Preparation method of multilevel twin structure silicon nitride high temperature ceramic material
A technology of high-temperature ceramics and silicon nitride, which is applied in the field of preparation of multi-level twinned silicon nitride high-temperature ceramic materials, can solve the problems of performance weakening and grain growth, so as to improve fluidity, inhibit grain growth, Accelerated densification effect
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[0018] A method for preparing a multi-level twin structure silicon nitride high-temperature ceramic material of the present invention comprises the following steps:
[0019] (1) Using three-dimensional eddy current resonance ball mill equipment to perform high-frequency impact treatment on silicon powder, the spindle speed is 150-300 rpm, the vibration frequency is 6-12 Hz, and then synthesized in a nitrogen atmosphere high-temperature tube furnace with a nitrogen flow rate of 100 ~240ml / min, synthetic temperature 1520~1590℃, heat preservation 100~120 minutes, heating and cooling rate 4~6℃ / min, to obtain nano-silicon nitride powder;
[0020] (2) Add glue to the nano-silicon nitride powder and centrifugally spheroidize it. The spheroidized glue is 35mol / L polyvinyl butyral alcohol solution, and the mass ratio of powder to glue is (86.3~94.3):(5.7~13.7), degreased Finally, it is formed in a two-way heavy pressing device, the degreasing temperature is 500-530°C, and the cold form...
Embodiment 1
[0024] (1) Using three-dimensional eddy current resonance ball mill equipment to carry out high-frequency impact treatment on elemental silicon powder, the spindle speed is 150 rpm, the vibration frequency is 6 Hz, and then synthesized in a nitrogen atmosphere high-temperature tube furnace, and the nitrogen flow rate is 240 ml / min. The synthesis temperature is 1520°C, the temperature is kept for 100 minutes, and the heating and cooling rate is 5°C / min to obtain nano-silicon nitride powder;
[0025] (2) Add glue to the nano-silicon nitride powder and centrifugally spheroidize it. The spheroidized glue is 35mol / L polyvinyl butyral alcohol solution, and the mass ratio of powder to glue is 87:13. After degreasing, it is molded in a two-way heavy pressure device , the degreasing temperature is 500°C, and the cold pressing pressure is 280MPa to obtain a polycrystalline silicon nitride green body;
[0026] (3) The molded body was placed in a four-way overpressure heat collector for u...
Embodiment 2
[0028] (1) Using three-dimensional eddy current resonance ball mill equipment to carry out high-frequency impact treatment on elemental silicon powder, the spindle speed is 170 rpm, the vibration frequency is 7 Hz, and then synthesized in a nitrogen atmosphere high-temperature tube furnace, and the nitrogen flow rate is 120 ml / min. The synthesis temperature is 1530°C, the temperature is kept for 100 minutes, and the heating and cooling rate is 5°C / min to obtain nano-silicon nitride powder;
[0029] (2) Add glue to the nano-silicon nitride powder and centrifugally spheroidize it. The spheroidized glue is 35mol / L polyvinyl butyral alcohol solution, and the mass ratio of powder to glue is 88:12. After degreasing, it is molded in a two-way heavy pressure device , the degreasing temperature is 520°C, and the cold pressing pressure is 250MPa to obtain a polycrystalline silicon nitride green body;
[0030] (3) The molded body was placed in a four-way overpressure heat collector for u...
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