细晶Si_3N_4/Al_2O_3复合陶瓷材料的制备及其力学性能的研究
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摘要
氮化硅复合陶瓷具有优良的物理、力学性能和耐磨、耐腐蚀特性，因而受到人们的广泛关注；但是该材料的脆性断裂特性依然存在，而且其机械可靠性也不尽如意，因此有必要进一步深入研究以充分发挥其性能优点。细化晶粒改善陶瓷性能是当前研究的热点。本文用热压方法制备了细晶氮化硅／氧化铝复合陶瓷，并对该材料的原料粉末的特性、烧结工艺、致密特性及力学性能进行了比较深入的实验研究和理论探讨，为下一步研究打下实验和理论基础。
首先研究了原料粉末的性能。研究发现原料粉末的团聚特性、氧吸附性对材料的烧结工艺、力学性能影响较大；对原料粉末在1200℃下进行热处理，可以使原料粉末转晶和钝化，最终烧结成细晶复合陶瓷。
其次研究了烧结温度和气氛对细晶陶瓷致密特性、力学性能的影响。随着烧结温度升高，材料的致密度上升，抗弯强度和硬度提高，但断裂韧性的变化与添加剂有关；当烧结气氛是氮气时，能有效地抑制原料粉末的分解和氧化；而当烧结气氛是氩气时，则会发生较严重的氧化现象。
再次研究了烧结添加剂种类对该材料的致密特性、力学性能的影响。随着烧结添加剂种类的增加，在相同温度下材料的致密度上升，力学性能提高。但当添加剂中氮含量升高到一定程度时就会得到相反的结果。
最后研究了烧结添加剂的数量对该材料的致密特性、力学性能的影响。随着烧结添加剂量的增加，在相同温度下材料的致密度上升，力学性能的变化与材料中的致密度、第二相粒子及晶间相有关。
SisN'-based composite ceramics have attracted attention owing to its
outstanding physical, mechanical properties and high wear-resistance, good
erosion-resistance. But the fatal brittleness still exists in these materials, and the
mechanical reliability is also low. The fine crystalline ceramics was researched
popularly at present. In this thesis, the fine-crystalline Si3N4/Al2O3 composite
ceramics were prepared by hot pressing. The phenomena including the properties of
powder, sintering process, densification and mechanical properties were discussed
by the experimented research and theoretical analysis. The experimenta1 and
theoreticaI basis has been presented for further research.
First, the research on the properties of powders was done. The results
revealed that the formation of agglomerates and the absorbed oxygen affected the
sintering process and mechanical properties of these fine-crystalline materials.
When the powders have been heat-treated at 1200C, the fine crystalline materia1s
have been obtained due to the phase transformation and thermal inactivation.
Second, the research on the effect of the sintering temperature and the
protective gas on the densification and the mechanical properties of these materials
was worked on. The higher the sintering temperature, the higher the density. the
better bend strength and hardness. but the variation of fracture toughness properties
depended on the kind of addition. When the protective gas was N2, the oxidation
and the decomposition have been pressed. But when Ar was used, the serious
oxidation has been happened.
Third, the research on the effect of the kind of addition on the densification
and the mechanical properties of these materials was conducted. Under the same
temperature, with the increase of the sort of the additions, the density and the
mechanical properties of these materials have increased. But a proper proportion of
nitrogen in the addition should been defined, otherwise, a contrary result has been
rec eived.
Last, the research on the effect of the quantity of addition on the densification
and the mechanical properties of these materials was done. Under the same
temperature, with the increase of the quantity of the additions, the density has
increased, and the variation of the mechanical properties of these materials
depended on the density and the quantities of the second-phase particle and intercrystalline phase of these materials.
首先研究了原料粉末的性能。研究发现原料粉末的团聚特性、氧吸附性对材料的烧结工艺、力学性能影响较大；对原料粉末在1200℃下进行热处理，可以使原料粉末转晶和钝化，最终烧结成细晶复合陶瓷。
其次研究了烧结温度和气氛对细晶陶瓷致密特性、力学性能的影响。随着烧结温度升高，材料的致密度上升，抗弯强度和硬度提高，但断裂韧性的变化与添加剂有关；当烧结气氛是氮气时，能有效地抑制原料粉末的分解和氧化；而当烧结气氛是氩气时，则会发生较严重的氧化现象。
再次研究了烧结添加剂种类对该材料的致密特性、力学性能的影响。随着烧结添加剂种类的增加，在相同温度下材料的致密度上升，力学性能提高。但当添加剂中氮含量升高到一定程度时就会得到相反的结果。
最后研究了烧结添加剂的数量对该材料的致密特性、力学性能的影响。随着烧结添加剂量的增加，在相同温度下材料的致密度上升，力学性能的变化与材料中的致密度、第二相粒子及晶间相有关。
SisN'-based composite ceramics have attracted attention owing to its
outstanding physical, mechanical properties and high wear-resistance, good
erosion-resistance. But the fatal brittleness still exists in these materials, and the
mechanical reliability is also low. The fine crystalline ceramics was researched
popularly at present. In this thesis, the fine-crystalline Si3N4/Al2O3 composite
ceramics were prepared by hot pressing. The phenomena including the properties of
powder, sintering process, densification and mechanical properties were discussed
by the experimented research and theoretical analysis. The experimenta1 and
theoreticaI basis has been presented for further research.
