Novel method for synthesizing silicon nitride powder with high alpha phases by catalysis and nitridation
The technology of a phase silicon nitride powder and a new method is applied in the field of catalyst synthesis of silicon nitride powder and the addition of diluents by normal pressure direct nitridation method. The effect of increasing activity
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Embodiment 1
[0031] A. Mixing of raw materials:
[0032] Si powder with an average particle size of 55 μm and a purity of 95.8%wt was mixed with Si powder with an average particle size of 5 μm 3 N 4 Powder, by mass percentage Si powder 69%wt, Si 3 N 4 Powder 30%wt, FeCl 3 ·6H 2 After mixing 1% wt of O powder, put it into a planetary ball mill and mill it for 1 hour to make it fully mixed;
[0033] B. Direct nitriding reaction:
[0034] Put the mixed material into the crucible, the bulk density is 1.1g / cm 3 ; Then put the crucible into the reaction furnace to wash the gas; start heating, press the attached Figure 4 to heat up. From room temperature to 300°C, the heating rate is 5°C / min; the holding time at 300°C is 10 minutes; the heating rate at 300-600°C is 10°C / min; the holding time at 600°C is 1.5h; min, 1200°C holding time is 3h, 1200°C is evenly raised to the reaction temperature, the heating time is 1h, and the heat preservation is started at 1400°C, and the heat preservati...
Embodiment 2
[0036] A. Mixing of raw materials:
[0037] Si powder with an average particle size of 15 μm and a purity of 95.6%wt was mixed with Si powder with an average particle size of 5 μm 3 N 4 Powder, by mass ratio Si powder 79.5%wt, Si 3 N 4 Powder 20%wt, FeCl 3 ·6H 2 After mixing 0.5%wt of O powder, put it into a planetary ball mill and mill it for 3 hours to make it fully mixed;
[0038] B. Direct nitriding reaction:
[0039] Put the mixture into the crucible, the bulk density is 1.3g / cm 3 ; Then put the crucible into the reaction furnace to wash the gas; start heating, press the attached Figure 4to heat up. From room temperature to 300°C, the heating rate is 5°C / min; the holding time at 300°C is 10 minutes; the heating rate at 300-600°C is 10°C / min; the holding time at 600°C is 1.5h; min, 1200°C holding time is 3h, 1200°C is evenly raised to the reaction temperature, the heating time is 1h, the heat preservation is started at 1450°C, and the heat preservation is 10h. T...
Embodiment 3
[0041] A. Mixing of raw materials:
[0042] Si powder with an average particle size of 30 μm and a purity of 93.7%wt was mixed with Si powder with an average particle size of 5 μm 3 N 4 Powder, by mass ratio Si powder is 48%wt, Si 3 N 4 Powder 50%wt, FeCl 3 ·6H 2 After mixing 2% wt of O powder, put it into a planetary ball mill and mill it for 2 hours to make it fully mixed;
[0043] B. Direct nitriding reaction:
[0044] Put the mixture into the crucible, the bulk density is 1.5g / cm 3 ; Then put the crucible into the reaction furnace to wash the gas; start heating, press the attached Figure 4 to heat up. From room temperature to 300°C, the heating rate is 5°C / min; the holding time at 300°C is 10 minutes; the heating rate at 300-600°C is 10°C / min; the holding time at 600°C is 1.5h; min, 1200°C holding time is 3h, 1200°C is evenly raised to the reaction temperature, the heating time is 1h, the heat preservation is started at 1350°C, and the heat preservation is 10h. ...
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