块体硅高效氮化制备高α相氮化硅陶瓷研究

    Study on Preparation of High α-Phase Silicon Nitride Ceramics by Efficient Nitridation of Bulk Silicon

    • 摘要: 通过直接氮化法结合高能球磨制备高α相氮化硅块体。以硅粉为原料,添加不同质量分数的α-Si3N4稀释剂混合冷压制成不同厚度的块体,在1350℃氮化不同时间制备了Si3N4块体,研究了块体硅直接氮化反应合成氮化硅块体的工艺因素,借助XRD检测手段测定氮化产物的物相组成。结果表明:含15%稀释剂(α-Si3N4)、厚度为3 mm的块体硅在流动氮气气氛下,于1350℃保温3 h的氮化效果最佳,氮化产物由3种物相组成,各物相的质量分数为88.7%α-Si3N4、10.2%β-Si3N4、1.1% Si,合成了含高α相的氮化硅块体。本研究结果可为块体高α相氮化硅的高效制备提供实验依据。

       

      Abstract: High α-phase silicon nitride bulk was prepared by direct nitridation method combined with high-energy ball milling. Taking silicon powder and α-Si3N4 diluents with different mass ratios as the raw material,the green block with different thicknesses were compressed,then the Si3N4 bulk materials were prepared by nitriding at 1350℃ for different times.The process factors for the synthesis of silicon nitride bulk materials through direct nitridation reaction of silicon blocks were investigated. The results show that when the silicon block with a thickness of 3 mm and 15% diluent (α-Si3N4) content is nitrided at 1350℃ for 3 h under a flowing nitrogen gas atmosphere,the nitridation effect is the best,and the products consist of three phases.The mass content of each phase is as follows:α-Si3N4(88.7%),β-Si3N4(10.2%),and Si(1.1%). The process successfully synthesizes silicon nitride bulk materials with a high α-phase content. The results of the study provide evidence for the efficient preparation of bulk silicon nitride with high α-phase content.

       

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