Method for preparing FeAs powder by mechanical alloying
A mechanical alloying and powder technology, applied in chemical instruments and methods, inorganic chemistry, iron compounds, etc., can solve the problems of easy generation of impurity phases and high cost, and achieve the effects of high purity, low temperature and low preparation cost.
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Embodiment 1
[0029] 1) Use iron powder and arsenic powder with a purity of 99.5% and 98% respectively, mix them in a molar ratio of 1:1, put them into a vacuum ball mill tank, and then inject high-purity argon gas of about 0.15 MPa;
[0030] 2) Place the vacuum ball milling tank in step 1) on a high-energy planetary ball mill, the lining material of the vacuum ball milling tank is stainless steel, the material of the grinding balls is stainless steel, and the grinding balls are 6mm and 10mm grinding balls distributed in a weight ratio of 1:1, The ball-to-material ratio is 10:1, and the mechanical alloying reaction is carried out at a rotation speed of 320r / min. During the reaction process, it runs continuously for 40 minutes and then pauses for 5 minutes. The reaction time is 40 hours. After the mechanical alloying reaction is completed, stand still for 2 hours before taking out the sample; Such as figure 1 As shown, the XRD diffraction peaks of the FeAs-MA sample after ball milling are ob...
Embodiment 2
[0034] 1) Use iron powder and arsenic powder with a purity of 99.5% and 98% respectively, mix them in a molar ratio of 1:1, put them into a vacuum ball mill tank, and then pass high-purity nitrogen gas of about 0.15 MPa;
[0035] 2) Place the vacuum ball mill in step 1) on a high-energy planetary ball mill. The lining material of the vacuum ball mill is corundum. The rotation speed of min is used for mechanical alloying reaction. During the reaction process, it runs continuously for 40 minutes and then pauses for 10 minutes. The reaction time is 32 hours. After the mechanical alloying reaction is over, let it stand for 2 hours before taking out the sample;
[0036] 3) The sample in step 2) is taken out, and placed in a nitrogen-purged tube furnace for annealing treatment. Raise from room temperature to 200°C at a rate of 10°C / min and hold for 1 hour; then raise the temperature to 850°C at a rate of 10°C / min and hold for 24 hours, and finally cool to room temperature with the f...
Embodiment 3
[0039] 1) Iron powder and arsenic powder with a purity of 99% are used, mixed according to a molar ratio of 1:1, put into a vacuum ball mill jar, and then high-purity argon gas of about 0.15MPa is introduced.
[0040] 2) Place the vacuum ball mill in step 1) on a high-energy planetary ball mill. The lining material of the vacuum ball mill is stainless steel, the material of the balls is stainless steel, the size of the balls is 6mm, the ball-to-material ratio is 20:1, and 320r / The rotation speed of min is used for mechanical alloying reaction. During the reaction process, it runs continuously for 60 minutes and then pauses for 15 minutes. The reaction time is 36 hours. After the mechanical alloying reaction is completed, stand still for 2 hours before taking out the sample;
[0041] 3) Take out the sample in step 2), place it in an argon-purged tube furnace for annealing treatment, raise it from room temperature to 200°C at a rate of 10°C / min and keep it warm for 1h; then heat...
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