新型快速微波烧结微观机理的同步辐射在线实验研究
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摘要
微波烧结是一种优于常规烧结的新型材料快速制备技术,研究微波烧结机理具有重要的理论和实际意义。本文首先阐述了对微波烧结微结构演化进行同步辐射CT(简称"SR-CT")在线观测的必要性和重要性。依此,通过对研制核心设备所存在技术难题的分析和解决,成功构建了一套SR-CT技术专用的微波烧结在线实验系统。基于该实验系统,分别开展了金属和陶瓷单一材料体系,以及金属-陶瓷混合体系微波烧结的SR-CT在线实验,研究了各自的微波烧结微结构演化特征及相应的微观烧结机理。最后,结合本文实验研究结果,对微波的“热效应”和“非热效应”做了进一步的讨论和分析。本文的主要研究内容和创新之处是：
一、构建了一套同步辐射CT专用的微波烧结在线实验系统,实现了快速微波烧结微结构演化的同步辐射CT在线观测,最高分辨率达亚微米量级。目前,国际上尚未见到与该实验系统相似的报道。
1)分体式结构设计解决了高衬度、高分辨率SR-CT实验平台的空间限制；
2)多维精密电控旋转台可实现高温微波场中样品精确定位和高精度旋转,这对于开展多场耦合或极端条件下高分辨率SR-CT实验具有积极意义；
3)特制的双重保温结构有效解决了小样品在不完全密闭环境中的通光、保温、测温及气氛保护等问题,为拓展该实验系统应用范围提供技术保障。
二、首次实现了金属、陶瓷等单一体系以及金属-陶瓷混合体系微波烧结SR-CT在线实验研究。观察到诸多不同于常规烧结的表面和界面快速演化现象,定量分析表明微波烧结与常规烧结具有不同的加热特性和物质扩散机制。
1)实现了金属、陶瓷以及金属-陶瓷混合材料在微波烧结过程中微结构演化的SR-CT在线实验,观测到了诸多不同于常规烧结的特殊烧结现象,并从微波“热效应”和“非热效应”等角度对这些现象进行了机理解释；
2)通过B样条插值方法提取了颗粒表面曲率参数,统计和分析了混合体系以及纯金属颗粒表面弯曲能的变化规律,结果表明,微波电磁场与材料的耦合机制与材料的物性密切相关,微波磁场有利于金属颗粒表面弯曲能的降低；
3)利用分水岭算法获得了金属、陶瓷以及金属-陶瓷混合材料的颈长动力学曲线,分析了各自的物质主导扩散机制和相应的微观机理,结果表明微波烧结与常规烧结的物质扩散机制不同,且不同材料之间也存在不同。此外,研究了微波与不同材料体系内部颗粒表面和界面的耦合机制,结果表明当陶瓷加入金属以后,微波将在混合体系中将引起界面极化,从而促进体系的加热。
三、探索了微波电磁场强度分布、传播方向以及材料微观构型等因素可能引起的“热效应”和“非热效应”,分析表明这些效应将促进物质扩散进程,并引起各向异性烧结。
1)在微波的“热效应”方面,主要分析了微波电场和磁场强度的不均匀分布,以及材料的微观构型对烧结进程可能产生的促进作用；
2)在微波的“非热效应”方面,主要分析了微波电场和磁场的方向以及材料的微观构型可能导致的各向异性烧结现象。
最后,对全文的工作进行了总结,给出了本文的主要研究内容和结果,并对需要进一步深入研究的课题提出了研究思路和方案。
Microwave sintering is a novel rapid material preparation method which is superior to the conventional sintering. It has important practical and theoretical significance to study the microwave sintering mechanism. In this paper, the importance and necessity of carrying out the SR-CT online observation of the microstructure evolution during microwave sintering was represented. According to this, a set of SR-CT technology based microwave sintering analyze system was successfully built. Depending on this system, the SR-CT experimental study on the microwave sintering of metal, ceramic and metal-ceramic hybrid materials were carried out. The microstructure evolution characteristics and the corresponding sintering mechanisms of these materials were analyzed by the comparison between different materials, as well as the microwave sintering and conventional sintering. Finally, the further discussion of the "thermal effects" and "non-thermal effects" of microwave were carried out. The main content and the innovation of this paper are:
Firstly, a new synchrotron radiation CT technology-based microwave sintering experimental system was built. The online observation of microstructure evolution during the fast microwave sintering by the synchrotron radiation CT technique was realized. The highest resolution reached submicron. At present, the news about such experimental system has not been reported.
