Al_2O_3/ZrO_2/YAG共晶陶瓷的制备及组织特征
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摘要
氧化物共晶陶瓷具有高强度、耐高温、耐氧化、高抗蠕变等优异性能,是高温氧化气氛下长期工作的优选超高温结构材料,其组织热稳定性好,使用温度可达1600～1700℃。现有共晶陶瓷制备技术中只有布里奇曼法适合制备较大尺寸的共晶陶瓷块体,但其生长速度慢,材料微观组织粗大、强度低；而其它技术制备的材料通常在毫米级以下。从工艺制备角度上,温度梯度、生长速度和微观尺寸之间内在关系限制了共晶陶瓷的加工制备。因此,如何同时实现较大尺寸样品的制备和微观组织控制,是制约共晶陶瓷进一步发展和结构件工程化应用的重要瓶颈。
本文以Al2O3/ZrO2(YSZ)/YAG共晶陶瓷为研究对象,采用温度梯度适中的高温熔凝工艺(适合制备大块共晶陶瓷材料),通过调整工艺参数改变熔体的凝固路径和晶体生长速度,实现了较大尺寸共晶陶瓷的制备及其凝固组织的优化与控制。研究了凝固组织的变化规律,并运用凝固原理中经典形核机制和Jackson-Hunt共晶生长模型,探讨了凝固组织的演变机理。主要结果如下：
通过提高熔体冷却速度,制备出组织细小的Al2O3/ZrO2/YAG共晶陶瓷块体,微观组织的特征尺寸细化到亚微米级。随着冷却速度增加,凝固体中依次出现三种典型的显微组织,分别为：晶团结构、树枝晶结构和胞状结构。建立三元共晶生长晶数学模型,给出Al2O3/ZrO2/YAG共晶凝固过程中溶质过冷度、曲率过冷度和动力过冷度与晶体生长速度的关系,阐释了溶质扩散特征长度和毛细作用特征长度对固-液界面形貌的影响。
通过调控熔体温度或保温时间,制备出直径30mm的Al2O3/ZrO2/YAG共晶陶瓷块体,微观共晶层间距为350nm。采用经典异质形核理论,从熔体的晶胚分布和异质晶核点钝化角度分析了熔体温度(或保温时间)对形核过冷度和凝固组织的作用。熔体温度对凝固体组织结构的影响可以划分为三个阶段。第一阶段：随着熔体温度升高或保温时间延长,熔体中原子团簇结构衰退,熔体成分均匀化,形核过冷度增加,共晶组织细化。第二阶段：随着熔体温度升高,异质晶核点不断钝化,形核过冷度增加,共晶组织细化。第三阶段：当熔体温度超过某一临界值T。时,异质晶核点钝化严重,凝固路径改变,过冷熔体选择YAP相形核,生成Al2O3-ZrO2-YAP亚稳态复合陶瓷。
提出“压力辅助成型”工艺,制备出坩埚形状Al2O3/ZrO2/YAG共晶陶瓷构件,该工艺可以有效地消除组织内部的缩松缺陷,抑制样块表面侵蚀性气孔的生成,有利于改善材料的力学性能。
Directionally solidified eutectic oxide ceramics (DSEO) are very attractive as ultra-high-temperature structural materials with long-term service due to the excellent mechanical properties, thermal stability, creep resistance and oxidation resistance in atmosphere at high temperature. Eutectic ceramics have good microstructural stability and the application temperature can reach1600-1700℃. Among processing techniques for the eutectic oxide ceramic, only Bridgman technique with relatively modest thermal gradient is the the optimum method for the fabrication of large volume samples. However, this method implies low growth rates and consequently large interphase spacing samples with low strength. Other methods can obtain samples with finer interspacing size but the products are limited to several millimeters due to the large temperature gradients. From the processing viewpoint, the relationships among thermal gradient, growth rate and micro structure size impose limitations on the sample processing. Hence, it is a problem for eutectic ceramic processing technique that how to prepare large dimession sample and control the microstructural characteristics simultaneously, which limits the materials developing and engeering application in components.
