Method for preparing lanthanide nitride using metal oxide
A nitride and oxide technology, applied in rare earth metal compounds, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of high temperature and long time, and achieve the effects of simple equipment, low cost, and avoiding low purity
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Embodiment 1
[0019] Using metallic lithium with a purity of 99% as raw material, in a flowing nitrogen atmosphere with a purity of 99.999%, the temperature is increased from room temperature to 450°C at a rate of 15°C / min, and the temperature is kept for 30 minutes; then at a rate of 10°C / min Raise the temperature to 600°C and keep it for 60 minutes; turn off the power and cool down with the furnace to synthesize lithium nitride. Weigh 0.01 mol of synthetic lithium nitride and 0.005 mol of lanthanum oxide into an agate mill and grind until the lithium nitride becomes a powder. After the two are evenly mixed, apply a pressure of 15 MPa to the powder with a tablet press. After the powder is pressed into flakes, it is placed in a crucible made of stainless steel with an outer diameter of 16mm, an inner diameter of 14mm, and a height of 15mm. The crucible is placed in a quartz tube and the vacuum system is quickly connected to vacuum to 10 -4 After Pa, fill it with 0.4 atmospheres of nitrogen with...
Embodiment 2
[0021] Using metallic calcium with a purity of 99% as raw material, in a flowing nitrogen atmosphere with a purity of 99.999%, the temperature is increased from room temperature to 450°C at a rate of 15°C / min, and the temperature is kept for 30 minutes; then at a rate of 10°C / min Warm up to 600℃, keep the temperature for 60 minutes, turn off the power, cool with the furnace to synthesize calcium nitride; weigh 0.011mol of synthesized calcium nitride and 0.011mol of lanthanum oxide into an agate mill and grind until calcium nitride becomes powder The two are mixed uniformly. Use a tablet press to apply a pressure of 18 MPa to the powder. After the powder is pressed into flakes, it is placed into a crucible made of stainless steel with an outer diameter of 16 mm, an inner diameter of 14 mm and a height of 15 mm. Put it into the quartz tube and quickly connect the vacuum system to vacuum to 10 -4 After Pa, fill it with 0.4 atmospheres of nitrogen with a purity of 99.999%, then close ...
Embodiment 3
[0023] Using metallic magnesium with a purity of 99% as raw material, in a flowing nitrogen atmosphere with a purity of 99.999%, the temperature is increased from room temperature to 450°C at a rate of 15°C / min, and the temperature is kept for 30 minutes; then at a rate of 10°C / min Heat up to 600°C and keep it for 60 minutes; turn off the power and cool with the furnace to synthesize magnesium nitride; weigh 0.020mol of synthesized magnesium nitride and 0.015mol of lanthanum oxide into an agate mill and grind until magnesium nitride becomes powder The two are mixed uniformly. Use a tablet press to apply a pressure of 20 MPa to the powder, press the powder into a sheet and put it into a platinum crucible, put the crucible into a quartz tube and quickly connect the vacuum system to vacuum at the same time To 10 -4 After Pa, fill it with 0.3 atmospheres of nitrogen with a purity of 99.999%, then close the quartz tube, heat it to 900°C within 4 hours, keep it at this temperature for 2...
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