Ukukhiqizwa kwe-6N (≥99.9999% ubumsulwa) isibabule esihlanzekile kakhulu sidinga ukucwiliswa kwezigaba eziningi, ukumuncwa okujulile, kanye nokuhlunga okuhlanzekile kakhulu ukuze kususwe izinsimbi ezincane, ukungcola okungokwemvelo, kanye nezinhlayiya. Ngezansi kunenqubo yezimboni ehlanganisa ukucwiliswa kwe-vacuum, ukuhlanzwa okusiza nge-microwave, kanye nobuchwepheshe obunembile ngemva kokwelashwa.
I. Ukwelashwa Kwangaphambi Kwezinto Ezingavuthiwe kanye Nokususwa Kokungcola
1. Ukukhethwa Kwezinto Ezingavuthiwe Nokwelashwa Kwangaphambi Kokwelashwa
- Izidingo: Ubumsulwa besibabule bokuqala ≥99.9% (ibanga le-3N), ukungcola kwensimbi okuphelele ≤500 ppm, okuqukethwe kwekhabhoni ephilayo ≤0.1%.
- Ukuncibilika Okusizwa Yi-Microwave:
I-sulfur engahluziwe icutshungulwa ku-reactor ye-microwave (imvamisa engu-2.45 GHz, amandla angu-10-15 kW) ku-140-150°C. Ukujikeleza kwe-dipole okubangelwa yi-microwave kuqinisekisa ukuncibilika okusheshayo ngenkathi kubola ukungcola okungokwemvelo (isb., ama-compounds e-tar). Isikhathi sokuncibilika: imizuzu engama-30-45; ukujula kokungena kwe-microwave: 10-15 cm - Ukugeza Amanzi Okungaxutshwanga:
I-sulfur encibilikisiwe ixutshwa namanzi acwengekile (ukumelana ≥18 MΩ·cm) ngesilinganiso esingu-1:0.3 sobuningi ku-reactor evuselelwe (120°C, ingcindezi yama-bar ama-2) ihora eli-1 ukuze kususwe usawoti oncibilikayo emanzini (isb., i-ammonium sulfate, i-sodium chloride). Isigaba samanzi siyasuswa futhi sisetshenziswe kabusha imijikelezo engu-2-3 kuze kube yilapho ugesi ufinyelela ku-≤5 μS/cm.
2. Ukumuncwa kanye nokuhlunga kwezigaba eziningi
- Umhlaba we-Diatomaceous/Ukumuncwa kwe-Carbon Esebenzayo:
I-diatomaceous earth (0.5–1%) kanye ne-activated carbon (0.2–0.5%) kungezwa ku-sulfur encibilikisiwe ngaphansi kwesivikelo se-nitrogen (130°C, ukuxubha amahora ama-2) ukuze kumunce izinsimbi zensimbi kanye nezinto eziphilayo ezisele. - Ukuhlunga Okunembile Kakhulu:
Ukuhlunga okunezigaba ezimbili kusetshenziswa izihlungi ze-titanium sintered (usayizi wembobo engu-0.1 μm) kungcindezi yesistimu engu-≤0.5 MPa. Inani lezinhlayiya ngemuva kokuhlunga: ≤10 izinhlayiya/L (usayizi >0.5 μm).
II. Inqubo Yokucwilisa I-Vacuum Enezigaba Eziningi
1. Ukuhluzwa Okuyinhloko (Ukususwa Kokungcola Kwensimbi)
- Imishini: Ikholomu yokucwilisa ye-quartz emsulwa kakhulu enokupakisha okuhlelekile kwensimbi engagqwali okungu-316L (≥amapuleti ayi-15 e-theory), i-vacuum cleaner ≤1 kPa.
- Amapharamitha Okusebenza:
- Izinga Lokushisa Lokuphakelayo: 250–280°C (isibabule siyabila ku-444.6°C ngaphansi kwengcindezi ye-ambient; i-vacuum inciphisa iphuzu lokubila libe ngu-260–300°C).
- Isilinganiso se-Reflux: 5:1–8:1; ukushintshashintsha kwezinga lokushisa eliphezulu kwekholomu ≤±0.5°C.
