I-7N Tellurium Crystal Growth and Purification

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I-7N Tellurium Crystal Growth and Purification

I-7N Tellurium Crystal Growth and Purification


I. I-Raw Material Pretreatment kanye Nokuhlanzwa Kwasekuqaleni

  1. .Ukukhethwa Kwezinto Eziluhlaza kanye Nokuchotshozwa.
  • .Izidingo Zempahla: Sebenzisa i-tellurium ore noma i-anode slime (Okuqukethwe kwe-Te ≥5%), okungcono kakhulu i-anode slime encibilikisa ithusi (equkethe i-Cu₂Te, Cu₂Se) njengento eluhlaza .
  • .Inqubo Yokwelapha Ngaphambili:
  • Ukuchotshozwa okuqinile kuya kusayizi wezinhlayiyana ≤5mm, kulandelwa ukugaya ibhola ukuya ku-≤200 mesh;
  • Ukuhlukaniswa kwamagnetic (amandla kazibuthe ≥0.8T) ukususa i-Fe, i-Ni, nokunye ukungcola kazibuthe;
  • I-Froth flotation (pH=8-9, abaqoqi be-xanthate) ukuze bahlukanise i-SiO₂, i-CuO, nokunye ukungcola okungekona kozibuthe .
  • .Izinyathelo zokuzivikela: Gwema ukufaka umswakamo ngesikhathi sokumanzisa (kudinga ukomiswa ngaphambi kokugazinga); lawula umswakama we-ambient ≤30%.
  1. .I-Pyrometallurgical Roasting kanye ne-Oxidation.
  • .Amapharamitha okucubungula:
  • Ukushisa kwe-oxidation yokuthosa: 350-600 ° C (ukulawula okuhleliwe: izinga lokushisa eliphansi le-desulfurization, izinga lokushisa eliphezulu le-oxidation);
  • Isikhathi sokuthosa: amahora angu-6-8, ngesilinganiso sokugeleza kwe-O₂ se-5–10 L/min;
  • I-Reagent: I-sulfuric acid egxilile (98% H₂SO₄), isilinganiso sesisindo Te₂SO₄ = 1:1.5 .
  • .Ukusabela Kwamakhemikhali:
    Cu2Te+2O2+2H2SO4→2CuSO4+TeO2+2H2OCu2Te+2O2+2H2 SO4​→2CuSO4+TeO2+2H2O
  • .Izinyathelo zokuzivikela: Lawula izinga lokushisa ≤600°C ukuze uvimbele ukuguquguquka kwe-TeO₂ (iphuzu elibilayo elingu-387°C); phatha igesi ephumayo ngezikhuhla ze-NaOH .

II. I-Electrorefining kanye ne-Vacuum Distillation

  1. .Electrorefining.
  • .Isistimu ye-Electrolyte:
  • Ukwakheka kwe-Electrolyte: H₂SO₄ (80–120g/L), i-TeO₂ (40–60g/L), isithako (i-gelatin 0.1–0.3g/L);
  • Ukulawulwa kwezinga lokushisa: 30–40°C, izinga lokugeleza kwegazi 1.5–2 m³/h .
  • .Amapharamitha okucubungula:
  • Ukuminyana kwamanje: 100–150 A/m², ugesi weseli 0.2–0.4V ;
  • Isikhala se-electrode: 80-120mm, ukujiya kwe-cathode 2-3mm/8h;
  • Ukusebenza kahle kokususa ukungcola: Cu ≤5ppm, Pb ≤1ppm.
  • .Izinyathelo zokuzivikela: Hlunga njalo i-electrolyte (ukunemba ≤1μm); Pholisha ngokuzenzakalelayo izindawo ezingaphezulu ze-anode ukuze kunqandwe ukudlula .
  1. .I-Vacuum Distillation.
  • .Amapharamitha okucubungula:
  • Izinga le-vacuum: ≤1×10⁻²Pa, izinga lokushisa lokukhipha isisu ngu-600–650°C ;
  • Izinga lokushisa lendawo ye-Condenser: 200–250°C, ukusebenza kahle kokufihlwa komhwamuko ≥95%;
  • Isikhathi sokukhipha isisu: 8–12h, umthamo weqoqo elilodwa ≤50kg .
  • .Ukusabalalisa Ukungcola: Ukungcola okubilayo okuphansi (Se, S) kunqwabelana ngaphambili kwe-condenser; ukungcola okubilayo kakhulu (Pb, Ag) kuhlala kuzinsalela .
  • .Izinyathelo zokuzivikela: Isistimu ye-vacuum ye-pre-pump ukuya ku-≤5×10⁻³Pa ngaphambi kokushisisa ukuvimbela i-Te oxidation.

