Ukuveliswa kwe-6N (≥99.9999% ukucoceka) i-sulfure ye-ultra-high-purity idinga i-distillation ye-multi-stage, i-adsorption enzulu, kunye ne-ultra-clean filtration ukuphelisa isinyithi, ukungcola kwezinto eziphilayo, kunye ne-particulates. Apha ngezantsi kukho inkqubo yomgangatho wemizi-mveliso edibanisa ivacuum distillation, ukucocwa okuncediswa yimicrowave, kunye nobuchwepheshe obuchanekileyo emva konyango.
I. Ukunyangwa kweMpathi ekrwada kunye nokususwa kokungcola
1. Ukukhethwa kweMathiriyeli ekrwada kunye nokuNyangwa kwangaphambili
- ...Iimfuno: Ukuhlanjululwa kwesulfure yokuqala ≥99.9% (ibakala le-3N), ukungcola kwetsimbi iyonke ≤500 ppm, umxholo wekhabhoni ophilayo ≤0.1%.
- ...Ukunyibilika okuNcedayo kwiMicrowave:
Isulfure ekrwada ilungiswa kwireactor yemicrowave (2.45 GHz frequency, 10–15 kW power) ku-140–150°C. I-Microwave-induced dipole rotation iqinisekisa ukunyibilika ngokukhawuleza ngelixa ukubola kwezinto ezingcolileyo ze-organic (umzekelo, iikhompawundi zetar). Ixesha lokunyibilikisa: imizuzu engama-30-45; ubunzulu bokungena kwi-microwave: 10-15 cm - ...Ukuhlamba Amanzi adiyinisiweyo:
Isulfure enyibilikisiweyo ixutywe namanzi adibeneyo (i-resistivity ≥18 MΩ · cm) kwi-1: 0.3 mass ratio kwi-reactor evuselelweyo (120 ° C, i-2 bar pressure) ngeyure ye-1 ukususa iityuwa ezinyibilikayo zamanzi (umzekelo, i-ammonium sulfate, i-sodium chloride). Isigaba samanzi sichithwa kwaye sisetyenziswe kwakhona kwimijikelezo ye-2-3 kude kube yi-conductivity ≤5 μS / cm.
2. I-Adsorption enezigaba ezininzi kunye noHlulo
- ...I-Diatomaceous Earth / iActed Carbon Adsorption:
Umhlaba we-Diatomaceous (0.5-1%) kunye nekhabhoni esebenzayo (0.2-0.5%) yongezwa kwisulfure etyhidiweyo phantsi kokhuseleko lwe-nitrogen (130 ° C, i-2-yure evuselelayo) ukubhengeza ii-complexes zetsimbi kunye ne-organics eseleyo. - ...UHluzo oluchanekileyo:
Ukuhluzwa kwamanqanaba amabini usebenzisa i-titanium sintered filters (0.1 μm ubungakanani bepore) kwi-≤0.5 MPa yoxinzelelo lwenkqubo. I-post-filtration ye-particulate count: ≤10 iincinci / L (ubukhulu> 0.5 μm).
II. Inkqubo ye-Multi-Stage Vacuum Distillation
1. I-Distillation yokuqala (ukususwa kokungcola kwesinyithi).
- ...Izixhobo: Ikholomu ye-quartz ecocekileyo ye-distillation ene-316L yensimbi engenasici epakishweyo (≥15 iipleyiti zethiyori), i-vacuum ≤1 kPa.
- ...Iiparamitha zokuSebenza:
- ...Ubushushu bokutya.
- ...Umlinganiselo weReflux: 5:1–8:1; ikholamu ephezulu yokutshintsha kweqondo lobushushu ≤±0.5°C.
- ...Imveliso: Ukucoceka kwesulfure econsisiweyo ≥99.99% (ibakala le-4N), ubumdaka bubonke besinyithi (Fe, Cu, Ni) ≤1 ppm.