- Umkhiqizo: Ubumsulwa besulfure obujiyile ≥99.99% (ibanga le-4N), ukungcola okuphelele kwensimbi (i-Fe, i-Cu, i-Ni) ≤1 ppm.
2. Ukuhluzwa Kwesibili Kwama-Molecular (Ukususwa Kokungcola Kwemvelo)
- Imishini: I-distiller yama-molecule ehamba ngendlela emfushane enegebe lokuhwamuka-ukujiya elingu-10-20 mm, izinga lokushisa lokuhwamuka lingu-300–320°C, i-vacuum ≤0.1 Pa.
- Ukuhlukaniswa Kokungcola:
Izinto eziphilayo ezibila kancane (isb., ama-thioether, ama-thiophene) ziyashiswa bese zikhishwa, kuyilapho ukungcola okubilayo kakhulu (isb., ama-polyaromatics) kuhlala ezinsaleleni ngenxa yokwehluka kwendlela yamahhala yama-molecule. - Umkhiqizo: Ubumsulwa besibabule ≥99.999% (ibanga le-5N), ikhabhoni ephilayo ≤0.001%, izinga lezinsalela <0.3%.
3. Ukucwengisiswa Kwendawo Ephakeme (Ukufeza Ubumsulwa be-6N)
- Imishini: Isihlungi sendawo evundlile esinokulawula izinga lokushisa lezindawo eziningi (± 0.1°C), isivinini sokuhamba sendawo singu-1–3 mm/h.
- Ukuhlukaniswa:
Ukusebenzisa ama-coefficient okuhlukanisa (K=Csolid/CliquidK=Cokuqinile/Cuketshezi), indawo engu-20–30 idlula izinsimbi ezigxilile (As, Sb) ekugcineni kwe-ingot. I-10–15% yokugcina ye-ingot yesulfure iyalahlwa.
III. Ukwakhiwa Kwangemva Kokwelashwa Nokuhlanza Kakhulu
1. Ukukhishwa kwe-Ultra-Pure Solvent
- Ukukhishwa kwe-Ether/Carbon Tetrachloride:
I-sulfur ixutshwa ne-ether ye-chromatographic-grade (isilinganiso sevolumu esingu-1:0.5) ngaphansi kosizo lwe-ultrasonic (40 kHz, 40°C) imizuzu engama-30 ukususa izinto eziphilayo ezi-polar ezilandelanayo. - Ukubuyiswa Kwesisombululo:
Ukumuncwa kwesihlungo sama-molecular kanye nokuhluzwa kwe-vacuum kunciphisa izinsalela ze-solvent zibe yi-≤0.1 ppm.
2. I-Ultrafiltration kanye ne-Ion Exchange
- Ukuhlunga kwe-PTFE Membrane Ultrafiltration:
Isibabule esincibilikisiwe sihlungwa ngama-membrane e-PTFE angu-0.02 μm ku-160–180°C kanye nomfutho we-≤0.2 MPa. - Ama-Resins Okushintshana Nge-Ion:
Ama-resin e-Chelating (isb., i-Amberlite IRC-748) asusa ama-ion ensimbi asezingeni le-ppb (Cu²⁺, Fe³⁺) ngamanani okugeleza kwe-1–2 BV/h.
3. Ukwakhiwa Kwendawo Ehlanzekile Kakhulu
- I-Inert Gas Atomization:
Egumbini lokuhlanza le-Class 10, isibabule esincibilikisiwe sihlanganiswa ne-nitrogen (umfutho we-0.8–1.2 MPa) sibe yizinhlayiya eziyindilinga ezingu-0.5–1 mm (umswakama <0.001%). - Ukupakisha i-Vacuum:
Umkhiqizo wokugcina uvalwa nge-vacuum ngefilimu ye-aluminium composite ngaphansi kwe-argon emsulwa kakhulu (≥99.9999% ubumsulwa) ukuvimbela i-oxidation.