Present investigation focuses on the above aspect of Al2O3/ZrO2/YAG searching method to prepare samples which combines large dimension as well as fine microstructure. High temperature mlet-grown method with modest thermal gradient was adopted to prepare large dimension eutectic bulk. Combining with rapid cooling or melt superheating treatment, the solidification microstructure can be optimized by controlling technological parameters which affeact the solidification path and crystal growth rate. Solidification microstructure evolutions were studied systematically and discussed in terms of the classical nucleation mechanism and Jackson-Hunt model. The primary conclusions are as follows:
By increasing the cooling rate, Al2O3/ZrO2/YAG eutectic bulks with the interspacing of microstructure in submicron level were fabricated successfully. With increasing the cooling rate, the microstructure characteristic scale of melt-grown samples decreases and the structure develops from colony to dendrite and finally to cell. The solidification Microstructure transitions were interpreted according to morphology variation of solid-liquid interfaces as a result of the interplay between solute diffusion and the curvature effects. Meanwhile, a mathematical model for ternary eutectic coupled growth was developed based on binary eutectic. With the mathematical model, solute, curvature, and kinetic undercoolings were deduced and calculated as a function of growth velocity.
By controlling melt temperature and holding time, Al2O3/ZrO2/YAG eutectic rods with30mm in diameter were produced. The solidification microstructure is homogenous and the minimum interspacing is only350nm. Making using of the classical nucleation mechanism, solidification microstructure transitions under different melt temperatures on was discussed in terms of the variations about atom clusters distribution in melts and the passivation of the heterogeneous nucleation sites, which affect the melt nucleation undercooling, solidification path and the final solidification microstructure. The melt temperature can be divided into three stages according to its role on microstructural change. The first stage:the microstructure refinement with the melt temperature increasing or with the holding time prolonging, is due to the decay of atom clusters which homogenizes the melt and makes an increase of the melt nucleation undercooling. The second stage:the higher melt temperature results in the eutectic micrsostructure further refined because of the passivation of the heterogeneous nucleation sites increasing the melt nucleation undercooling. The third stage:the melt temperature beyonds a certain crtical value Tc the melt-grown sample is Al2O3-ZrO2-YAP metastable composite because the passivation of the heterogeneous nucleation sites is serious and the YAP nucleates instead of YAG.
A method referred to as "pressure assistaned-solidification formation" was first suggested for the shape-forming of melt growth eutectic ceramics, and practically implemented for Al2O3/YAG/ZrO2composite. A component with crucible shape was prepared successfully. It was found the defects in the intercolony region and on the surface reduce dramatically, which is beneficial to improve the mechnical properties.
本文以Al2O3/ZrO2(YSZ)/YAG共晶陶瓷为研究对象,采用温度梯度适中的高温熔凝工艺(适合制备大块共晶陶瓷材料),通过调整工艺参数改变熔体的凝固路径和晶体生长速度,实现了较大尺寸共晶陶瓷的制备及其凝固组织的优化与控制。研究了凝固组织的变化规律,并运用凝固原理中经典形核机制和Jackson-Hunt共晶生长模型,探讨了凝固组织的演变机理。主要结果如下：
通过提高熔体冷却速度,制备出组织细小的Al2O3/ZrO2/YAG共晶陶瓷块体,微观组织的特征尺寸细化到亚微米级。随着冷却速度增加,凝固体中依次出现三种典型的显微组织,分别为：晶团结构、树枝晶结构和胞状结构。建立三元共晶生长晶数学模型,给出Al2O3/ZrO2/YAG共晶凝固过程中溶质过冷度、曲率过冷度和动力过冷度与晶体生长速度的关系,阐释了溶质扩散特征长度和毛细作用特征长度对固-液界面形貌的影响。
通过调控熔体温度或保温时间,制备出直径30mm的Al2O3/ZrO2/YAG共晶陶瓷块体,微观共晶层间距为350nm。采用经典异质形核理论,从熔体的晶胚分布和异质晶核点钝化角度分析了熔体温度(或保温时间)对形核过冷度和凝固组织的作用。熔体温度对凝固体组织结构的影响可以划分为三个阶段。第一阶段：随着熔体温度升高或保温时间延长,熔体中原子团簇结构衰退,熔体成分均匀化,形核过冷度增加,共晶组织细化。第二阶段：随着熔体温度升高,异质晶核点不断钝化,形核过冷度增加,共晶组织细化。第三阶段：当熔体温度超过某一临界值T。时,异质晶核点钝化严重,凝固路径改变,过冷熔体选择YAP相形核,生成Al2O3-ZrO2-YAP亚稳态复合陶瓷。
提出“压力辅助成型”工艺,制备出坩埚形状Al2O3/ZrO2/YAG共晶陶瓷构件,该工艺可以有效地消除组织内部的缩松缺陷,抑制样块表面侵蚀性气孔的生成,有利于改善材料的力学性能。
