Kev tsim cov sulfur uas muaj 6N (≥99.9999% purity) uas muaj ultra-high-purity xav tau kev sib xyaw ua ke ntawm ntau theem, kev nqus dej tob, thiab kev lim dej kom huv si kom tshem tawm cov hlau tsis muaj zog, cov organic impurities, thiab cov khoom me me. Hauv qab no yog cov txheej txheem kev lag luam uas suav nrog kev sib xyaw ua ke ntawm lub tshuab nqus tsev, kev ntxuav los ntawm microwave, thiab cov thev naus laus zis tom qab kho kom raug.
I. Kev kho ua ntej ntawm cov khoom siv raw thiab kev tshem tawm cov khoom tsis huv
1. Kev Xaiv Khoom Siv Raw thiab Kev Kho Mob Ua Ntej
- Cov Kev CaiThawj qhov huv ntawm cov leej faj ≥99.9% (3N qib), tag nrho cov hlau tsis huv ≤500 ppm, cov ntsiab lus ntawm cov pa roj carbon organic ≤0.1%.
- Kev Pab Yaj Los Ntawm Microwave:
Cov sulfur nyoos raug ua tiav hauv lub tshuab hluav taws xob microwave (2.45 GHz zaus, 10–15 kW zog) ntawm 140–150 ° C. Kev tig dipole uas ua rau lub microwave ua rau yaj sai thaum rhuav tshem cov organic impurities (piv txwv li, cov tshuaj tar). Lub sijhawm yaj: 30–45 feeb; qhov tob ntawm microwave nkag mus: 10–15 cm - Kev Ntxuav Dej Deionized:
Cov sulfur uas yaj lawm yog sib xyaw nrog dej uas tsis muaj zog (resistivity ≥18 MΩ·cm) ntawm qhov sib piv ntawm 1:0.3 hauv lub tshuab ua kom sov (120°C, 2 bar siab) rau 1 teev kom tshem tawm cov ntsev uas yaj tau hauv dej (piv txwv li, ammonium sulfate, sodium chloride). Cov theem aqueous raug decanted thiab rov siv dua rau 2-3 lub voj voog kom txog thaum conductivity ≤5 μS/cm.
2. Kev nqus thiab lim dej ntau theem
- Lub Ntiaj Teb Diatomaceous / Cov Pa roj carbon uas ua kom muaj zog Adsorption:
Cov av diatomaceous (0.5–1%) thiab cov pa roj carbon activated (0.2–0.5%) raug ntxiv rau cov sulfur molten nyob rau hauv kev tiv thaiv nitrogen (130 ° C, 2-teev do) kom nqus cov hlau sib xyaw thiab cov organic seem. - Kev lim dej ultra-precision:
Kev lim dej ob theem siv cov lim dej titanium sintered (qhov loj ntawm 0.1 μm) ntawm qhov siab ntawm lub kaw lus ≤0.5 MPa. Cov khoom me me tom qab lim: ≤10 cov khoom me me/L (qhov loj >0.5 μm).
II. Txheej Txheem Distillation Nqus Tsev Ntau Theem
1. Kev Distillation Thawj Zaug (Kev Tshem Tawm Cov Hlau Tsis Muaj Peev Xwm)
- Cov khoom sivCov kem distillation quartz siab purity nrog 316L stainless hlau qauv packing (≥15 theoretical phaj), nqus tsev ≤1 kPa.
- Cov Kev Ntsuas Ua Haujlwm:
- Kub pub: 250–280 ° C (sulfur npau ntawm 444.6 ° C nyob rau hauv qhov siab ambient; nqus tsev txo qhov kub npau mus rau 260–300 ° C).
- Qhov piv ntawm Reflux: 5: 1–8: 1; qhov kub thiab txias sab saum toj ntawm kem hloov pauv ≤ ± 0.5 ° C.
- KhoomKev ntshiab ntawm cov sulfur uas tau sib xyaw ua ke ≥99.99% (qib 4N), tag nrho cov hlau tsis huv (Fe, Cu, Ni) ≤1 ppm.
