Hafnium iodide refining process conditions shown in Table 1, the hafnium arc melting process conditions are shown in Table 2, the electron beam melting hafnium parameters in Table 3. Table 1 iodine refining process conditions Hot wire material W or Hf Rough temperature / °C 600 Hot wire temperature / °C 1400~1600 Twin rod purity /% Hf>99.9, C=0.20, O=0.01-0.04, N=0.001-0.004, Fe=0.003～0.08 Hardness HB 170 Dissociation reaction Table 2 Process conditions of arc melting Smelting method Non-consumable electrode Consumable electrode arc melting Double arc melting Non-consumable electrode 1 Consumable electrode Electrode head Tungsten or tungsten coated with 1% to 2% ThO2 has a diameter of 1.27 to 1.91 cm and a length of 1.91 to 3.81 cm embedded in a water-cooled copper electrode. Hf W Hf crucible An inner diameter of 10.16 ~ 12.7cm, water-cooled copper crucible disposed in advance some of the feedstock to a very small amount of magnesium Inner diameter 10.16 ~ 12.7cm, water-cooled copper crucible The inner diameter of 6.35cm is first plugged with the tip of the crucible at the bottom of the copper crucible. The inner diameter is 10.16~12. 7cm Vacuum before filling with inert gas /kPa 1.33×10 - 3 (1.33~2)×10 - 3 (1.33~2)×10 - 3 (1.33~2)×10 - 3 atmosphere 5He+1Ar 1He+1Ar 2He+1Ar 1He+1Ar Total pressure / kPa 101.3 16.88 101.3 16.88 Melting voltage / V 48~50 30~35 38~42 30~35 Smelting current / kA 1.0 to 1.1 2.8~2.9 1.2 to 1.8 2.3 to 2.5 Smelting speed /kg·h - 1 4.54 27.22 81.65 Recovery rate/% 97 铪 ingot hardness HB 184 171 Table 3 铪 electron beam melting parameters Material size / cm 8.4 铪 ingot diameter / cm 8.4 11 Smelting times 1 2 Melting vacuum / kPa 1.33×10 - 5 1.07×10 - 5 Smelting power / kW 46~48 58～60 铪 smelting speed / kg · h - 1 12~14 20~24 Cooling time / h 2.5 3.5 1kg 铪 power consumption / kW · h 3.4 to 4.0 2.5 to 3 Ingot rate /% 92～94 96 The conditions for 铪 electron beam melting given by Thomas Thomas are: Furnace power: 225 kW (with two oil diffusion pumps with a displacement of 34 m 3 /s). 铪 ingot diameter: 7.62 ~ 15.24cm Melting degree of vacuum: ≥1.33×10 - 5 kPa Melting voltage: 4000～12000V Electron gun bombardment current: 0 ~ 15A Monthly production capacity: 1814kg The first stage of smelting: 4h, rapid melting of the slightly pressed sponge into a bismuth ingot, diameter 7.62cm, length 10.16cm; The second stage of smelting: 6h, the re-melting of the bismuth ingot, to ensure a certain degree of superheat, the diameter is still 7.62cm; The third stage of smelting: 1h, and then smelted into a bismuth ingot, the diameter of 10.16cm, length 5.08cm; The impurity content of the electron beam melting crucible is shown in Table 4. Table 4 Impurity content of electron beam melting crucible /10 - 6 element raw material Electron beam melting bismuth ingot top bottom top bottom Al 60 75 25 25 B 7 3 0.3 0.5 C 30 30 30 30 Cd 1 2 1 1 Co 5 5 5 5 Cr 40 50 20 20 Cu 30 30 30 30 Fe 110 140 50 50 Mg 10 10 20 20 Mn 10 10 10 10 Mo 40 40 40 40 N 35 63 28 35 O 850 1100 298 266 Si 200 200 70 70 Ti 100 120 10 10 Zr 2.2% 2.1% 1.8% 1.4% Hardness HB 188 171 Pharmaceutical Raw Materials Sodium Hydride,Desiccant Alkylating Agent 7646-69-7,Sodium Hydride 7646-69-7,Cyclopropanamine Cas 765-30-0 Shandong YunFengLian Chemical Co.,Ltd , https://www.yfluorine.com
HfI 4 =Hf+4I, 1gK=21390/T+4.463 (1200～1600K)
1 Each barium ingot weight is 15.88kg.
Preparation of high purity and compact