1. The separated structure resolves the problem of the space limitation of the high contrast, high-resolution SR-CT experiment platform;
2. The multi-dimensional precision electronic control rotary device can realize the high precise of positioning and rotation of the sample in the high-temperature microwave field, which has positive significance for conducting the SR-CT experiment under multi-field coupling or extreme conditions;
3. The specially designed double insulation structure resolved the problem of light-through, heat insulation, temperature measurement and atmosphere protection. This provides technical support for expanding the application scope of this analytical system.
Secondly, the first SR-CT experimental study on metals, ceramics and metal-ceramic hybrid materials were realized. The special sintering phenomena and the corresponding sintering kinetics mechanisms were analyzed. The quantitative analysis showed that there were different sintering dominate mass diffusion mechanisms between microwave and conventional sintering.
1. The SR-CT online experiments and observations on the microstructure evolution of metals, ceramics, and metal-ceramic mixed materials in the microwave sintering were achieved. Various special sintering phenomena that were different from the conventional sintering were observed. The explanation for these phenomena was given from the aspects of "thermal effect" and "non-thermal effect" of the microwave;
2. The statistics and analysis of the variation of particle surface bending energy of the hybrid system and the pure metal were carried out by adopting the method of B-spline interpolation. The results indicated that coupling mechanism of "microwave-material" is related to the property of materials, the microwave field is good for the decrease of particle surface bending energy.
3. The watershed algorithm was used to extract the sintering-neck of metals, ceramics and metal-ceramic hybrid materials, and the sintering-neck growth kinetic curves were obtained. Then, the dominant diffusion mechanism and the corresponding microscopic mechanism were analyzed. The results show that there were dominate mass diffusion mechanisms between microwave and conventional sintering, as well as between the different materials. In addition, the study of the coupling mechanism between microwave and the surface and interface of different material systems, it was shown that the addition of ceramic materials will induce interfacial polarization, which will promote the sintering process.
In addition, the "thermal effects" and "non-thermal effects" that were in connection with the intensity distribution and propagation direction of microwave were further analyzed. The result indicated that these effects will promote the mass diffusion process and induce anisotropic sintering.
1. As in the aspect of "thermal effects", the main analysis was on the promotion of sintering process induced by the uneven distribution of the microwave electric field and magnetic field, as well as the microscopic configuration of the material;
2. As in the aspect of "non-thermal effects", the main analysis was on the anisotropic sintering which has relation with the direction of microwave electric field and magnetic field, as well as the microscopic configuration of the material.
Finally, a summary of the full text was made, the main research contents and results were given, and the research ideas and programs for the problems which need further in-depth study were raised.
一、构建了一套同步辐射CT专用的微波烧结在线实验系统,实现了快速微波烧结微结构演化的同步辐射CT在线观测,最高分辨率达亚微米量级。目前,国际上尚未见到与该实验系统相似的报道。
1)分体式结构设计解决了高衬度、高分辨率SR-CT实验平台的空间限制；
2)多维精密电控旋转台可实现高温微波场中样品精确定位和高精度旋转,这对于开展多场耦合或极端条件下高分辨率SR-CT实验具有积极意义；
3)特制的双重保温结构有效解决了小样品在不完全密闭环境中的通光、保温、测温及气氛保护等问题,为拓展该实验系统应用范围提供技术保障。
二、首次实现了金属、陶瓷等单一体系以及金属-陶瓷混合体系微波烧结SR-CT在线实验研究。观察到诸多不同于常规烧结的表面和界面快速演化现象,定量分析表明微波烧结与常规烧结具有不同的加热特性和物质扩散机制。
1)实现了金属、陶瓷以及金属-陶瓷混合材料在微波烧结过程中微结构演化的SR-CT在线实验,观测到了诸多不同于常规烧结的特殊烧结现象,并从微波“热效应”和“非热效应”等角度对这些现象进行了机理解释；
2)通过B样条插值方法提取了颗粒表面曲率参数,统计和分析了混合体系以及纯金属颗粒表面弯曲能的变化规律,结果表明,微波电磁场与材料的耦合机制与材料的物性密切相关,微波磁场有利于金属颗粒表面弯曲能的降低；
3)利用分水岭算法获得了金属、陶瓷以及金属-陶瓷混合材料的颈长动力学曲线,分析了各自的物质主导扩散机制和相应的微观机理,结果表明微波烧结与常规烧结的物质扩散机制不同,且不同材料之间也存在不同。此外,研究了微波与不同材料体系内部颗粒表面和界面的耦合机制,结果表明当陶瓷加入金属以后,微波将在混合体系中将引起界面极化,从而促进体系的加热。
三、探索了微波电磁场强度分布、传播方向以及材料微观构型等因素可能引起的“热效应”和“非热效应”,分析表明这些效应将促进物质扩散进程,并引起各向异性烧结。
1)在微波的“热效应”方面,主要分析了微波电场和磁场强度的不均匀分布,以及材料的微观构型对烧结进程可能产生的促进作用；
2)在微波的“非热效应”方面,主要分析了微波电场和磁场的方向以及材料的微观构型可能导致的各向异性烧结现象。
最后,对全文的工作进行了总结,给出了本文的主要研究内容和结果,并对需要进一步深入研究的课题提出了研究思路和方案。
