Rare earth fluoride and its production method
A technology of rare earth fluoride and production method, applied in rare earth metal compounds, chemical instruments and methods, inorganic chemistry, etc., can solve problems such as restricting application and development, and achieve the effects of stable product quality and simple production method
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Embodiment 1
[0034] Place the commercially available lanthanum fluoride raw material in a tungsten crucible and put it into a vacuum resistance furnace, install a molybdenum collection cover with openings on the upper part (open holes are conducive to the escape of volatile substances) on the crucible, and connect the outside of the molybdenum collection cover Water cooling; vacuumize and keep the absolute pressure in the resistance furnace ≤ 10Pa, heat up, keep warm after the temperature of the lanthanum fluoride raw material in the crucible reaches 1450 °C, and control the temperature of the collection cover by water cooling to ≤ 1000 °C; stop heating, take out after cooling and collect cover and attached lanthanum fluoride. The content of non-rare earth impurities in the distilled rare earth fluoride products was measured, and O was measured by LeCo TC400 oxygen and nitrogen analyzer. The following embodiments are the same.
[0035] Put the above-mentioned lanthanum fluoride taken from...
Embodiment 2
[0041] Put the dysprosium fluoride raw material into a molybdenum crucible and place it in a vacuum resistance furnace, and install the molybdenum collection cover on the crucible; vacuumize and keep the absolute pressure in the resistance furnace ≤ 20Pa; heat up and control the distillation temperature to 1350±50°C , control the temperature of the collection cover to ≤900°C; stop heating, and take out the collection cover and attachments after cooling. Peel off the attachment on the molybdenum flake collection cover is dysprosium fluoride product. The analysis results of dysprosium fluoride before and after distillation are shown in Table 2:
[0042]Table 2: Detection results of dysprosium fluoride before and after distillation (unit: wt%)
[0043] Non-rare earth impurities O SiO 2 C Fe 2 o 3 Al 2 o 3 CaO before distillation 0.12 0.01 0.02 0.01 0.10 0.091 after distillation 0.01 0.004 0.005 0.006 0.005 0.005
Embodiment 3
[0045] Put the yttrium fluoride raw material into the niobium crucible and place it in the vacuum intermediate frequency furnace, install the molybdenum collection cover on the crucible; evacuate and keep the absolute pressure in the intermediate frequency furnace ≤ 20Pa to heat up, control the distillation temperature to 1300±10 degrees and Heat preservation, control the temperature of the collection hood to ≤1000°C; stop heating, let it cool naturally for 2 hours, and then flow argon gas into the collection hood to accelerate cooling. When the material in the collection hood is close to room temperature and comes out of the oven, take out the collection hood and attachments. The material on the stripping collection cover is distilled yttrium fluoride. The analysis results of yttrium fluoride before and after distillation are shown in Table 3:
[0046] Table 3: Test results before and after distillation of yttrium fluoride (unit: wt%)
[0047] Non-rare earth impuri...
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