Selenium, a matsayin muhimmin abu mai mahimmanci na semiconductor da albarkatun masana'antu, yana da aikin sa kai tsaye ya shafi tsarkinsa. A lokacin aikin tsarkakewa na vacuum distillation, iskar oxygen na ɗaya daga cikin manyan abubuwan da ke tasiri ga tsabtar selenium. Wannan labarin yana ba da cikakken bayani game da hanyoyi da dabaru daban-daban don rage abun ciki na oxygen yayin tsarkakewar selenium ta hanyar distillation.

I. Rage Abun Oxygen a Matsayin Magani na Raw Material Preatment

1. Tsarkakewar Raw Kayayyakin Farko

Raw selenium yawanci yana ƙunshe da datti iri-iri, gami da oxides. Kafin shigar da tsarin distillation, ya kamata a yi amfani da hanyoyin tsaftace sinadarai don cire oxides na saman. Maganin tsaftacewa da aka saba amfani da su sun haɗa da:

• Maganin hydrochloric acid (5-10% maida hankali): Yana narkar da oxides yadda ya kamata kamar SeO₂
• Ethanol ko acetone: Ana amfani dashi don cire gurɓataccen ƙwayar cuta
• Ruwan da aka cire: Rinses da yawa don cire ragowar acid

Bayan tsaftacewa, ya kamata a yi bushewa a ƙarƙashin iskar gas mara amfani (misali, Ar ko N₂) yanayi don hana sake yin iskar oxygen.

2. Kafin Rage Maganin Raw Materials

Rage jiyya na albarkatun ƙasa kafin cirewar iska na iya rage yawan iskar oxygen:

• Ragewar hydrogen: Gabatar da hydrogen mai tsabta (tsarki ≥99.999%) a 200-300 ° C don rage SeO₂ zuwa selenium na farko.
• Ragewar Carbothermal: Haɗa albarkatun kasa na selenium tare da foda mai tsabta mai tsabta da zafi zuwa 400-500 ° C a ƙarƙashin injin motsa jiki ko yanayi mara kyau, yana haifar da amsawar C + SeO₂ → Se + CO₂
• Rage Sulfide: Gases irin su H₂S na iya rage selenium oxides a ƙananan yanayin zafi

II. Zane da Inganta Ayyuka na Tsarin Distillation na Vacuum

1. Zabi da Tsarin Tsarin Matsala

Mahalli mai girma yana da mahimmanci don rage abun ciki na oxygen:

• Yi amfani da famfon watsawa + haɗin famfo na inji, tare da matuƙar injin da zai kai aƙalla 10⁻ Pa
• Ya kamata a sanya tsarin tare da tarkon sanyi don hana yaduwar tururin mai
• Duk hanyoyin haɗin gwiwa yakamata suyi amfani da hatimin ƙarfe don gujewa fitar da iskar gas daga hatimin roba
• Ya kamata tsarin ya sha isassun gasa-fita (200-250 ° C, 12-24 hours)

2. Daidaitaccen Gudanar da Zazzaɓin Distillation da Matsi

Haɗin madaidaicin tsarin tsari:

• Distillation zafin jiki: Sarrafa a cikin kewayon 220-280C (kasa da selenium ta tafasar batu na 685°C)
• Matsin tsarin: Tsayawa tsakanin 1-10 Pa
• Yawan dumama: 5-10 ° C / min don kauce wa tashin hankali da tashin hankali
• Yanayin zafin jiki na yanki: Ana kiyaye shi a 50-80 ° C don tabbatar da cikakken iskar selenium

3. Fasaha Distillation Multi-Stage

Distillation Multi-mataki na iya ci gaba da rage oxygen abun ciki:

• Mataki na farko: M distillation don kawar da mafi yawan ƙazanta masu canzawa
• Mataki na biyu: Madaidaicin sarrafa zafin jiki don tattara babban juzu'i
• Mataki na uku: Ƙananan zafin jiki, jinkirin distillation don samun samfur mai tsabta
  Za'a iya amfani da yanayin zafi daban-daban tsakanin matakai don matsewar juzu'i