Microwave sintering is a novel rapid material preparation method which is superior to the conventional sintering. It has important practical and theoretical significance to study the microwave sintering mechanism. In this paper, the importance and necessity of carrying out the SR-CT online observation of the microstructure evolution during microwave sintering was represented. According to this, a set of SR-CT technology based microwave sintering analyze system was successfully built. Depending on this system, the SR-CT experimental study on the microwave sintering of metal, ceramic and metal-ceramic hybrid materials were carried out. The microstructure evolution characteristics and the corresponding sintering mechanisms of these materials were analyzed by the comparison between different materials, as well as the microwave sintering and conventional sintering. Finally, the further discussion of the "thermal effects" and "non-thermal effects" of microwave were carried out. The main content and the innovation of this paper are:
Firstly, a new synchrotron radiation CT technology-based microwave sintering experimental system was built. The online observation of microstructure evolution during the fast microwave sintering by the synchrotron radiation CT technique was realized. The highest resolution reached submicron. At present, the news about such experimental system has not been reported.
1. The separated structure resolves the problem of the space limitation of the high contrast, high-resolution SR-CT experiment platform;
2. The multi-dimensional precision electronic control rotary device can realize the high precise of positioning and rotation of the sample in the high-temperature microwave field, which has positive significance for conducting the SR-CT experiment under multi-field coupling or extreme conditions;
3. The specially designed double insulation structure resolved the problem of light-through, heat insulation, temperature measurement and atmosphere protection. This provides technical support for expanding the application scope of this analytical system.
Secondly, the first SR-CT experimental study on metals, ceramics and metal-ceramic hybrid materials were realized. The special sintering phenomena and the corresponding sintering kinetics mechanisms were analyzed. The quantitative analysis showed that there were different sintering dominate mass diffusion mechanisms between microwave and conventional sintering.
1. The SR-CT online experiments and observations on the microstructure evolution of metals, ceramics, and metal-ceramic mixed materials in the microwave sintering were achieved. Various special sintering phenomena that were different from the conventional sintering were observed. The explanation for these phenomena was given from the aspects of "thermal effect" and "non-thermal effect" of the microwave;
2. The statistics and analysis of the variation of particle surface bending energy of the hybrid system and the pure metal were carried out by adopting the method of B-spline interpolation. The results indicated that coupling mechanism of "microwave-material" is related to the property of materials, the microwave field is good for the decrease of particle surface bending energy.
3. The watershed algorithm was used to extract the sintering-neck of metals, ceramics and metal-ceramic hybrid materials, and the sintering-neck growth kinetic curves were obtained. Then, the dominant diffusion mechanism and the corresponding microscopic mechanism were analyzed. The results show that there were dominate mass diffusion mechanisms between microwave and conventional sintering, as well as between the different materials. In addition, the study of the coupling mechanism between microwave and the surface and interface of different material systems, it was shown that the addition of ceramic materials will induce interfacial polarization, which will promote the sintering process.
In addition, the "thermal effects" and "non-thermal effects" that were in connection with the intensity distribution and propagation direction of microwave were further analyzed. The result indicated that these effects will promote the mass diffusion process and induce anisotropic sintering.
1. As in the aspect of "thermal effects", the main analysis was on the promotion of sintering process induced by the uneven distribution of the microwave electric field and magnetic field, as well as the microscopic configuration of the material;
2. As in the aspect of "non-thermal effects", the main analysis was on the anisotropic sintering which has relation with the direction of microwave electric field and magnetic field, as well as the microscopic configuration of the material.
Finally, a summary of the full text was made, the main research contents and results were given, and the research ideas and programs for the problems which need further in-depth study were raised.
引文
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