I-Selenium, njengempahla ebalulekile ye-semiconductor kanye nempahla eluhlaza yezimboni, inomthelela ekusebenzeni kwayo ngokuqondile ngenxa yobumsulwa bayo. Ngesikhathi senqubo yokuhlanza i-vacuum distillation, ukungcola komoyampilo kungenye yezinto eziyinhloko ezithonya ubumsulwa be-selenium. Lesi sihloko sinikeza ingxoxo enemininingwane yezindlela namasu ahlukahlukene okunciphisa okuqukethwe komoyampilo ngesikhathi sokuhlanzwa kwe-selenium nge-vacuum distillation.

I. Ukunciphisa Okuqukethwe Kweoksijini Esigabeni Sokwelashwa Kwangaphambi Kwezinto Ezingavuthiwe

1. Ukuhlanzwa Kokuqala Kwezinto Ezingavuthiwe

I-selenium eluhlaza ngokuvamile iqukethe ukungcola okuhlukahlukene, okuhlanganisa ama-oxide. Ngaphambi kokungena ohlelweni lwe-vacuum distillation, izindlela zokuhlanza amakhemikhali kufanele zisetshenziswe ukuze kukhishwe ama-oxide angaphezulu. Izixazululo ezivame ukusetshenziswa zokuhlanza zihlanganisa:

• Dilute hydrochloric acid solution (5-10% concentration): Incibilikisa ngempumelelo ama-oxide afana ne-SeO₂
• I-Ethanol noma i-acetone: Isetshenziselwa ukususa ukungcola okuphilayo
• Amanzi akhishwe nge-deionized: Amahlanzi amaningi ukuze asuse i-asidi esele

Ngemuva kokuhlanza, ukomiswa kufanele kwenziwe ngaphansi kwegesi engasebenzi (isb, i-Ar noma i-N₂) emkhathini ukuvimbela ukuphinda kufakwe i-oxidation.

2. Ukwelashwa Kwangaphambi Kokuncishiswa Kwezinto Ezingavuthiwe

Ukwehliswa kokwelashwa kwezinto ezingavuthiwe ngaphambi kokukhishwa kwe-vacuum kunganciphisa kakhulu okuqukethwe komoyampilo:

• Ukunciphisa i-Hydrogen: Yethula i-hydrogen ehlanzekile kakhulu (ukuhlanzeka ≥99.999%) ku-200-300 ° C ukunciphisa i-SeO₂ ku-elenium elemental
• Ukwehliswa kwe-Carbothermal: Hlanganisa i-selenium eluhlaza kanye ne-carbon powder ehlanzekile kakhulu kanye nokushisa ku-400-500 ° C ngaphansi kwe-vacuum noma umkhathi ongenayo, udale ukusabela kwe-C + SeO₂ → Se + CO₂
• Ukunciphisa i-sulfide: Amagesi afana ne-H₂S anganciphisa ama-selenium oxides emazingeni okushisa aphansi kakhulu

II. Ukuklama kanye Nokuthuthukiswa Kokusebenza Kohlelo Lokukhipha I-Vacuum Distillation

1. Ukukhethwa Nokucushwa Kwesistimu Yevacuum

Indawo enevacuum ephezulu ibalulekile ekwehliseni okuqukethwe komoyampilo:

• Sebenzisa iphampu yokusabalalisa + inhlanganisela yepompo yomshini, enevacuum yokugcina efinyelela okungenani ku-10⁻⁴ Pa
• Isistimu kufanele ifakwe isicupho esibandayo ukuvimbela ukusabalalisa emuva komhwamuko kawoyela
• Konke ukuxhumana kufanele kusebenzise izigxivizo zensimbi ukuze kugwenywe ukuphuma kogesi ezigxivizweni zenjoloba
• Isistimu kufanele ikhishwe ngokwanele yokubhaka-out (200-250 ° C, amahora angu-12-24)

2. Ukulawula Okunembayo Kwezinga Lokushisa Lokukhipha I-Distillation kanye Nokucindezela

Inhlanganisela yepharamitha yenqubo elungile:

• Izinga lokushisa lokukhipha isisu: Ilawulwa ngaphakathi kwebanga lika-220-280°C (ngaphansi kwendawo yokubilisa ye-selenium engu-685°C)
• Ingcindezi yesistimu: Igcinwe phakathi kuka-1-10 Pa
• Izinga lokushisa: 5-10°C/min ukuze kugwenywe ukuhwamuka okunodlame kanye nokuzilolonga
• Izinga lokushisa lendawo ye-Condensation: Igcinwe ku-50-80°C ukuze kuqinisekiswe ukufiphala okuphelele kwe-selenium

3. Multi-Stage Distillation Technology

I-multi-stage distillation inganciphisa kancane kancane okuqukethwe komoyampilo:

• Isigaba sokuqala: I-distillation engalungile ukususa ukungcola okuningi okuguquguqukayo
• Isigaba sesibili: Ukulawula izinga lokushisa okunembile ukuze kuqoqwe ingxenyenamba enkulu
• Isigaba sesithathu: Izinga lokushisa eliphansi, ukuphuza utshwala kancane ukuze uthole umkhiqizo ohlanzekile kakhulu
  Amazinga okushisa ahlukene e-condensation angasetshenziswa phakathi kwezigaba zokufingqa okuyingxenye