Directionally solidified eutectic oxide ceramics (DSEO) are very attractive as ultra-high-temperature structural materials with long-term service due to the excellent mechanical properties, thermal stability, creep resistance and oxidation resistance in atmosphere at high temperature. Eutectic ceramics have good microstructural stability and the application temperature can reach1600-1700℃. Among processing techniques for the eutectic oxide ceramic, only Bridgman technique with relatively modest thermal gradient is the the optimum method for the fabrication of large volume samples. However, this method implies low growth rates and consequently large interphase spacing samples with low strength. Other methods can obtain samples with finer interspacing size but the products are limited to several millimeters due to the large temperature gradients. From the processing viewpoint, the relationships among thermal gradient, growth rate and micro structure size impose limitations on the sample processing. Hence, it is a problem for eutectic ceramic processing technique that how to prepare large dimession sample and control the microstructural characteristics simultaneously, which limits the materials developing and engeering application in components.
Present investigation focuses on the above aspect of Al2O3/ZrO2/YAG searching method to prepare samples which combines large dimension as well as fine microstructure. High temperature mlet-grown method with modest thermal gradient was adopted to prepare large dimension eutectic bulk. Combining with rapid cooling or melt superheating treatment, the solidification microstructure can be optimized by controlling technological parameters which affeact the solidification path and crystal growth rate. Solidification microstructure evolutions were studied systematically and discussed in terms of the classical nucleation mechanism and Jackson-Hunt model. The primary conclusions are as follows:
By increasing the cooling rate, Al2O3/ZrO2/YAG eutectic bulks with the interspacing of microstructure in submicron level were fabricated successfully. With increasing the cooling rate, the microstructure characteristic scale of melt-grown samples decreases and the structure develops from colony to dendrite and finally to cell. The solidification Microstructure transitions were interpreted according to morphology variation of solid-liquid interfaces as a result of the interplay between solute diffusion and the curvature effects. Meanwhile, a mathematical model for ternary eutectic coupled growth was developed based on binary eutectic. With the mathematical model, solute, curvature, and kinetic undercoolings were deduced and calculated as a function of growth velocity.
By controlling melt temperature and holding time, Al2O3/ZrO2/YAG eutectic rods with30mm in diameter were produced. The solidification microstructure is homogenous and the minimum interspacing is only350nm. Making using of the classical nucleation mechanism, solidification microstructure transitions under different melt temperatures on was discussed in terms of the variations about atom clusters distribution in melts and the passivation of the heterogeneous nucleation sites, which affect the melt nucleation undercooling, solidification path and the final solidification microstructure. The melt temperature can be divided into three stages according to its role on microstructural change. The first stage:the microstructure refinement with the melt temperature increasing or with the holding time prolonging, is due to the decay of atom clusters which homogenizes the melt and makes an increase of the melt nucleation undercooling. The second stage:the higher melt temperature results in the eutectic micrsostructure further refined because of the passivation of the heterogeneous nucleation sites increasing the melt nucleation undercooling. The third stage:the melt temperature beyonds a certain crtical value Tc the melt-grown sample is Al2O3-ZrO2-YAP metastable composite because the passivation of the heterogeneous nucleation sites is serious and the YAP nucleates instead of YAG.
A method referred to as "pressure assistaned-solidification formation" was first suggested for the shape-forming of melt growth eutectic ceramics, and practically implemented for Al2O3/YAG/ZrO2composite. A component with crucible shape was prepared successfully. It was found the defects in the intercolony region and on the surface reduce dramatically, which is beneficial to improve the mechnical properties.
引文
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