First, the research on the properties of powders was done. The results
revealed that the formation of agglomerates and the absorbed oxygen affected the
sintering process and mechanical properties of these fine-crystalline materials.
When the powders have been heat-treated at 1200C, the fine crystalline materia1s
have been obtained due to the phase transformation and thermal inactivation.
Second, the research on the effect of the sintering temperature and the
protective gas on the densification and the mechanical properties of these materials
was worked on. The higher the sintering temperature, the higher the density. the
better bend strength and hardness. but the variation of fracture toughness properties
depended on the kind of addition. When the protective gas was N2, the oxidation
and the decomposition have been pressed. But when Ar was used, the serious
oxidation has been happened.
Third, the research on the effect of the kind of addition on the densification
and the mechanical properties of these materials was conducted. Under the same
temperature, with the increase of the sort of the additions, the density and the
mechanical properties of these materials have increased. But a proper proportion of
nitrogen in the addition should been defined, otherwise, a contrary result has been
rec eived.
Last, the research on the effect of the quantity of addition on the densification
and the mechanical properties of these materials was done. Under the same
temperature, with the increase of the quantity of the additions, the density has
increased, and the variation of the mechanical properties of these materials
depended on the density and the quantities of the second-phase particle and intercrystalline phase of these materials.
引文
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[3] 师昌绪．新型材料与材料科学．北京：科学出版社，1988：2
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[10] 张立德．纳米材料研究的新进展及在 21 世纪的战略地位．中国粉体技术．2000；6(1)：1-5
[11] 潘劲松，黄学辉，顾少轩．纳米材料的类别划分及其依据．材料导报．2000；14(11)：28-29
[12] U.Betz, A.Sturm, J.F.Loffier, W. Wagner, A.Wiedenmann, H.Hahn. Microstrural development during final-stage sintering of nanostructured zirconia based ceramics. Materials Science and Engineering. 2000; A281: 68-74
[13] 赵秦生，胡海南．新材料与新能源．北京：轻工业出版社，1987
[14] Catherine L.Hewett, Yi-Bing Cheng, Barry C.Muddle. Phase Relationships and Related Microstructure Observations in the Ca-Si-Al-O-N System. J.Am. Ceram. Soc. 1998; 81(7): 1781-88
[15] C.J.Spacie, K.Liddell, D.P. Thompson. The U-phase in heat-treated Sialon ceramics. Journal of Materials Science Letters. 1988; 7:95-96
[16] Wei-Ying Sun, Tseng-Ying Tien, Tung-Sheng Yen. Subsolidus Phase Relationships in Part of the System Si, Al, Y/N, O: The System Si_3N_4-AlN-YN-Y_2O_3. J.Am. Ceram. Soc. 1991; 74(11): 2753-58
[17] Zhen-Kun Huang, Yao-Zhong Jiang, Tseng-Ying Tien. Formation of a-Sialons with dual modifying cations(Li+Y and Ca+Y). Journal of Materials Science Letters. 1997; 16:747-751
[18] Thommy Ekstrom, Lena K.L.Falk, Zhi-Jian Shen. Duplex α-β-Sialon Ceramics Stabilized by Dysprosium and Samarium. J.Am. Ceram. Soc. 1997; 80(2): 301-12
[19] 崔国文．缺陷、扩散与烧结．北京：清华大学出版社，1990
[20] 张艳丽．热压氮化硅-氧化锆复合陶瓷的研究：[硕士论文]，合肥：合肥工业大学材料科学与工程学院，1995
[21] Wei-Ying Sun, Tseng-Ying Tien, Tung-Sheng Yen. Solubility Limits of a-Sialon Solid Solution in the System Si,Al,Y/N,O. J.Am. Ceram.Soc. 1991; 74(10): 2547-50
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