IV. Amapharamitha Enqubo Eyinhloko
| Isigaba Senqubo | Izinga lokushisa (°C) | Ingcindezi | Isikhathi/Isivinini | Imishini Eyinhloko |
| Ukuncibilika kwe-Microwave | 140–150 | I-Ambient | 30–45 amaminithi | I-Microwave Reactor |
| Ukugeza Amanzi Okungaxutshwanga | 120 | Ibha emi-2 | Ihora eli-1/umjikelezo | I-Reactor Eshukunyisiwe |
| Ukuhluzwa Kwama-Molecular | 300–320 | ≤0.1 Pa | Okuqhubekayo | I-Distiller Yamamolekyuli Endlela Emfushane |
| Ukucwengisisa Indawo | 115–120 | I-Ambient | 1–3 mm/h | Isihlungi Sendawo Evundlile |
| Ukuhlunga kwe-PTFE Ultra | 160–180 | ≤0.2 MPa | Ukugeleza okungu-1–2 m³/h | Isihlungi Sokushisa Okuphezulu |
| Ukwenziwa kwe-nitrogen | 160–180 | 0.8–1.2 MPa | Ama-granules angu-0.5–1 mm | Umbhoshongo Wokwenza I-Atomization |
V. Ukulawulwa Kwekhwalithi Nokuhlolwa
- Ukuhlaziywa Kokungcola Kokulandelela:
- I-GD-MS (i-Glow Discharge Mass Spectrometry): Ithola izinsimbi ku-≤0.01 ppb.
- Isihlaziyi se-TOC: Kukala ikhabhoni ephilayo ≤0.001 ppm.
- Ukulawula Usayizi Wezinhlayiyana:
I-laser diffraction (Mastersizer 3000) iqinisekisa ukuphambuka kwe-D50 ≤±0.05 mm. - Ukuhlanzeka Komphezulu:
I-XPS (i-X-ray Photoelectron Spectroscopy) iqinisekisa ukujiya kwe-surface oxide ≤1 nm.
VI. Umklamo Wokuphepha Nokwemvelo
- Ukuvimbela Ukuqhuma:
Izitholi zomlilo ze-infrared kanye nezinhlelo zezikhukhula ze-nitrogen zigcina amazinga e-oxygen <3% - Ukulawulwa Kokukhishwa Kwegesi:
- Amagesi e-asidi: Ukuhlikihla i-NaOH okunezigaba ezimbili (20% + 10%) kususa okungu-≥99.9% H₂S/SO₂.
- Ama-VOCI-Zeolite rotor + RTO (850°C) yehlisa ama-hydrocarbon angewona ama-methane abe yi-≤10 mg/m³.
- Ukuphinda Kusetshenziswe Imfucuza:
Ukunciphisa izinga lokushisa eliphezulu (1200°C) kubuyisa izinsimbi; okuqukethwe kwe-sulfur okusele <0.1%.
VII. Amamethrikhi Obuchwepheshe Nomnotho
- Ukusetshenziswa Kwamandla: ugesi ongu-800–1200 kWh kanye nomusi wamathani angu-2–3 ngethani lesibabule esingu-6N.
- Veza: Ukubuyiselwa kwe-sulfur ≥85%, izinga lezinsalela <1.5%.
- IzindlekoIzindleko zokukhiqiza ~120,000–180,000 CNY/ton; intengo yemakethe 250,000–350,000 CNY/ton (ibanga le-semiconductor).
Le nqubo ikhiqiza i-sulfur engu-6N yama-photoresist e-semiconductor, ama-substrate e-III-V compound, kanye nezinye izinhlelo zokusebenza ezithuthukisiwe. Ukuqapha kwesikhathi sangempela (isb., ukuhlaziywa kwezinto eziyisisekelo ze-LIBS) kanye nokulinganiswa kwegumbi lokuhlanza le-ISO Class 1 kuqinisekisa ikhwalithi ehambisanayo.
Imibhalo yaphansi
- Inkomba 2: Izindinganiso Zokuhlanzwa Kwesibabule Sezimboni
- Inkomba 3: Amasu Okuhlunga Athuthukisiwe Kubunjiniyela Bamakhemikhali
- Inkomba 6: Incwadi Yokucubungula Izinto Ezihlanzekile Kakhulu
- Inkomba 8: Izinqubo Zokukhiqiza Amakhemikhali Ezingamaphesenti Ayisithupha
- Inkomba 5: Ukulungiswa Kokuhluzwa Kwe-Vacuum
Isikhathi sokuthunyelwe: Ephreli-02-2025