A kind of preparation method of multi-component silicon-based compound
A silicon-based compound and multi-component technology, applied in electrical components, battery electrodes, circuits, etc., can solve the problems of poor product phase uniformity, sample oxidation and carbonization, and low product purity, and achieve low cost, easy operation, and high purity. Effect
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Embodiment 1
[0030] In a glove box with an argon atmosphere, weigh LiH and MgH at a molar ratio of 2:1:1 2 and Si, put them into a ball mill jar, the ball-to-material ratio is 40:1, and the grinding balls are stainless steel balls. Will contain LiH, MgH 2 Put the ball mill jar of the mixture with Si on the planetary ball mill, and ball mill for 96 hours at a speed of 300 rpm to obtain 2LiH-MgH 2 -Si mixture. 2LiH-MgH 2 -Si mixture is heated to dehydrogenate in vacuum at a heating rate of 5°C / min. After the temperature rises to 600°C, it is kept warm for 2 hours and the system is evacuated, and then the furnace is cooled to room temperature. Take it out from the glove box of the atmosphere to get Li 2 MgSi sample.
[0031] figure 1 2LiH-MgH after ball milling 2 -The graph of the hydrogen desorption of the Si mixture as a function of temperature, from figure 1 It can be seen from the figure that the initial temperature of the dehydrogenation reaction is around 240°C, and after the te...
Embodiment 2
[0033] In a glove box with a nitrogen atmosphere, weigh LiH and MgH at a molar ratio of 2:1:1 2 and Si, put them into a ball mill jar, the ball-to-material ratio is 80:1, and the grinding balls are zirconia balls, which will contain LiH, MgH 2 Put the ball mill jar of the mixture with Si on the planetary ball mill, and ball mill for 48 hours at a speed of 400 rpm to obtain 2LiH-MgH 2 -Si mixture. 2LiH-MgH 2 -Si mixture is heated to release hydrogen in a reactor with nitrogen gas at a heating rate of 10°C / min. After heating to 600°C, it is kept for 8 hours, and then the furnace is cooled to room temperature, and the obtained sample is removed from the nitrogen atmosphere. Take it out of the glove box to get Li 2 MgSi sample.
[0034] figure 2 2LiH-MgH 2 The XRD pattern (X-ray diffraction pattern) of the product after the Si mixture is heated to release hydrogen, from figure 2 It can be seen that the crystallinity of the product is good.
Embodiment 3
[0036] In a glove box with an argon atmosphere, weigh LiH and MgH at a molar ratio of 2:1:1 2 and Si, put them into a ball mill jar, the ball-to-material ratio is 120:1, and the grinding balls are stainless steel balls, which will contain LiH, MgH 2 Put the ball mill jar of the mixture with Si on the planetary ball mill, and ball mill for 24 hours at a speed of 550 rpm to obtain 2LiH-MgH 2 -Si mixture. 2LiH-MgH 2 -Si mixture is heated to release hydrogen in a reactor with argon gas at a heating rate of 12°C / min. After the heating temperature rises to 600°C, it is kept for 6 hours, and then the furnace is cooled to room temperature, and the obtained sample is removed from the argon atmosphere. Take it out of the glove box to get Li 2 MgSi sample.
[0037] image 3 2LiH-MgH 2 The scanning electron micrograph of the product after the Si mixture is heated to release hydrogen, and the scanning electron micrograph shows that the product particles are submicron.
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