III. Ukukhula Kwe-Crystal (I-Crystallization Eqondile).

  1. .Ukucushwa Kwezisetshenziswa.
  • .Amamodeli Wesithando Sokukhula KweCrystalTDR-70A/B (30kg umthamo) noma TRDL-800 (60kg umthamo);
  • Izinto ezibonakalayo: I-graphite ehlanzekile (okuqukethwe komlotha ≤5ppm), ubukhulu Φ300×400mm;
  • Indlela yokushisa: Ukushisa kokumelana ne-graphite, izinga lokushisa eliphakeme ngu-1200°C.
  1. .Amapharamitha okucubungula.
  • .Melt Control:
  • Izinga lokushisa elincibilikayo: 500-520°C, ncibilikisa ichibi ukujula 80-120mm;
  • Igesi evikelayo: I-Ar (ukuhlanzeka ≥99.999%), izinga lokugeleza 10-15 L/min.
  • .I-Crystallization Parameters:
  • Izinga lokudonsa: 1-3mm / h, isivinini sokujikeleza kwe-crystal 8-12rpm;
  • I-gradient yokushisa: I-Axial 30-50 ° C / cm, i-radial ≤10 ° C / cm;
  • Indlela yokupholisa: Isisekelo sethusi esipholiswe ngamanzi (ukushisa kwamanzi 20-25°C), ukupholisa ngemisebe ephezulu .
  1. .Ukulawula Ukungcola.
  • .Umphumela Wokuhlukanisa: Ukungcola okufana ne-Fe, i-Ni (i-coefficient yokuhlukanisa <0.1) inqwabelana emingceleni yokusanhlamvu;
  • .I-Remelting Cycles: Imijikelezo engu-3–5, ukungcola okuphelele kokugcina ≤0.1ppm .
  1. .Izinyathelo zokuzivikela:
  • Mboza indawo encibilikayo ngamapuleti e-graphite ukuze ucindezele i-Te volatilization (izinga lokulahlekelwa ≤0.5%);
  • Gada ububanzi bekristalu ngesikhathi sangempela usebenzisa izikali ze-laser (ukunemba ±0.1mm);
  • Gwema ukushintshashintsha kwezinga lokushisa > ±2°C ukuze uvimbele ukwanda kokuminyana kokususwa (thagethi ≤10³/cm²) .

IV. Ukuhlolwa kwekhwalithi kanye namamethrikhi angukhiye

Into yokuhlola

Inani Elijwayelekile

Indlela Yokuhlola

Umthombo

.Ubumsulwa.

≥99.99999% (7N)

I-ICP-MS

.Ukungcola Kwe-Metallic Okuphelele.

≤0.1ppm

I-GD-MS (Glow Discharge Mass Spectrometry)

.Okuqukethwe Oksijini.

≤5ppm

Ukumuncwa kwe-Inert Gas Fusion-IR

.Crystal Ubuqotho.

Ukuminyana Kokususwa ≤10³/cm²

I-X-ray Topography

.Ukungazweli (300K).

0.1–0.3Ω·cm

Indlela ye-Four-Probe


V. Izinqubo Zemvelo Nokuphepha

  1. .I-Exhaust Gas Treatment:
  • I-roast exhaust: Yenza i-SO₂ ne-SeO₂ ingathathi hlangothi ngezikhuhli ze-NaOH (pH≥10);
  • I-vacuum distillation exhaust: Hlanganisa futhi ubuyisele umhwamuko; amagesi asele akhangiswa ngekhabhoni ecushiwe.
  1. .I-Slag Recycling:
  • I-Anode slime (equkethe i-Ag, Au): Buyisela nge-hydrometallurgy (isistimu ye-H₂SO₄-HCl);
  • Izinsalela ze-Electrolysis (eziqukethe i-Pb, Cu): Buyela ezinhlelweni zokuncibilikisa ithusi.
  1. .Izinyathelo Zokuphepha:
  • Abaqhubi kufanele bagqoke imaski yegesi (I-Te vapor inobuthi); gcina umoya ocindezelayo ongemuhle (izinga lokushintshana komoya ≥10 imijikelezo/h) .

Imihlahlandlela Yokuthuthukisa Inqubo

  1. .Ukuzijwayeza kwe-Raw Material: Lungisa izinga lokushisa lokushiswa nesilinganiso se-asidi ngokuguquguqukayo ngokusekelwe emithonjeni ye-anode slime (isb., ithusi uma liqhathaniswa nokuncibilikiswa komthofu);
  2. .Ukufaniswa Kwezinga Lokudonsa Kwe-Crystal: Lungisa isivinini sokudonsa ngokuya nge- convection encibilikayo (inombolo ye-Reynolds Re≥2000) ukuze ucindezele ukupholisa okukhulu komthethosisekelo;
  3. .Ukusebenza Kwamandla: Sebenzisa ukushisisa kwendawo enamazinga okushisa akabili (izoni eyinhloko 500°C, indawo engaphansi engu-400°C) ukuze unciphise ukusetshenziswa kwamandla okumelana nama-graphite ngo-30%.

Isikhathi sokuthumela: Mar-24-2025