Ukuveliswa kwe-6N (≥99.9999% yobumsulwa) i-sulfur ecocekileyo kakhulu ifuna i-distillation enezigaba ezininzi, i-deep adsorption, kunye ne-ultra-clean filtration ukuze kususwe ii-trace metals, ukungcola kwezinto eziphilayo, kunye nee-particles. Apha ngezantsi kukho inkqubo yobukhulu bemizi-mveliso edibanisa i-vacuum distillation, i-microwave-assisted cleansing, kunye netekhnoloji yokuchaneka emva konyango.
I. Unyango lwangaphambi kokusetyenziswa kwezinto eziluhlaza kunye nokususwa kokungcola
1. Ukukhethwa kwezinto eziluhlaza kunye nonyango lwangaphambi kwexesha
- Iimfuno: Ubumsulwa besalfure bokuqala ≥99.9% (udidi lwe-3N), ukungcola kwesinyithi okupheleleyo ≤500 ppm, umxholo wekhabhoni yendalo ≤0.1%.
- Ukunyibilika okuxhaswa yi-microwave:
I-sulfur ekrwada icutshungulwa kwi-reactor ye-microwave (i-frequency ye-2.45 GHz, amandla e-10–15 kW) kwi-140–150°C. Ukujikeleza kwe-dipole okubangelwa yi-microwave kuqinisekisa ukunyibilika ngokukhawuleza ngelixa kubola ukungcola okuphilayo (umz., iikhompawundi ze-tar). Ixesha lokunyibilika: imizuzu engama-30–45; ubunzulu bokungena kwi-microwave: 10–15 cm - Ukuhlamba Amanzi Angenazo I-ionized:
I-sulfur enyibilikisiweyo ixutywa namanzi anyibilikisiweyo (i-resistivity ≥18 MΩ·cm) kumlinganiselo we-1:0.3 mass kwi-reactor eshukunyisiweyo (120°C, uxinzelelo lwe-bar ezi-2) iyure e-1 ukususa iityuwa ezinyibilikayo emanzini (umz., i-ammonium sulfate, i-sodium chloride). Isigaba samanzi siyasuswa kwaye sisetyenziswe kwakhona kangangemijikelo emi-2-3 de kube yi-conductivity ≤5 μS/cm.
2. Ukufunxwa kunye nokuhluzwa kweZiteji ezininzi
- Umhlaba weDiatomaceous/Ukufunxwa kweKhabhoni eVuselelweyo:
Umhlaba we-diatomaceous (0.5–1%) kunye ne-activated carbon (0.2–0.5%) zongezwa kwi-sulfur enyibilikisiweyo phantsi kokhuseleko lwe-nitrogen (130°C, ukuxutywa iiyure ezi-2) ukuze zifunxe ii-complexes zesinyithi kunye nezinto eziphilayo ezisele. - Ukucoca Okuchanekileyo Kakhulu:
Ukucoca okunezigaba ezibini kusetyenziswa izihluzi ze-titanium sintered (ubungakanani be-pore ye-0.1 μm) kuxinzelelo lwenkqubo ye-≤0.5 MPa. Inani lamasuntswana emva kokucoca: ≤10 amasuntswana/L (ubukhulu >0.5 μm).
II. Inkqubo yokuCoca iVacuum eneZigaba ezininzi
1. Ukucoca okuPhambili (Ukususwa kokungcola kwesinyithi)
- IzixhoboIkholamu yokunyibilikisa i-quartz ecocekileyo kakhulu ene-316L stainless steel packing (≥15 theoretical plates), i-vacuum ≤1 kPa.
- Iiparameters zokusebenza:
- Ubushushu bokutya: 250–280°C (isulfur iyabila kwi-444.6°C phantsi koxinzelelo lwemozulu; i-vacuum inciphisa iqondo lokubila liye kwi-260–300°C).
- Umlinganiselo weReflux: 5:1–8:1; ukutshintshatshintsha kobushushu obuphezulu bekholamu ≤±0.5°C.