III. Matakan Tsarukan Taimako

1. Fasahar Kariyar Gas Inert

Ko da yake aiki a ƙarƙashin injin, gabatarwar da ta dace na iskar gas mai tsabta mai tsabta yana taimakawa rage abun ciki na oxygen:

• Bayan fitar da tsarin, cika da argon mai tsabta (tsarki ≥99.9995%) zuwa 1000 Pa
• Yi amfani da kariyar kwararar gas mai ƙarfi, ci gaba da gabatar da ƙaramin adadin argon (10-20 sccm)
• Shigar da masu tsabtace iskar gas mai inganci a mashigar iskar gas don cire ragowar iskar oxygen da danshi

2. Ƙara Oxygen Scavengers

Ƙara abubuwan da suka dace na iskar oxygen zuwa albarkatun ƙasa na iya rage yawan iskar oxygen yadda ya kamata:

• Karfe na Magnesium: Ƙarfin ƙarfi don oxygen, yana samar da MgO
• Aluminum foda: Zai iya cire oxygen da sulfur lokaci guda
• Rare ƙasa karafa: Irin su Y, La, da dai sauransu, tare da kyakkyawan sakamako cire oxygen
  Yawan iskar oxygen shine yawanci 0.1-0.5 wt% na albarkatun kasa; yawan adadin zai iya shafar tsabtar selenium

3. Fasahar Filtration ta Narke

Tace narkakkar selenium kafin distillation:

• Yi amfani da ma'adini ko matatun yumbu tare da girman pore na 1-5 μm
• Sarrafa zafin tacewa a 220-250 ° C
• Zai iya cire tsayayyen barbashi oxide
• Ya kamata a riga an share matattara a ƙarƙashin babban injin

IV. Bayan Jiyya da Ajiya

1. Tarin Samfura da Gudanarwa

• Yakamata a ƙera mai tara na'urar a matsayin tsarin da za'a iya cirewa don sauƙin dawo da kayan a cikin yanayin da ba shi da aiki.
• Ya kamata a tattara ingots selenium da aka tattara a cikin akwatin safar hannu na argon
• Ana iya yin etching saman idan ya cancanta don cire yuwuwar yadudduka oxide

2. Kula da Yanayin Ajiye

• Ya kamata a kiyaye muhallin ajiya a bushe (madaidaicin raɓa ≤-60°C)
• Yi amfani da marufi da aka hatimi mai Layer biyu cike da iskar gas mai tsafta mai tsafta
• Shawarar zazzabin ajiya ƙasa da 20°C
• Guji bayyanar haske don hana halayen oxidation na photocatalytic

V. Ingancin Kulawa da Gwaji

1. Fasahar Sa Ido ta Kan layi

• Shigar da ragowar gas analyzers (RGA) don saka idanu da matsa lamba na ɓangaren oxygen a cikin ainihin lokaci
• Yi amfani da firikwensin oxygen don sarrafa abun ciki na oxygen a cikin iskar kariya
• Yi amfani da infrared spectroscopy don gano halayen kololuwar abubuwan sha na Se-O

2. Ƙarshen Binciken Samfur

• Yi amfani da inert gas fusion-infrared hanyar sha don tantance abun cikin oxygen
• Na biyu ion mass spectrometry (SIMS) don nazarin rarraba oxygen
• X-ray photoelectron spectroscopy (XPS) don gano jihohin sinadarai na saman

Ta hanyar ingantattun matakan da aka bayyana a sama, ana iya sarrafa abun ciki na oxygen a ƙasa da 1 ppm yayin tsaftacewar tsabtace selenium, biyan buƙatun don aikace-aikacen selenium mai tsabta. A cikin ainihin samarwa, ya kamata a inganta sigogin tsari bisa ga yanayin kayan aiki da buƙatun samfur, kuma ya kamata a kafa tsarin kula da ingancin inganci.