Synthesis of refractory silicon nitride using liquid phase with high nitrogen content

高氮液相合成难熔氮化硅

• 批准号: 15360355
• 负责人: HIROSAKI Naoto
• 金额: $ 9.66万
• 依托单位: National Institute for Materials Science
• 依托单位国家: 日本
• 项目类别: Grant-in-Aid for Scientific Research (B)
• 财政年份: 2003
• 资助国家: 日本
• 起止时间: 2003 至 2005
• 项目状态: 已结题
• 来源: https://kaken.nii.ac.jp/grant/KAKENHI-PROJECT-15360355/
• 关键词: gas turbine; silicon nitride; grain-boundary base; high-temperature strength; oxidation; creep; high-temperature deformation; rare earth; 結晶化; 希土類元素; ルテチウム; 耐熱性; 窒化物; ガス圧焼結; 液相焼結; 状態図; 構造解析

Silicon nitride sintered material in which the grain boundary phase crystallized as Lu-containing oxynitride found to have the excellent high-temperature properties. By reduction and crystallization of the intergranular glassy phase, further improvement is expected. As a result of examining the phase relationships in detail, we found that the grain boundary composition was controlled as Lu_4Si_2O_7N_2 using the liquid phase with high nitrogen content. New silicon nitride was fabricated using high nitrogen content liquid phase in the Si_3N_4-LuN-Lu_2O_3 system.Pure lutetium nitride LuN), indispensable for high nitrogen content liquid phases, was synthesized. Lu metal was directly nitrided by gas-pressure sintering. Using this LuN, Si_3N_4-Lu_2O_3-LuN reaction root was designed for a new high-nitrogen content phase in Lu-Si-O-N quaternary system, and the phase relationship and the crystal structure was refined by X-ray analysis. Finally, we fabricate the silicon nitride ceramics with Lu-oxynitride grain boundary phase by the addition of small amount of Lu_2O_3 and by gas-pressure hot-pressing. This material showed excellent strength, oxidation resistance, high-fracture toughness and creep resistance at 1500 ℃ during 1400 h under 137 MPa tensile stress.

发现其中晶界相结晶为含Lu的氮氧化物的氮化硅烧结材料具有优异的高温性能。通过晶间玻璃相的还原和结晶，有望得到进一步的改善。详细研究了相关系的结果发现，采用高氮液相时，晶界成分被控制为Lu_4Si_2O_7N_2。在Si_3N_4-LuN-Lu_2 O_3体系中，采用高氮液相法制备了新型氮化硅，合成了高氮液相法所必需的纯氮化镥（LuN）。采用气压烧结法对金属Lu进行了直接氮化处理。利用该LuN，设计了Si_3N_4-Lu_2O_3-LuN反应根，作为Lu-Si-O-N四元体系中的一种新的高氮相，并通过X射线衍射分析确定了其相关系和晶体结构。最后，通过添加少量Lu_2O_3和气压热压法制备了具有Lu-Oxide晶界相的氮化硅陶瓷。该材料在1500 ℃、137 MPa的拉伸应力作用下，经1400 h的高温拉伸后，具有良好的强度、抗氧化性、断裂韧性和抗蠕变性能。

项目成果

High-Temperature Properties of Silicon Nitride with Lu-Si-O-N Grain Boundary Phases

Lu-Si-O-N晶界相氮化硅的高温性能

• 发表时间: 2006
• 期刊: Key Eng. Mat. 317-318
• 作者: Norio Tsubokawa;坪川紀夫;Norio Tsubokawa;Norio Tsubokawa;N.Tsubokawa;N.Tsubokawa;N.Tsubokawa;Y.Yamamoto
• 通讯作者: Y.Yamamoto

Microstructual characterization and high-temperature strength of hot-pressed silicon nitride ceramics with Lu_2O_3 additives

Lu_2O_3添加剂热压氮化硅陶瓷的微观结构表征及高温强度

• 发表时间: 2003
• 期刊: Pill. Mag. Lett. 83・6
• 作者: S.Guo;N.Hirosaki et al.;S.Guo
• 通讯作者: S.Guo

S.Guo, N.Hirosaki, et al.: "Microstructural characterization and high-temperature strength of hot-pressed silicon nitride ceramics with Lu2O3 additives"Philosophical Magazine Letters. 83・6. 357-365 (2003)

S.Guo、N.Hirosaki 等：“含 Lu2O3 添加剂的热压氮化硅陶瓷的微观结构表征和高温强度”哲学杂志快报 83・6 (2003)。

Hot-pressed Si3N4 ceramics with Lu2O3 additives: Grain-boundary phase and strength

• DOI: 10.1016/j.msea.2005.05.025
• 发表时间: 2005-11
• 期刊: Materials Science and Engineering A-structural Materials Properties Microstructure and Processing
• 影响因子: 6.4
• 作者: Shuqi Guo;N. Hirosaki;Yoshinobu Yamamoto;T. Nishimura;Y. Kagawa

Compressive creep behaviour of Yb_4Si_2O_7N_2 containing silicon nitride ceramic between 1400 and 1500 ℃

含氮化硅陶瓷Yb_4Si_2O_7N_2在1400~1500 ℃时的压缩蠕变行为

• 发表时间: 2003
• 期刊: Mater. Sci, Technol. 19・4
• 作者: S.Guo;N.Hirosaki et al.;S.Guo;J.Takahashi;S.Guo;S.Guo
• 通讯作者: S.Guo