- Imveliso: Ubumsulwa besalfure edityanisiweyo ≥99.99% (umgangatho we-4N), ukungcola kwesinyithi okupheleleyo (i-Fe, i-Cu, i-Ni) ≤1 ppm.
2. Ukususwa kokungcola kweMolekyuli yesibini (Ukususwa kokungcola kwendalo)
- Izixhobo: Isixhobo sokucoca iimolekyuli esifutshane esinesithuba se-10–20 mm sokukhupha umphunga kunye nokufuma, ubushushu bokufuma bube yi-300–320°C, i-vacuum ≤0.1 Pa.
- Ukwahlukana Kobumdaka:
Izinto eziphilayo ezibila kancinci (umz., iithioethers, iithiophene) ziyaphehlwa kwaye zikhutshwe, ngelixa ukungcola okubilayo kakhulu (umz., iipolyaromatics) kuhlala kwiintsalela ngenxa yokwahluka kwendlela ekhululekileyo yeemolekyuli. - Imveliso: Ubumsulwa besalfure ≥99.999% (ibanga le-5N), ikhabhoni yendalo ≤0.001%, izinga lentsalela <0.3%.
3. Ukucocwa kweNdawo ePhakamileyo (Ukufezekisa ubunyulu be-6N)
- Izixhobo: Isicoci sendawo ethe tye esinolawulo lobushushu beendawo ezininzi (± 0.1°C), isantya sokuhamba sendawo yi-1–3 mm/h.
- Ukwahlulwahlulwa:
Ukusebenzisa ii-coefficients zokwahlulwahlulwa (K=Csolid/CliquidK=Ceqinileyo/Culwelo), indawo engama-20–30 idlula iimetali ezixineneyo (As, Sb) ekupheleni kwe-ingot. I-10–15% yokugqibela ye-ingot yesulfure iyalahlwa.
III. Ukwenziwa Emva Konyango kunye Nokucocwa Kakhulu
1. Ukukhupha iSolvent ecocekileyo kakhulu
- Ukukhupha i-Ether/Carbon Tetrachloride:
I-Sulfur ixutywa ne-ether ye-chromatographic-grade (1:0.5 volume ratio) phantsi koncedo lwe-ultrasonic (40 kHz, 40°C) imizuzu engama-30 ukususa izinto eziphilayo ezi-trace polar. - Ukubuyiselwa kweSolvent:
Ukufunxwa kwesihluzo semolekyuli kunye nokucocwa kwevacuum kunciphisa iintsalela zesinyibilikisi ukuya kwi-≤0.1 ppm.
2. I-Ultrafiltration kunye ne-Ion Exchange
- Ukucoca nge-PTFE Membrane Ultrafiltration:
I-sulfur enyibilikisiweyo ihluzwa ngee-membrane ze-PTFE ze-0.02 μm kwi-160–180°C kunye noxinzelelo lwe-≤0.2 MPa. - IiResins zoTshintshiselwano lweeIon:
Ii-resin ze-Chelating (umz., i-Amberlite IRC-748) zisusa ii-ion zesinyithi ezikwinqanaba le-ppb (Cu²⁺, Fe³⁺) kwizinga lokuhamba kwe-1–2 BV/h.
3. Ukwenziwa kweNdalo ecocekileyo kakhulu
- I-Atomization yeGesi engasebenziyo:
Kwigumbi lokucoca leKlasi le-10, i-sulfur enyibilikisiweyo ifakwa kwi-atom nge-nitrogen (uxinzelelo lwe-0.8–1.2 MPa) ukuya kwiigranules ezingqukuva ze-0.5–1 mm (ukufuma <0.001%). - Ukupakishwa kweVacuum:
Imveliso yokugqibela ivalwa nge-vacuum kwifilimu ye-aluminium composite phantsi kwe-argon ecocekileyo kakhulu (≥99.9999% ubumsulwa) ukuthintela i-oxidation.