2. I-Distillation yeSekondari yeMolekyuli (Ukususwa koBumdaka obuphilayo).
- ...Izixhobo: Umzila omfutshane we-molecular distiller kunye ne-10-20 mm ye-evaporation-condensation gap, i-evaporation ye-300-320 ° C, i-vacuum ≤0.1 Pa.
- ...Ukwahlula Ukungcola:
Izinto eziphilayo ezibilayo ezisezantsi (umzekelo, i-thioethers, i-thiophene) zifakwe ngumphunga kwaye zikhutshwe, ngelixa ukungcola okuphezulu (umzekelo, i-polyaromatics) kuhlala kwiintsalela ngenxa yomahluko kwi-molecular free path. - ...Imveliso: Ucoceko lwesulfure ≥99.999% (ibakala le-5N), i-organic carbon ≤0.001%, ireyithi yentsalela <0.3%.
3. Ukusulungekiswa koMmandla weMfundo ePhakamileyo (Ukuzuza ubunyulu be-6N).
- ...Izixhobo: Isisulungesi sezowuni ethe tyaba enolawulo lweqondo lobushushu lezowuni ezininzi (±0.1°C), isantya sohambo lwezowuni 1–3 mm/h.
- ...Ukwahlulahlula:
Ukusebenzisa i-coefficients yokwahlula (K=Csolid/CliquidK=Cqinile/Culwelo), indawo engama-20–30 idlula isinyithi esigxininisekileyo (Njengokuba, Sb) ekugqibeleni ingot. I-10-15% yokugqibela ye-ingot yesulfure ilahlwa.
III. Emva koNyango kunye noCwangciso oluPhezulu lokwenziwa
1. Ukutsalwa kwe-Solvent ye-Ultra-Pure
- ...Ukutsalwa kwe-Ether/Carbon Tetrachloride:
Isulfure ixutywe ne-ether ye-chromatographic-grade (1: 0.5 umthamo wevolumu) phantsi koncedo lwe-ultrasonic (40 kHz, 40 ° C) imizuzu engama-30 ukususa umkhondo we-polar organics. - ...UkuBuyiselwa kweNyibiliko:
I-adsorption ye-molecular sieve kunye ne-vacuum distillation inciphisa iintsalela ze-solvent ukuya kwi-≤0.1 ppm.
2. I-Ultrafiltration kunye ne-Ion Exchange
- ...PTFE Membrane Ultrafiltration:
Isulfure etyhidiweyo ihluzwa nge-0.02 μm PTFE membranes kwi-160-180 ° C kunye ne-≤0.2 MPa uxinzelelo. - ...Ion Exchange Resins:
I-Chelating resins (umzekelo, i-Amberlite IRC-748) isusa iiyoni zentsimbi ze-ppb (Cu²⁺, Fe³⁺) kwi-1–2 BV/h amazinga okuhamba.
3. Ukwenziwa kokuSingqongileyo okuCoceke Kakhulu
- ...I-Atomization yegesi engasebenziyo:
Kwigumbi elicocekileyo leKlasi le-10, i-sulfure etyhidiweyo i-atomized nitrogen (0.8-1.2 MPa uxinzelelo) kwi-0.5-1 mm i-spherical granules (umswakama <0.001%). - ...Ukupakishwa kweVacuum:
Imveliso yokugqibela i-vacuum-itywinwe kwifilimu edibeneyo ye-aluminium phantsi kwe-ultra-pure argon (≥99.9999% ubumsulwa) ukukhusela i-oxidation.