2. Kev Sib Distillation Molecular Thib Ob (Kev Tshem Tawm Cov Khoom Uas Tsis Muaj Organic)
- Cov khoom siv: Lub tshuab distiller molecular luv luv nrog 10–20 hli qhov sib txawv ntawm evaporation-condensation, qhov kub ntawm evaporation 300–320 ° C, lub tshuab nqus tsev ≤0.1 Pa.
- Kev Sib Cais Impurity:
Cov organic uas kub tsawg (piv txwv li, thioethers, thiophene) raug ua pa thiab tshem tawm, thaum cov khoom tsis huv uas kub heev (piv txwv li, polyaromatics) tseem nyob hauv cov seem vim muaj qhov sib txawv ntawm txoj kev dawb molecular. - KhoomSulfur purity ≥99.999% (5N qib), organic carbon ≤0.001%, residue tus nqi <0.3%.
3. Kev Kho Dua Thaj Chaw Tertiary (Ua tiav 6N Purity)
- Cov khoom siv: Lub tshuab ua kom huv thaj tsam kab rov tav nrog kev tswj qhov kub ntau thaj tsam (± 0.1 ° C), qhov ceev ntawm thaj tsam mus ncig 1–3 hli / teev.
- Kev sib cais:
Siv cov coefficients sib cais (K = Csolid / Cliquid)K=Ckhov khoCkua), 20–30 cheeb tsam hla cov hlau concentrate (As, Sb) ntawm qhov kawg ntawm ingot. Qhov kawg 10–15% ntawm cov sulfur ingot raug pov tseg.
III. Tom Qab Kho Mob thiab Kev Tsim Kho Kom Huv Si
1. Ultra-Pure Solvent Extraction
- Kev rho tawm Ether/Carbon Tetrachloride:
Sulfur yog sib xyaw nrog chromatographic-qib ether (1: 0.5 ntim piv) nyob rau hauv ultrasonic kev pab (40 kHz, 40 ° C) rau 30 feeb kom tshem tawm cov kab mob polar organics. - Kev Rov Qab Los Ntawm Cov Tshuaj Solvent:
Kev nqus cov molecular sieve thiab kev distillation hauv lub tshuab nqus tsev txo cov kuab tshuaj seem rau ≤0.1 ppm.
2. Ultrafiltration thiab Ion Exchange
- PTFE Membrane Ultrafiltration:
Cov sulfur uas yaj lawm raug lim los ntawm 0.02 μm PTFE membranes ntawm 160–180°C thiab ≤0.2 MPa siab. - Cov Resins Hloov Ion:
Cov tshuaj chelating resins (piv txwv li, Amberlite IRC-748) tshem tawm cov hlau ions ppb (Cu²⁺, Fe³⁺) ntawm tus nqi ntws 1–2 BV/h.
3. Kev Tsim Ib puag ncig huv si heev
- Kev Ua Pa Roj Inert:
Hauv chav huv Class 10, cov sulfur uas yaj lawm raug atomized nrog nitrogen (0.8–1.2 MPa siab) rau hauv cov granules kheej kheej 0.5–1 hli (dej noo <0.001%). - Ntim Khoom Siv Nqus Tsev:
Cov khoom kawg yog nqus tsev kaw hauv cov zaj duab xis txhuas sib xyaw hauv qab argon ntshiab heev (≥99.9999% purity) kom tiv thaiv kev oxidation.
