Process for preparing SiBONC ceramic with high temp stabilized
A high-temperature stable, ceramic technology, applied in the field of preparation of amorphous silicon-based ceramics, can solve the problems of poor reliability and relatively high cost
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specific Embodiment approach 1
[0015] Specific embodiment one: this embodiment includes the following steps: (one) synthesizing SiONC precursor; (two) synthesizing SiBONC precursor; (three) cracking SiBONC precursor, making SiBONC ceramic powder; the core content of this method In the step (1), the SiONC precursor is synthesized as follows: organic silicone oil and alkylamine are used as raw materials, dissolved in an organic solvent, mixed and stirred, and kept at 70-100° C. for 20-30 hours to synthesize the SiONC precursor. In the step (2) of this embodiment, the SiBONC precursor is synthesized as follows: Boride is introduced into the SiONC organic polymer, and reacted at 60-150°C for 5-15 hours to obtain the SiBONC organic polymer, wherein Si The molar ratio of / B is between 1:0.1-0.5, and the boron compound is boron trichloride, borane or diborane. In step (3), the SiBONC precursor is cracked to obtain SiBONC powder: In a tubular atmosphere protection furnace, nitrogen or inert gas is introduced, at 30...
specific Embodiment approach 2
[0016] Specific embodiment two: this embodiment differs from specific embodiment one in that it also includes step (four): the prepared SiBONC powder is sintered to obtain dense SiBONC amorphous and microcrystalline ceramic products, which can be passed through the following steps: The above two methods are realized: one method is to sinter the prepared Si-B-O-N-C powder in a pressure sintering furnace, feed nitrogen or inert gas, control the reaction temperature at 1100-1900 °C, and the heating rate is 5-50 °C / min , pressure of 0.1 ~ 10Mpa under the condition of heat preservation for 2 ~ 4 hours, after sintering to obtain dense SiBONC amorphous and microcrystalline ceramic products; another method is to prepare SiBONC powder in a vacuum / atmosphere hot pressing sintering furnace Sintering, heat preservation under the conditions of 1400-1900°C and 10-40MPa for 1-3 hours, and obtain dense SiBONC amorphous and microcrystalline ceramic products after sintering. Other reaction step...
specific Embodiment approach 3
[0017] Specific embodiment three: this embodiment takes high hydrogen-containing methyl silicone oil (HPSO) and ethylenediamine as raw materials, and toluene is a solvent, and it prepares SiBONC ceramics in this way: (1) get 120ml HPSO and be dissolved in 400ml toluene, and 44ml ethylenediamine and 100ml toluene are slowly dripped into the mixed solution of HPSO and toluene with a dropping funnel, and stirred for 24 hours with a stirrer to form a SiONC organic precursor; (2) 300gAlCl 3 with 200gKBF 4 Ball mill and mix in a special stainless steel reactor for 3-11 hours, and generate BCl in an oil bath at 70-180°C 3 , then the resulting BCl 3 The gas is passed into the SiONC organic precursor, and reacted at 70-100 °C for 10 hours to obtain the SiBONC organic polymer; (3) In the tubular atmosphere protection furnace, nitrogen gas is introduced, at 800-1000 °C, the heating rate Control the reaction at 1-5°C / min for 10 hours to crack the SiBONC organic polymer to obtain SiBONC ...
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