IV. Iiparamitha zeNkqubo engundoqo
Inqanaba lenkqubo | Iqondo lobushushu (°C). | Uxinzelelo | Ixesha/Isantya | Isixhobo esingundoqo |
Ukunyibilika kweMicrowave | 140–150 | I-Ambient | 30–45 imiz | Microwave Reactor |
Ukuhlamba Amanzi adiyinisiweyo | 120 | 2 ibha | 1 iyure/umjikelo | I-Reactor evuselelweyo |
I-Distillation yeMolekyuli | 300–320 | ≤0.1 Pa | Ngokuqhubekayo | Indlela emfutshane yeMolekyuli Distiller |
Ukusulungekiswa kwendawo | 115–120 | I-Ambient | 1–3 mm/h | Isisulungekisi soMmandla othe tye |
PTFE Ultrafiltration | 160–180 | ≤0.2 MPa | 1–2 m³/h ukuhambahamba | Isihluzi soBubushushu obuphezulu |
Nitrogen Atomization | 160–180 | 0.8–1.2 MPa | 0.5-1 mm iigranules | Inqaba yeAtomization |
V. Ulawulo lomgangatho kunye noVavanyo
- ...Ukulandelela Uhlalutyo Lokungacoceki:
- ...I-GD-MS (i-Glow Discharge Mass Spectrometry): Ibona iintsimbi ku-≤0.01 ppb.
- ...I-TOC Analyzer: Ilinganisa i-organic carbon ≤0.001 ppm.
- ...Ulawulo lobungakanani beNcam:
I-Laser diffraction (i-Mastersizer 3000) iqinisekisa ukutenxa kwe-D50 ≤±0.05 mm. - ...Ukucoceka koMphezulu:
I-XPS (i-X-reyi I-Photoelectron Spectroscopy) iqinisekisa ubukhulu be-oksidi yomphezulu ≤1 nm .
VI. Ukhuseleko kunye noYilo lokusiNgqongileyo
- ...UThintelo lokuqhushumba:
Izixhobo zokukhangela amadangatye e-infrared kunye neenkqubo zokukhukula kwe-nitrogen zigcina amanqanaba e-oxygen <3% - ...Ulawulo lokukhupha:
- ...Iigesi ze-Acid: Ukukhuhla kwe-NaOH enamanqanaba amabini (20% + 10%) kususa ≥99.9% H₂S/SO₂.
- ...IiVOCs: I-rotor ye-Zeolite + RTO (850°C) yehlisa ii-non-methane hydrocarbons ukuya ku-≤10 mg/m³.
- ...Inkunkuma yokurisayikilisha:
Ukunciphisa ubushushu obuphezulu (1200 ° C) kubuyisela iintsimbi; umxholo wesulfure oshiyekileyo <0.1%.
VII. I-Techno-Economic Metrics
- ...Ukusetyenziswa kwamandlaUmbane: 800–1200 kWh kunye neetoni ezi-2–3 zomphunga ngetoni ye-6N yesulfure.
- ...Yima kancinci: Ukubuyisela isulfure ≥85%, ireyithi yentsalela <1.5%.
- ...Iindleko: Iindleko zemveliso ~120,000–180,000 CNY/toni; ixabiso lemarike 250,000–350,000 CNY/toni (ibakala semiconductor) .
Le nkqubo ivelisa i-6N isulfure ye-photoresists ye-semiconductor, i-III-V ye-compound substrates, kunye nezinye izicelo eziphambili. Ukubeka iliso ngexesha langempela (umzekelo, uhlalutyo olusisiseko se-LIBS) kunye ne-ISO Class 1 yokucoceka kwegumbi lokulinganisa iqinisekisa umgangatho ongaguqukiyo.
Imibhalo esemazantsi
- Isalathiso sesi-2: ImiGangatho yokuCocwa kweSulfur yoShishino
- Isalathiso sesi-3: Ubuchwephesha obukwinqanaba eliphezulu lobuNjineli boBunjineli beMichiza
- Isalathiso sesi-6: INcwadana yoLungiso lweMpahla eZisulungekileyo
- Isalathiso 8: IiProtocol zeMveliso yeMichiza yeSemiconductor-Grade
- Isalathiso sesi-5: Ukuphuculwa kweVacuum Distillation
Ixesha lokuposa: Apr-02-2025