IV. Cov Txheej Txheem Tseem Ceeb
| Theem Txheej Txheem | Kub (°C) | Kev nyuaj siab | Lub Sijhawm / Ceev | Cov khoom siv tseem ceeb |
| Kev yaj hauv lub tshuab hluav taws xob microwave | 140–150 | Ib puag ncig | 30–45 feeb | Lub Tshuab Hluav Taws Xob Microwave |
| Kev Ntxuav Dej Deionized | 120 | 2 bar | 1 teev/lub voj voog | Cov Tshuaj Reactor Sib Xyaws |
| Kev Sib Tsoo Molecular | 300–320 | ≤0.1 Pa | Txuas ntxiv mus | Kev Siv Tshuaj Distiller Luv-Kev |
| Kev Ua Kom Zoo Dua Hauv Cheeb Tsam | 115–120 | Ib puag ncig | 1–3 hli/teev | Kab rov tav Zone Refiner |
| PTFE Ultrafiltration | 160–180 | ≤0.2 MPa | 1–2 m³/teev ntws | Lim Kub Siab |
| Kev Ua Pa Nitrogen | 160–180 | 0.8–1.2 MPa | Cov hmoov me me 0.5–1 hli | Lub Tsev Atomization |
V. Kev Tswj Xyuas Zoo thiab Kev Ntsuas
- Kev Tshawb Fawb Txog Kev Ua Phem Tsis Zoo:
- GD-MS (Kev Ntsuas Qhov Kub thiab Txias): Nrhiav tau cov hlau ntawm ≤0.01 ppb.
- Tus Tshuaj Xyuas TOCNtsuas cov pa roj carbon organic ≤0.001 ppm.
- Kev Tswj Qhov Loj ntawm Cov Khoom Me Me:
Laser diffraction (Mastersizer 3000) ua kom D50 deviation ≤±0.05 hli. - Kev Huv Si ntawm Qhov Chaw:
XPS (X-ray Photoelectron Spectroscopy) lees paub qhov tuab ntawm cov oxide saum npoo ≤1 nm.
VI. Kev Nyab Xeeb thiab Kev Tsim Kho Ib puag ncig
- Kev Tiv Thaiv Kev Tawg:
Cov cuab yeej ntes nplaim taws infrared thiab cov tshuab nitrogen flooding tswj cov pa oxygen <3% - Kev Tswj Xyuas Pa Tawm:
- Cov pa roj acidKev txhuam NaOH ob theem (20% + 10%) tshem tawm ≥99.9% H₂S/SO₂.
- Cov VOCs: Zeolite rotor + RTO (850°C) txo cov hydrocarbons uas tsis yog methane rau ≤10 mg/m³.
- Kev Siv Cov Khib Nyhiab Rov Qab:
Kev txo qhov kub siab (1200 ° C) rov qab tau cov hlau; cov ntsiab lus sulfur seem <0.1%.
VII. Cov Kev Ntsuas Txog Kev Lag Luam thiab Kev Siv Tshuab
- Kev Siv Hluav Taws Xob: 800–1200 kWh hluav taws xob thiab 2–3 tons ntawm cov pa rau ib tuj ntawm 6N sulfur.
- Cov qoob looKev rov qab los ntawm sulfur ≥85%, tus nqi seem <1.5%.
- Tus nqiTus nqi tsim khoom ~ 120,000–180,000 CNY / ton; tus nqi ua lag luam 250,000–350,000 CNY / ton (qib semiconductor).
Cov txheej txheem no tsim cov sulfur 6N rau cov photoresists semiconductor, III-V compound substrates, thiab lwm yam kev siv siab heev. Kev saib xyuas tiag tiag (piv txwv li, LIBS elemental analysis) thiab ISO Class 1 cleanroom calibration ua kom muaj qhov zoo sib xws.
Cov Lus Cim Hauv Qab
- Siv 2: Cov Qauv Kev Ntxuav Sulfur Hauv Kev Lag Luam
- Siv 3: Cov Txuj Ci Kev Lim Dej Siab Hauv Kev Tsim Kho Tshuaj
- Siv 6: Phau Ntawv Qhia Txog Kev Ua Cov Khoom Siv Uas Muaj Kev Ntshiab Siab
- Cov Lus Qhia 8: Cov Txheej Txheem Tsim Tshuaj Semiconductor-Grade
- Siv 5: Kev Txhim Kho Kev Siv Lub Tshuab Nqus Tsev
Lub sijhawm tshaj tawm: Plaub Hlis-02-2025