IV. Iiparameter zeNkqubo ePhambili
| Inqanaba leNkqubo | Ubushushu (°C) | Uxinzelelo | Ixesha/Isantya | Izixhobo eziphambili |
| Ukunyibilika kweMicrowave | 140–150 | Indalo | imizuzu engama-30–45 | Isixhobo sokuphendula kwi-microwave |
| Ukuhlamba Amanzi Angenazo I-ionized | 120 | Ibha ezi-2 | Iyure e-1/umjikelo | I-Reactor evuselelayo |
| Ukucoca iimolekyuli | 300–320 | ≤0.1 Pa | Iqhubekeka | I-Distiller yeMolecular yeNdlela emfutshane |
| Ukucocwa kweNdawo | 115–120 | Indalo | 1–3 mm/h | Umcoci weNdawo ethe tye |
| Ukucoca nge-PTFE Ultra | 160–180 | ≤0.2 MPa | Ukuhamba kwe-1–2 m³/h | Isihluzi sobushushu obuphezulu |
| Ukwenziwa kweNitrogen | 160–180 | 0.8–1.2 MPa | Iigranule eziyi-0.5–1 mm | Inqaba yokwenziwa kwe-atomization |
V. Ulawulo loMgangatho kunye noVavanyo
- Uhlalutyo loBumdaka bokulandelela:
- I-GD-MS (i-Glow Discharge Mass Spectrometry): Ifumana iintsimbi kwi ≤0.01 ppb.
- Isihlalutyi seTOC: Ilinganisa i-carbon yendalo ≤0.001 ppm.
- Ulawulo lobungakanani beenxalenye:
I-laser diffraction (Mastersizer 3000) iqinisekisa ukuphambuka kwe-D50 ≤±0.05 mm. - Ucoceko Lomphezulu:
I-XPS (i-X-ray Photoelectron Spectroscopy) iqinisekisa ubukhulu be-oxide yomphezulu ≤1 nm.
VI. Uyilo loKhuseleko kunye nokusingqongileyo
- Ukuthintela Ukuqhuma:
Izixhobo zokubona ilangatye ezisebenzisa i-infrared kunye neenkqubo ze-nitrogen ezikhukulayo zigcina amanqanaba eoksijini <3% - Ulawulo lokukhupha ukungcola:
- Iigesi ze-asidi: Ukuhlafuna i-NaOH enamanqanaba amabini (20% + 10%) kususa i-≥99.9% H₂S/SO₂.
- IiVOCI-Zeolite rotor + RTO (850°C) inciphisa ii-hydrocarbons ezingezizo ze-methane ukuya kwi-≤10 mg/m³.
- Ukuphinda kusetyenziswe inkunkuma:
Ukunciphisa ubushushu obuphezulu (1200°C) kubuyisela iintsimbi; intsalela yesalfure ingaphantsi kwe-0.1%.
VII. IiMetriki zeTekhnoloji-yoQoqosho
- Ukusetyenziswa kwamandlaUmbane we-800–1200 kWh kunye neetoni ezi-2–3 zomphunga ngetoni nganye yesalfure ye-6N.
- Yima kancinci: Ukubuyiswa kwesalfure ≥85%, izinga lentsalela <1.5%.
- IxabisoIindleko zemveliso ~120,000–180,000 CNY/ton; ixabiso lemarike yi-250,000–350,000 CNY/ton (udidi lwe-semiconductor).
Le nkqubo ivelisa i-6N sulfur kwi-semiconductor photoresists, ii-III-V compound substrates, kunye nezinye izicelo eziphambili. Ukubeka esweni ngexesha langempela (umz., uhlalutyo lwezinto ze-LIBS) kunye nokulinganiswa kwegumbi lokucoca le-ISO Class 1 kuqinisekisa umgangatho ohambelanayo.
Imibhalo esemazantsi
- Isalathiso 2: Imigangatho yokuCoca iSulfur yoShishino
- Isalathiso 3: Iindlela zokucoca eziPhambili kwiNjineli yeKhemikhali
- Isalathiso 6: Incwadi Yokucwangciswa Kwezinto Ezicocekileyo Kakhulu
- Isalathiso 8: IiProtokholi zeMveliso yeeKhemikhali zeSemiconductor-Grade
- Isalathiso 5: Ukuphucula iVacuum Distillation
Ixesha leposi: Epreli-02-2025
