直接氮化法制备高品质氮化硅陶瓷粉体  

High-quality silicon nitride ceramic powders by direct nitriding method

作　　者：赵丽艳 刘耀耀 杨静思 韩江则[1] 李昆杰[1] 赵瑞红[1] 赵佳赛 ZHAO Liyan;LIU Yaoyao;YANG Jingsi;HAN Jiangze;LI Kunjie;ZHAO Ruihong;ZHAO Jiasai(School of Chemical and Pharmaceutical Engineering,Hebei University of Science and Technology,Shijiazhuang 050018,China)

机构地区：[1]河北科技大学化学与制药工程学院,石家庄050018

出　　处：《粉末冶金技术》2025年第1期61-70,共10页Powder Metallurgy Technology

基　　金：河北省高等学校科学技术研究重点项目(ZD2021320)。

摘　　要：以硅粉为原料,采用直接氮化法制备高品质氮化硅陶瓷粉体,研究了氮化温度、升温速率、硅粉粒径及稀释剂用量对氮化硅陶瓷粉体的影响。结果表明,原料硅粉不添加稀释剂,反应温度为1400℃时,在1100~1400℃温度区间将升温速率控制在5℃·min^(−1),硅粉完全氮化,制备得到粒径均匀的(396~458 nm)类球状氮化硅材料,材料分散性好,α相质量分数高达95.02%。研究表明,随着氮化温度的升高,硅粉直接氮化反应呈现出明显的阶段性。在相同反应时间下,最佳氮化温度为1400℃,反应温度过高或过低都会影响硅粉界面α-Si_(3)N_(4)向β-Si_(3)N_(4)转变与内部氮化反应的竞争关系,影响α-Si_(3)N_(4)含量。升温速率为控制反应进程的关键因素,最佳升温速率为5℃·min^(−1),当升温速率过快或者过慢时,氮化硅α相到β相的转化程度超过内部反应程度,硅粉反应不完全。适宜的球磨时间能够减小原料硅粉的粒度,增加比表面积,同时增加硅粉与氮气接触面积,有利于提高氮化率,增加α-Si_(3)N_(4)质量分数。添加α-Si_(3)N_(4)粉末稀释剂能降低硅粉中的氧含量和氮化温度,加速氮化过程,促进产物中α-Si_(3)N_(4)的形成,还能吸收硅和氮之间反应释放的额外热量,起到受热体的作用。High-quality silicon nitride ceramic powders were prepared by direct nitriding method with silicon powders as the raw materials.The effects of nitriding temperature,heating rate,particle size of silicon powders,and dosage of diluent on the silicon nitride ceramic powders were studied.In the results,when the reaction temperature is 1400℃and the heating rate is controlled at 5℃·min^(−1) during 1100~1400℃,the raw silicon powders without the Si_(3)N_(4) diluent are completely nitrided,the spherical silicon nitride materials with the uniform particle size(396~458 nm)and good dispersion are prepared,and the mass fraction of theαphase is 95.02%.The results show that,with the increase of nitriding temperature,the direct nitriding reaction of silicon powders shows an obvious stage.At the same reaction time,the best nitriding temperature is 1400℃,too high or too low reaction temperature could affect the competitive relationship between the transition fromα-Si_(3)N_(4) toβ-Si_(3)N_(4) at the silicon powder interface and the internal nitriding reaction,affecting the content ofα-Si_(3)N_(4).The heating rate is the key factor to control the reaction process,and the optimal heating rate is 5℃·min^(−1).When the heating rate is too fast or too slow,the transformation degree of silicon nitride fromαphase toβphase exceeds the internal reaction degree,and the silicon powder reaction is incomplete.The suitable milling time can reduce the particle size of raw silicon powders,increase the specific surface area,and increase the contact area between silicon powders and nitrogen,which can improve the nitriding rate and increase the mass fraction ofα-Si_(3)N_(4).The addition ofα-Si_(3)N_(4) diluent can reduce the oxygen content and nitriding temperature of silicon powders,accelerate the nitriding process,and promote the formation ofα-Si_(3)N_(4) in the product.It can also absorb the additional heat released by the reaction between silicon and nitrogen,and mainly plays the role of heating body in the direct nitridin

关 键 词：氮化硅 直接氮化法 陶瓷粉体 升温速率 α-Si_(3)N_(4) 

分 类 号：TF123[冶金工程—粉末冶金] TB321[冶金工程—冶金物理化学]