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Hafnium: Iodide Vapour Split on a Tungsten Wire Heated beyond 1600 °C (van Arkel and de Boer, US 1,671,213)
Hafnium will not come out of its chloride and hydrogen as clean metal. Van Arkel and de Boer instead let the vapour of hafnium iodide pass a white-hot wire in an evacuated vessel: the iodide splits and pure hafnium grows on the wire.
Result: hafnium metal deposited on the wire.
Source: A. E. van Arkel and J. H. de Boer, US 1,671,213 (1928). The wire runs white-hot; iodine vapour is released. Picture: the patent drawing.
Advanced
1 day
Instructions
1
1
Set up the vessel and wire
Set up the vessel and wire
Hang a wire, for example of tungsten, inside the vessel, fixed with small screws to two leading-in wires sealed through its narrowed top. A side tube goes to a pump. For the high temperatures the iodides need, the patent advises a vessel of suitable metal such as chrome iron rather than glass.
Tools needed:
Glass Vessel
Tungsten Wire
DC Power Supply2
2
Pump out the air
Pump out the air
Put the hafnium iodide in the vessel and pump out the air and any other gas that would spoil the reaction.
Materials for this step:
Hafnium Iodide1 as requiredTools needed:
Vacuum Pump3
3
Evaporate the iodide
Evaporate the iodide
Heat the vessel until the iodide gives enough vapour. The patent gives 400-600 °C only for zirconium iodide; for hafnium iodide the temperature is not given. Ours: a furnace round the vessel.
Tools needed:
Tube Furnace4
4
Deposit hafnium on the white-hot wire
Deposit hafnium on the white-hot wire
Pass a current through the wire to heat it beyond 1600 °C while the iodide vapour flows along it. The iodide splits and hafnium deposits on the wire. Do not overheat: the deposit can alloy with the wire.
Tools needed:
DC Power Supply
PyrometerTungsten WireMaterials
1- 1 as requiredPlaceholder
Tools Required
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