稀土氧化物热障涂层陶瓷材料的缺陷化学及热物理性能
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摘要
随着热能发动机的发展,对热障涂层陶瓷层材料的性能要求越来越高,传统的Y2O3稳定的ZrO_2(YSZ)材料已经很难满足这种需求,研发综合性能更加优异的新一代热障涂层陶瓷材料具有重要的现实意义和应用价值。本论文以综合性能比较好的稀土氧化物陶瓷材料为研究对象,通过掺杂、非化学计量比、稀土元素替代、成分设计等方法和手段,研究了材料晶体结构以及各种点缺陷对材料热物理性能的影响,为新型热障涂层陶瓷材料的选择与性能调控打下了基础。主要研究内容如下:
以焦绿石结构稀土锆酸盐为研究对象,研究了二价元素掺杂对Sm_2Zr_2O_7热物理性能的影响。结果显示,掺杂MgO可以在小幅提高Sm_2Zr_2O_7材料热导率的情况下,显著改善其热膨胀性能,平均热膨胀系数最高可达11.94×10-6 K~(-1)(室温~1000℃)。通过分析固溶体的拉曼光谱、点阵参数、X射线光电子能谱以及实测密度,提出并确认了一种不同于之前研究的涉及多种点缺陷和一个机理转变点的固溶模型,并解释了材料热物理性能的变化。
以焦绿石/萤石相区的SmO_(1.5)-ZrO_2体系固溶体为研究对象,研究了非化学计量比对材料晶体结构、缺陷类型以及热物理性能方面的影响。研究表明,非化学计量比同时降低了材料的热导率和热膨胀系数,其中,0.55 SmO_(1.5)·0.45ZrO_2具有最好的综合性能。该体系拉曼光谱的分析提供了萤石/焦绿石结构转变的重要信息,并为焦绿石结构拉曼光谱振动模式分析提供了有力的证据支持。
研究了具有稳定焦绿石结构的稀土锡酸盐体系的晶体结构和热物理性能,发现其1000℃下的热导率为1.9~2.3W/(m·K),平均热膨胀系数在8.3~9.3×10-6K-1之间(30~1000℃)。极限热导率计算认为,其热导率还有较大的下降空间。
首次研究了成分容忍度高的磷灰石结构稀土硅酸盐的热物理性能。通过材料成分设计的方法,在材料中引入了多种点缺陷,研究了不同点缺陷种类与浓度对材料热导率的影响。测试结果表明,该体系化合物具有基本不随温度变化的极低的热导率,阴阳离子空位浓度的增大可以进一步降低材料的热导率,而氧离子间隙对材料热导率的影响不大。
With the development of heat engines, there is a growing demand for a better performance of the ceramic top-coat in thermal barrier coatings (TBCs) whereas conventional yttria-stabilized zirconia (YSZ) ceramics can not meet the demand any more. Thus it is integral to identify novel materials with better combination property for the next generation thermal barrier coating applications. In this dissertation, several rare-earth oxides series ceramics were identified and the effect of crystal structure and point defects on the thermophysical properties of materials was investigated by means of doping, nonstoichiometry, substitution of rare earth ions and composition design, which is crucial to the materials selection and properties tailoring.
Alkaline earth ions doping was carried out to tailor the thermophysical properties of rare-earth zirconate Sm_2Zr_2O_7. The results show that the thermal expansion coefficient of material is remarkably increased through MgO doping with a maximum value around 11.94×10~(-6) K~(-1) (RT~1000℃) though there is a slight increase in thermal conductivity. A new solid-solution model that is different from previous research was proposed and confirmed by analyzing the variation of the Raman spectroscopy, lattice parameters, X-ray photoelectron spectroscopy, and experimental density of samples. It involves various kinds of point defects and a turning point in solid solution mechanism, which may be responsible for the variation of the thermophysical properties.
The solid solutions of SmO_(1.5)-ZrO_2 system in pyrochlore/fluorite phase region were identified and the effect of nonstoichiometry on the crystal structure, defect species and thermlphysical properties was investigated. It has been shown that the thermal conductivity and thermal expansion coefficient decrease simultaneously with the nonstoichiometry. Sample with composition of 0.55 SmO_(1.5)·0.45ZrO_2 turns out to be the one with best combination property, that is, low thermal conductivity and relative high thermal expansion coefficient. Moreover, the Raman spectra of this system provide some important information of fluorite/pyrochlore phase transformation and experimental evidence for the assignments of vibration modes.
The crystal structure and thermophysical properties of rare-earth stannate pyrochlores were also investigated. The experimental data of thermal conductivity and average thermal expansion coefficient of rare-earth stannates are 1.9~2.3 W/(m·K) and 8.3~9.3×10-6 K~(-1) (30~1000℃), respectively. The minimum thermal conductivity calculated by Clarke model shows that there is a possibility to reduce the thermal conductivity further.
