulu

IV. Unyango kunye nokugcinwa emva koNyango

1. Ukuqokelelwa nokuphathwa kweMveliso

• Umqokeleli we-condenser kufuneka ayilwe njengesakhiwo esinokususwa ukuze kube lula ukufumana izinto kwindawo engasebenziyo
• Iingots zeselenium eziqokelelweyo kufuneka zipakishwe kwibhokisi yeglavu ye-argon
• Ukugrumba umphezulu kungenziwa ukuba kuyimfuneko ukususa iileya ezinokubakho ze-oxide

2. Ulawulo lweMeko yoGcino

• Indawo yokugcina kufuneka igcinwe yomile (indawo yokubanda ≤-60°C)
• Sebenzisa upakisho olutywiniweyo olunezingqimba ezimbini oluzaliswe yigesi engenamanzi ecocekileyo kakhulu
• Ubushushu bokugcina obucetyiswayo obungaphantsi kwama-20°C
• Kuphephe ukuvezwa ekukhanyeni ukuze uthintele iimpendulo ze-photocatalytic oxidation

V. Ulawulo loMgangatho kunye noVavanyo

1. Itekhnoloji yokubeka esweni kwi-Intanethi

• Faka ii-residual gas analyzers (RGA) ukuze ujonge uxinzelelo lwe-oxygen oluyinxenye ngexesha langempela
• Sebenzisa izinzwa zeoksijini ukulawula umxholo weoksijini kwiigesi ezikhuselayo
• Sebenzisa i-infrared spectroscopy ukuchonga iincopho zokufunxwa kweempawu ze-Se-O bonds

2. Uhlalutyo lweMveliso oluGqityiweyo

• Sebenzisa indlela yokufunxa igesi engangenisi gazi ukuze ubone ubungakanani beoksijini
• I-Secondary ion mass spectrometry (SIMS) yokuhlalutya ukusasazwa kweoksijini
• I-X-ray photoelectron spectroscopy (XPS) ukufumanisa imeko yeekhemikhali ezikumphezulu

Ngokusebenzisa amanyathelo apheleleyo achazwe apha ngasentla, umxholo weoksijini unokulawulwa ngaphantsi kwe-1 ppm ngexesha lokucocwa kwe-selenium nge-vacuum distillation, ukuhlangabezana neemfuno zokusetyenziswa kwe-selenium ecocekileyo kakhulu. Kwimveliso yokwenyani, iiparameter zenkqubo kufuneka ziphuculwe ngokusekelwe kwiimeko zezixhobo kunye neemfuno zemveliso, kwaye kufuneka kusekwe inkqubo yokulawula umgangatho engqongqo.