I-Selenium, njengezinto ezibalulekile ze-semiconductor kanye nezinto zokusetshenziswa zezimboni, ukusebenza kwayo kuthinteka ngqo ubumsulwa bayo. Ngesikhathi senqubo yokuhlanzwa kwe-vacuum distillation, ukungcola kwe-oxygen kungenye yezinto eziyinhloko ezithonya ubumsulwa be-selenium. Lesi sihloko sinikeza ingxoxo eningiliziwe yezindlela namasu ahlukahlukene okunciphisa okuqukethwe kwe-oxygen ngesikhathi sokuhlanzwa kwe-selenium nge-vacuum distillation.

I. Ukunciphisa Okuqukethwe Oksijini Esigabeni Sokwelashwa Kwangaphambi Kokusetshenziswa Kwezinto Eziluhlaza

1. Ukuhlanzwa Kwasekuqaleni Kwezinto Zokusetshenziswa

I-selenium eluhlaza ngokuvamile iqukethe ukungcola okuhlukahlukene, okuhlanganisa ama-oxide. Ngaphambi kokungena ohlelweni lokuhluza nge-vacuum, izindlela zokuhlanza ngamakhemikhali kufanele zisetshenziswe ukususa ama-oxide angaphezulu. Izixazululo zokuhlanza ezivame ukusetshenziswa zifaka:

• Nciphisa isixazululo se-hydrochloric acid (ukuhlushwa okungu-5-10%): Incibilikisa ngempumelelo ama-oxide afana ne-SeO₂
• I-ethanol noma i-acetone: Isetshenziselwa ukususa ukungcola okungokwemvelo
• Amanzi ahlanjululwe: Ukuhlanza okuningi ukususa i-asidi esele

Ngemva kokuhlanza, ukomisa kufanele kwenziwe ngaphansi kwesimo segesi esingasebenzi (isib., i-Ar noma i-N₂) ukuvimbela ukuphinda kufakwe i-oxidation.

2. Ukwelashwa Kwangaphambi Kokunciphisa Izinto Ezingavuthiwe

Ukwelashwa kokunciphisa izinto zokusetshenziswa ngaphambi kokucwiliswa kwe-vacuum kunganciphisa kakhulu okuqukethwe yi-oxygen:

• Ukunciphisa i-hydrogen: Faka i-hydrogen ehlanzekile kakhulu (ubumsulwa ≥99.999%) ku-200-300°C ukuze kuncishiswe i-SeO₂ ibe yi-selenium eyisisekelo
• Ukunciphisa ama-carbohydrate: Hlanganisa izinto zokusetshenziswa ze-selenium ne-carbon powder ehlanzekile kakhulu bese ushisa ku-400-500°C ngaphansi kwe-vacuum noma umoya ongasebenzi, okubangela ukusabela kwe-C + SeO₂ → Se + CO₂
• Ukunciphisa i-sulfide: Amagesi anjenge-H₂S anganciphisa i-selenium oxides emazingeni okushisa aphansi kakhulu

II. Ukuklama Nokwenza Kahle Ukusebenza Kohlelo Lokuhluza I-Vacuum

1. Ukukhethwa Nokucushwa Kohlelo Lokuhlanza I-Vacuum

Indawo ene-vacuum ephezulu ibalulekile ekunciphiseni okuqukethwe yi-oxygen:

• Sebenzisa inhlanganisela yephampu yokusabalalisa kanye nephampu yomshini, ene-vacuum ephezulu efinyelela okungenani ku-10⁻⁴ Pa
• Uhlelo kufanele lufakwe isicupho esibandayo ukuvimbela ukusabalala komphunga kawoyela ngemuva
• Zonke izixhumanisi kufanele zisebenzise izivalo zensimbi ukuze zigweme ukuphuma kwegesi ezivaloni zerabha
• Uhlelo kufanele lukhiphe igesi eyanele ekubhakeni (200-250°C, amahora angu-12-24)

2. Ukulawulwa Okunembile Kokushisa Nokucindezela Kwe-Distillation

Ukuhlanganiswa kwepharamitha yenqubo efanele:

• Izinga lokushisa lokucwilisa: Lilawulwa ngaphakathi kobubanzi obungu-220-280°C (ngaphansi kwezinga lokubila le-selenium elingu-685°C)
• Ukucindezela kwesistimu: Kugcinwa phakathi kuka-1-10 Pa
• Izinga lokushisa: 5-10°C/min ukugwema ukuhwamuka okunamandla kanye nokufakwa kwe-training
• Izinga lokushisa lendawo yokuvunda: Ligcinwa ku-50-80°C ukuqinisekisa ukuvunda okuphelele kwe-selenium

3. Ubuchwepheshe Bokuhluza Izigaba Eziningi

Ukuhluzwa kwezigaba eziningi kunganciphisa kancane kancane okuqukethwe komoya-mpilo:

• Isigaba sokuqala: Ukucwiliswa okuqinile ukuze kususwe ukungcola okuningi okuguquguqukayo
• Isigaba sesibili: Ukulawula izinga lokushisa okunembile ukuqoqa ingxenye eyinhloko
• Isigaba sesithathu: Ukushisa okuphansi, ukuhluzwa kancane ukuze kutholakale umkhiqizo ohlanzekile kakhulu
  Amazinga okushisa ahlukene okufiphaza angasetshenziswa phakathi kwezigaba zofiphaza oluyingxenye