III. Izinyathelo Zenqubo Esizayo

1. I-Inert Gas Protection Technology

Nakuba isebenza ngaphansi kwe-vacuum, ukwethulwa okufanele kwegesi ye-inert ehlanzekile kakhulu kusiza ukunciphisa okuqukethwe komoyampilo:

• Ngemva kokukhipha isistimu, gcwalisa nge-argon ephezulu yokuhlanzeka (ukuhlanzeka ≥99.9995%) kuya ku-1000 Pa
• Sebenzisa ukuvikelwa kokugeleza kwegesi okuguquguqukayo, ngokuqhubekayo wethula inani elincane le-argon (10-20 sccm)
• Faka izihlanzi zegesi ezisebenza kahle kakhulu ezindaweni zokungena igesi ukuze ususe umoya-mpilo osele kanye nomswakama

2. Ukwengezwa Kwe-Oxygen Scavengers

Ukwengeza ama-scavenger afanele komoyampilo ezintweni ezingavuthiwe kunganciphisa ngempumelelo okuqukethwe komoyampilo:

• I-Magnesium metal: Ukuhlangana okunamandla kwe-oksijini, kwakha i-MgO
• I-aluminium powder: Ingasusa kanyekanye umoya-mpilo nesibabule
• Izinsimbi zomhlaba ezingavamile: Ezifana ne-Y, La, njll., ezinemiphumela emihle kakhulu yokususa umoya-mpilo
  Inani le-oxygen scavenger ngokuvamile liyi-0.1-0.5 wt% yezinto ezingavuthiwe; amanani eqile angathinta ubumsulwa be-selenium

3. I-Molten Filtration Technology

Ukuhlunga i-selenium encibilikisiwe ngaphambi kwe-distillation:

• Sebenzisa izihlungi ze-quartz noma ze-ceramic ezinosayizi wembotshana ongu-1-5 μm
• Lawula izinga lokushisa lokuhlunga ku-220-250°C
• Ingasusa izinhlayiya ze-oxide eqinile
• Izihlungi kufanele zikhishwe ngaphambili ngaphansi kwe-vacuum ephezulu

IV. Ngemuva Kokwelashwa kanye Nesitoreji

1. Ukuqoqwa Nokuphathwa Komkhiqizo

• Isiqoqi se-condenser kufanele sidizayinwe njengesakhiwo esikhiphekayo ukuze kube lula ukubuyiswa kwempahla endaweni engasebenzi
• Ama-selenium ingots aqoqiwe kufanele ahlanganiswe ebhokisini legilavu ​​ye-argon
• Ukufaka i-surface kungenziwa uma kunesidingo ukuze kukhishwe izendlalelo ze-oxide ezingaba khona

2. Ukulawula Isimo Sesitoreji

• Indawo yokugcina kufanele igcinwe yomile (iphuzu lamazolo ≤-60°C)
• Sebenzisa amaphakheji avaliwe anezendlalelo ezimbili agcwaliswe ngegesi ye-inert yokuhlanzeka okuphezulu
• Izinga lokushisa elinconyiwe lesitoreji ngaphansi kuka-20°C
• Gwema ukuchayeka ekukhanyeni ukuze uvimbele ukusabela kwe-photocatalytic oxidation

V. Ukulawula Ikhwalithi Nokuhlola

1. Online Monitoring Technology

• Faka izihlaziyi zegesi ezisele (RGA) ukuze uqaphe ukucindezela kwengxenye komoyampilo ngesikhathi sangempela
• Sebenzisa izinzwa zomoya-mpilo ukuze ulawule okuqukethwe komoyampilo kumagesi avikelayo
• Sebenzisa i-infrared spectroscopy ukuze uhlonze izici eziphakeme zokumunca zamabhondi e-Se-O

2. Ukuhlaziywa Kwemikhiqizo Eqediwe

• Sebenzisa indlela yokumunca i-inert gas fusion-infrared ukuze unqume okuqukethwe komoyampilo
• I-ion mass spectrometry (SIMS) yokuhlaziya ukusatshalaliswa komoyampilo
• I-X-ray photoelectron spectroscopy (XPS) ukuthola izimo zamakhemikhali ezingaphezulu

Ngezinyathelo ezibanzi ezichazwe ngenhla, okuqukethwe komoyampilo kungalawulwa ngaphansi kwe-1 ppm ngesikhathi sokuhlanzwa kwe-vacuum distillation ye-selenium, kuhlangatshezwana nezidingo zokusetshenziswa kwe-selenium yobumsulwa obukhulu. Ekukhiqizeni kwangempela, amapharamitha wenqubo kufanele athuthukiswe ngokusekelwe ezimweni zemishini kanye nezidingo zomkhiqizo, futhi kufanele kusungulwe uhlelo oluqinile lokulawula ikhwalithi.