高能球磨-盐辅助氮化低温合成α-Si_3N_4粉体
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摘要
以硅粉为原料,NaCl-NaF复合盐为反应介质和稀释剂,采用高能球磨-盐辅助氮化法制备出α-Si_3N_4粉体。研究了氮化温度、保温时间、盐硅比及复合盐中NaF含量对合成α-Si_3N_4的影响。利用X射线衍射仪(XRD)和场发射扫描电子显微镜(FE-SEM)对产物的物相组成和显微结构进行了分析表征。结果表明:氮化温度为1 200℃、保温时间为4 h、盐硅比为2∶1、复合盐中NaF含量为10%时,硅粉完全氮化。合成的产物中存在大量的α-Si_3N_4晶须,晶须的直径为40～280 nm,长度为几微米到几十微米;晶须的生长机制为VC机制。
α-Si_3N_4 powders were synthesized by a method combined high-energy ball milling with salt-assisted nitridation using silicon powders as raw materials,and Na Cl-NaF as reaction medium and diluents. The effects of nitridation temperature,holding time,salt/silicon ratio and Na F content( with in Na Cl+Na F) on the formation of α-Si_3N_4 were investigated. The phase composition and microstructure of the samples were analysed and characterized by XRD and FE-SEM. The results showed that the complete nitridation of silicon powders can be achieved at salt/silicon ratio of 2 ∶1 and Na F content of 10% after a 1 200 ℃ and 4 h heat treatment. The formation of α-Si_3N_4 whiskers with 40—280 nm in diameter and several microns to tens of microns in length was observed in the final products. The crystal growth process of α-Si_3N_4 whiskers follows vapor-crystal( VC) mechanism.
α-Si_3N_4 powders were synthesized by a method combined high-energy ball milling with salt-assisted nitridation using silicon powders as raw materials,and Na Cl-NaF as reaction medium and diluents. The effects of nitridation temperature,holding time,salt/silicon ratio and Na F content( with in Na Cl+Na F) on the formation of α-Si_3N_4 were investigated. The phase composition and microstructure of the samples were analysed and characterized by XRD and FE-SEM. The results showed that the complete nitridation of silicon powders can be achieved at salt/silicon ratio of 2 ∶1 and Na F content of 10% after a 1 200 ℃ and 4 h heat treatment. The formation of α-Si_3N_4 whiskers with 40—280 nm in diameter and several microns to tens of microns in length was observed in the final products. The crystal growth process of α-Si_3N_4 whiskers follows vapor-crystal( VC) mechanism.
引文
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21 Ge Y, Wang Q, Cui W, et al. Journal of the American Ceramic Society,2015,98(10),3398.
2 Klemm H. Journal of the American Ceramic Society,2010,93(6),1501.
3 Krstic Z, Krstic V D. Journal of Materials Science,2012,47(2),535.
4 Zhu X, Sakka Y. Science & Technology of Advanced Materials,2008,9(3),033001.
5 Li Yawei, Zang Xin, Tian Haibin, et al. Bulletin of the Chinese Ceramic Society,2003,22(1),30(in Chinese).李亚伟,张忻,田海兵,等.硅酸盐通报,2003,22(1),30.
6 Vlasova M V, Bartnitskaya T S, Sukhikh L L, et al. Journal of Materials Science,1995,30(20),5263.
7 Chen Yixiang, Li Jiangtao, Du Jisheng. Materials Research Bulletin,2008,43(6),1598.
8 Bi Yuhui, Cheng Fei, Li Jun, et al. Journal of Wuhan University of Technology,2007,29(2),8(in Chinese).毕玉惠,陈斐,李君,等.武汉理工大学学报,2007,29(2),8.
9 Kijima K, Setaka N, Tanaka H. Journal of Crystal Growth,1974,24(10),183.
10 Ding J, Deng C, Yuan W, et al. Ceramics International,2013,39(3),2995.
11 Ding J, Zhu H, Li G, et al. Ceramics International,2016,42(2),2892.
12 Chai Z, Ding J, Deng C, et al. Advanced Powder Technology,2016,27(4),1637.
13 Tian Lang, Liang Feng, Zhang Jiefeng, et al. Journal of Ceramics,2017,38(3),352(in Chinese).田亮,梁峰,张杰峰,等.陶瓷学报,2017,38(3),352.
14 Liu J, Ding J, Zhu H, et al. Journal of the Ceramic Society of Japan,2017,125(3),155.
15 Kameshima Y, Irie M, Yasumori A, et al. Solid State Ionics,2004,172(1),185.
16 Ren K G, Chen K X, Zhou H P, et al. Key Engineering Materials,2008,368-372,862.
17 Liu Xinkuan, Ma Mingliang. Journal of the Chinese Ceramic Society,2000,28(5)468(in Chinese).刘新宽,马明亮.硅酸盐学报,2000,28(5),468.
18 Huang Juntong, Zhang Shaowei, Huang Zhaohui, et al. Ceramics International,2014,40(7),11063.
19 Gu Y, Lu L, Zhang H, et al. Journal of the American Ceramic Society,2015,98(6),1762.
20 Campos-Loriz D, Howlett S P, Riley F L, et al. Journal of Materials Science,1979,14(10),2325.
21 Ge Y, Wang Q, Cui W, et al. Journal of the American Ceramic Society,2015,98(10),3398.