III. Izinyathelo Zenqubo Esizayo

1. Ubuchwepheshe Bokuvikela Igesi Engasebenzi

Nakuba isebenza ngaphansi kwe-vacuum, ukufakwa okufanele kwegesi ehlanzekile kakhulu kusiza ukunciphisa okuqukethwe yi-oxygen:

• Ngemva kokuphuma ohlelweni, gcwalisa nge-argon ehlanzekile kakhulu (ubumsulwa ≥99.9995%) kuya ku-1000 Pa
• Sebenzisa ukuvikelwa kokugeleza kwegesi okuguquguqukayo, ngokuqhubekayo ufaka inani elincane le-argon (10-20 sccm)
• Faka izihlanzi zegesi ezisebenza kahle kakhulu ezindaweni zokungenisa igesi ukuze ususe i-oxygen eseleyo kanye nomswakama

2. Ukwengezwa Kwezinto Zokususa Umoya-mpilo

Ukwengeza izinto zokususa umoya-mpilo ezifanele ezintweni ezingavuthiwe kunganciphisa ngempumelelo okuqukethwe umoya-mpilo:

• Insimbi ye-Magnesium: Ukusondelana okunamandla komoya-mpilo, okwakha i-MgO
• Impuphu ye-aluminium: Ingasusa umoya-mpilo nesibabule ngasikhathi sinye
• Izinsimbi zomhlaba ezingavamile: Njenge-Y, i-La, njll., ezinemiphumela emihle kakhulu yokususa umoya-mpilo
  Inani le-oxygen scavenger ngokuvamile liyi-0.1-0.5 wt% yezinto zokusetshenziswa; amanani amaningi angathinta ubumsulwa be-selenium

3. Ubuchwepheshe Bokuhlunga Okuncibilikisiwe

Ukuhlunga i-selenium encibilikisiwe ngaphambi kokuyihluza:

• Sebenzisa izihlungi ze-quartz noma ze-ceramic ezinobukhulu be-pore obungu-1-5 μm
• Lawula izinga lokushisa lokuhlunga ku-220-250°C
• Ingasusa izinhlayiya ze-oxide eqinile
• Izihlungi kufanele zikhishwe ugesi ngaphambi kokusebenzisa i-vacuum ephezulu

IV. Ukwelashwa Nokugcinwa Ngemva Kokwelashwa

1. Ukuqoqwa Nokuphathwa Komkhiqizo

• Isiqoqi se-condenser kufanele sakhiwe njengesakhiwo esingasuswa ukuze kube lula ukuthola izinto endaweni engasebenzi kahle.
• Ama-ingot e-selenium aqoqiwe kufanele afakwe ebhokisini legilavu ​​​​le-argon
• Ukugcaba okungaphezulu kungenziwa uma kudingeka ukuze kususwe izingqimba ezingaba khona ze-oxide

2. Ukulawulwa Kwesimo Sesitoreji

• Indawo yokugcina kufanele igcinwe yomile (indawo yamazolo ≤-60°C)
• Sebenzisa iphakheji evaliwe enezingqimba ezimbili egcwele igesi engenasici ehlanzekile kakhulu
• Izinga lokushisa elinconyiwe lokugcina ngaphansi kwama-20°C
• Gwema ukuvezwa ekukhanyeni ukuze uvimbele ukusabela kwe-photocatalytic oxidation

V. Ukulawulwa Kwekhwalithi Nokuhlolwa

1. Ubuchwepheshe Bokuqapha Ku-inthanethi

• Faka ama-residual gas analyzers (RGA) ukuze uqaphe ingcindezi engaphelele ye-oxygen ngesikhathi sangempela
• Sebenzisa izinzwa ze-oxygen ukulawula okuqukethwe kwe-oxygen kumagesi avikelayo
• Sebenzisa i-infrared spectroscopy ukuhlonza iziqongo zokumuncwa kwezimpawu zezibopho ze-Se-O

2. Ukuhlaziywa Komkhiqizo Oqediwe

• Sebenzisa indlela yokumunca igesi engasebenzisi i-infrared ukuze uthole okuqukethwe yi-oxygen
• I-Secondary ion mass spectrometry (SIMS) ukuhlaziya ukusatshalaliswa komoya-mpilo
• I-X-ray photoelectron spectroscopy (XPS) ukuthola izimo zamakhemikhali angaphezulu

Ngezinyathelo eziphelele ezichazwe ngenhla, okuqukethwe komoya-mpilo kungalawulwa ngaphansi kwe-1 ppm ngesikhathi sokuhlanzwa kwe-selenium nge-vacuum distillation, okuhlangabezana nezidingo zokusetshenziswa kwe-selenium ehlanzekile kakhulu. Ekukhiqizweni kwangempela, amapharamitha enqubo kufanele alungiselelwe ngokusekelwe ezimweni zemishini kanye nezidingo zomkhiqizo, futhi kufanele kusungulwe uhlelo lokulawula ikhwalithi oluqinile.