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Silicon nitride powder precursor, silicon nitride powder and preparation method thereof
The invention discloses a silicon nitride powder precursor, silicon nitride powder and a preparation method thereof.The preparation method of the silicon nitride powder comprises the following steps that S1, Si powder, silicon nitride powder, triethyl phosphate, polyvinyl butyral and ethyl alcohol are taken and subjected to ball milling and mixing, and precursor slurry is obtained; s2, carrying out spray granulation on the precursor slurry to obtain a precursor; and S3, adding the precursor into an inclined rotating fluidized bed reaction chamber, introducing N2 into the rotating reaction chamber under N2 airflow, and heating the granulation powder, so that the granulation powder and N2 are subjected to a nitridation reaction, and Si3N4 powder is obtained. The continuous batch preparation of the target powder is realized by controlling the adding rate and the reaction temperature of the granulated powder, the rotation rate of the fluidized bed reaction chamber and the flow of the high-purity N2; and meanwhile, the ratio of the alpha phase in the prepared Si3N4 powder is increased, and the impurity content is stable.
本发明公开了一种氮化硅粉体前驱体、氮化硅粉体及其制备方法,该氮化硅粉体的制备方法包括如下步骤:S1取Si粉、氮化硅粉、磷酸三乙酯、聚乙烯醇缩丁醛和乙醇球磨混合,得到前驱体料浆;S2对所述前驱体料浆进行喷雾造粒,得到前驱体;S3将所述前驱体加入倾斜旋转流化床反应室,在N2气流下,旋转反应室中通入N2并加热所述造粒粉,使其与N2发生氮化反应,得到Si3N4粉。本发明通过控制造粒粉的加入速率、反应温度、流化床反应室的旋转速率及高纯N2流量,实现目标粉体的连续批量化制备;同时实现所制备Si3N4粉体中α相比例升高,以及杂质含量的稳定。
Silicon nitride powder precursor, silicon nitride powder and preparation method thereof
The invention discloses a silicon nitride powder precursor, silicon nitride powder and a preparation method thereof.The preparation method of the silicon nitride powder comprises the following steps that S1, Si powder, silicon nitride powder, triethyl phosphate, polyvinyl butyral and ethyl alcohol are taken and subjected to ball milling and mixing, and precursor slurry is obtained; s2, carrying out spray granulation on the precursor slurry to obtain a precursor; and S3, adding the precursor into an inclined rotating fluidized bed reaction chamber, introducing N2 into the rotating reaction chamber under N2 airflow, and heating the granulation powder, so that the granulation powder and N2 are subjected to a nitridation reaction, and Si3N4 powder is obtained. The continuous batch preparation of the target powder is realized by controlling the adding rate and the reaction temperature of the granulated powder, the rotation rate of the fluidized bed reaction chamber and the flow of the high-purity N2; and meanwhile, the ratio of the alpha phase in the prepared Si3N4 powder is increased, and the impurity content is stable.
本发明公开了一种氮化硅粉体前驱体、氮化硅粉体及其制备方法,该氮化硅粉体的制备方法包括如下步骤:S1取Si粉、氮化硅粉、磷酸三乙酯、聚乙烯醇缩丁醛和乙醇球磨混合,得到前驱体料浆;S2对所述前驱体料浆进行喷雾造粒,得到前驱体;S3将所述前驱体加入倾斜旋转流化床反应室,在N2气流下,旋转反应室中通入N2并加热所述造粒粉,使其与N2发生氮化反应,得到Si3N4粉。本发明通过控制造粒粉的加入速率、反应温度、流化床反应室的旋转速率及高纯N2流量,实现目标粉体的连续批量化制备;同时实现所制备Si3N4粉体中α相比例升高,以及杂质含量的稳定。
Silicon nitride powder precursor, silicon nitride powder and preparation method thereof
一种氮化硅粉体前驱体、氮化硅粉体及其制备方法
GAO PENGZHAO (author) / XIAO HANNING (author) / QIN HANG (author) / GUO WENMING (author)
2024-11-29
Patent
Electronic Resource
Chinese
IPC:
C04B
Kalk
,
LIME
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