The thermal conductivities of rare-earth silicates with apatite structure which shows a good composition tolerance were studied for the first time. Various kinds of point defects were introduced into the crystal through composition design, and the effect of defect species and concentration on the thermal conductivity was investigated. These compounds show a very low and almost temperature-independent thermal conductivity. The increase of cation and anion vacancies in crystal further reduces the thermal conductivity while oxygen interstitial ions exhibit no remarkable influence.
以焦绿石结构稀土锆酸盐为研究对象,研究了二价元素掺杂对Sm_2Zr_2O_7热物理性能的影响。结果显示,掺杂MgO可以在小幅提高Sm_2Zr_2O_7材料热导率的情况下,显著改善其热膨胀性能,平均热膨胀系数最高可达11.94×10-6 K~(-1)(室温~1000℃)。通过分析固溶体的拉曼光谱、点阵参数、X射线光电子能谱以及实测密度,提出并确认了一种不同于之前研究的涉及多种点缺陷和一个机理转变点的固溶模型,并解释了材料热物理性能的变化。
以焦绿石/萤石相区的SmO_(1.5)-ZrO_2体系固溶体为研究对象,研究了非化学计量比对材料晶体结构、缺陷类型以及热物理性能方面的影响。研究表明,非化学计量比同时降低了材料的热导率和热膨胀系数,其中,0.55 SmO_(1.5)·0.45ZrO_2具有最好的综合性能。该体系拉曼光谱的分析提供了萤石/焦绿石结构转变的重要信息,并为焦绿石结构拉曼光谱振动模式分析提供了有力的证据支持。
研究了具有稳定焦绿石结构的稀土锡酸盐体系的晶体结构和热物理性能,发现其1000℃下的热导率为1.9~2.3W/(m·K),平均热膨胀系数在8.3~9.3×10-6K-1之间(30~1000℃)。极限热导率计算认为,其热导率还有较大的下降空间。
首次研究了成分容忍度高的磷灰石结构稀土硅酸盐的热物理性能。通过材料成分设计的方法,在材料中引入了多种点缺陷,研究了不同点缺陷种类与浓度对材料热导率的影响。测试结果表明,该体系化合物具有基本不随温度变化的极低的热导率,阴阳离子空位浓度的增大可以进一步降低材料的热导率,而氧离子间隙对材料热导率的影响不大。
With the development of heat engines, there is a growing demand for a better performance of the ceramic top-coat in thermal barrier coatings (TBCs) whereas conventional yttria-stabilized zirconia (YSZ) ceramics can not meet the demand any more. Thus it is integral to identify novel materials with better combination property for the next generation thermal barrier coating applications. In this dissertation, several rare-earth oxides series ceramics were identified and the effect of crystal structure and point defects on the thermophysical properties of materials was investigated by means of doping, nonstoichiometry, substitution of rare earth ions and composition design, which is crucial to the materials selection and properties tailoring.
Alkaline earth ions doping was carried out to tailor the thermophysical properties of rare-earth zirconate Sm_2Zr_2O_7. The results show that the thermal expansion coefficient of material is remarkably increased through MgO doping with a maximum value around 11.94×10~(-6) K~(-1) (RT~1000℃) though there is a slight increase in thermal conductivity. A new solid-solution model that is different from previous research was proposed and confirmed by analyzing the variation of the Raman spectroscopy, lattice parameters, X-ray photoelectron spectroscopy, and experimental density of samples. It involves various kinds of point defects and a turning point in solid solution mechanism, which may be responsible for the variation of the thermophysical properties.
The solid solutions of SmO_(1.5)-ZrO_2 system in pyrochlore/fluorite phase region were identified and the effect of nonstoichiometry on the crystal structure, defect species and thermlphysical properties was investigated. It has been shown that the thermal conductivity and thermal expansion coefficient decrease simultaneously with the nonstoichiometry. Sample with composition of 0.55 SmO_(1.5)·0.45ZrO_2 turns out to be the one with best combination property, that is, low thermal conductivity and relative high thermal expansion coefficient. Moreover, the Raman spectra of this system provide some important information of fluorite/pyrochlore phase transformation and experimental evidence for the assignments of vibration modes.
The crystal structure and thermophysical properties of rare-earth stannate pyrochlores were also investigated. The experimental data of thermal conductivity and average thermal expansion coefficient of rare-earth stannates are 1.9~2.3 W/(m·K) and 8.3~9.3×10-6 K~(-1) (30~1000℃), respectively. The minimum thermal conductivity calculated by Clarke model shows that there is a possibility to reduce the thermal conductivity further.
The thermal conductivities of rare-earth silicates with apatite structure which shows a good composition tolerance were studied for the first time. Various kinds of point defects were introduced into the crystal through composition design, and the effect of defect species and concentration on the thermal conductivity was investigated. These compounds show a very low and almost temperature-independent thermal conductivity. The increase of cation and anion vacancies in crystal further reduces the thermal conductivity while oxygen interstitial ions exhibit no remarkable influence.
引文
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