Method for preparing magnesium silicide-based powder thermoelectric material by utilizing polysilicon byproduct
A technology of thermoelectric materials and by-products, applied in the direction of nanotechnology for materials and surface science, metal silicide, hydrogen production, etc., can solve the problems of difficult SiCl recovery and reduce production costs
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Embodiment approach 1
[0016] First weigh 0.26mol of MgH 2 (particle size≤45μm, purity≥99.5%) and 1.04mol of C 4 h 8 O (purity 99.2%) was placed in the three-necked flask 4, and sealed, and then weighed 0.13mol of MgH 2 (particle size ≤ 45μm, purity ≥ 99.5%) placed in U-shaped reactor 10, and sealed, the three-necked flask 4 and filter device 5, drying device 6, gas cylinder 7, pressure reducing valve 8, flow meter 9, The U-shaped reactor 10 and the mineral oil 12 are connected sequentially by quartz tubes, wherein the three-necked flask 4 is immersed in a glycerin bath 13 with a temperature of 120 ° C, and is continuously stirred with an electric stirrer 2 , and the U-shaped reactor 10 is placed in a heating furnace 11 . First pass 80ml / min of carrier gas Ar into the entire connection device for cleaning for 5min, then adjust the flow rate to 20ml / min, and inject 0.065mol of SiCl with syringe 3 4 (purity 99%) was injected into the three-necked flask 4, and the product SiH was obtained after the...
Embodiment approach 2
[0018] First weigh 0.13mol of MgH 2 (particle size≤45μm, purity≥99.5%) and 1.04mol of C 4 h 8 O (purity 99.2%) was placed in the three-necked flask 4, and sealed, and then weighed 0.13mol of MgH 2(particle size ≤ 45μm, purity ≥ 99.5%) placed in U-shaped reactor 10, and sealed, the three-necked flask 4 and filter device 5, drying device 6, gas cylinder 7, pressure reducing valve 8, flow meter 9, The U-shaped reactor 10 and the mineral oil 12 are connected sequentially by quartz tubes, wherein the three-necked flask 4 is immersed in a glycerin bath 13 with a temperature of 125°C, and is continuously stirred with an electric stirrer 2, and the U-shaped reactor 10 is placed in a heating furnace 11 . First pass 80ml / min of carrier gas Ar into the entire connecting device for cleaning for 8min, then adjust the flow rate to 20ml / min, and inject 0.065mol of SiCl with syringe 3 4 (purity 99%) was injected into the three-necked flask 4, and the product SiH was obtained after the rea...
Embodiment approach 3
[0020] First weigh 0.13mol of MgH 2 (particle size≤45μm, purity≥99.5%) and 0.52mol of C 4 h 8 O (purity 99.2%) was placed in the three-necked flask 4, and sealed, and then weighed 0.13mol of MgH 2 (particle size ≤ 45μm, purity ≥ 99.5%) placed in U-shaped reactor 10, and sealed, the three-necked flask 4 and filter device 5, drying device 6, gas cylinder 7, pressure reducing valve 8, flow meter 9, The U-shaped reactor 10 and the mineral oil 12 are connected sequentially by quartz tubes, wherein the three-necked flask 4 is immersed in a glycerin bath 13 with a temperature of 130° C. and continuously stirred with an electric stirrer 2 , and the U-shaped reactor 10 is placed in a heating furnace 11 . First pass 80ml / min of carrier gas Ar into the entire connection device for cleaning for 10min, then adjust the flow rate to 20ml / min, and use syringe 3 to inject 0.065mol of SiCl 4 (purity 99%) was injected into the three-necked flask 4, and the product SiH was obtained after th...
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