陶瓷固相烧结的同步辐射CT技术研究
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摘要
本文阐述了对陶瓷固相烧结过程进行无损、实时研究的必要性和重要性,概述了陶瓷固相烧结演化过程和现象、热力学机制、理论模型和控制方程;总结了同步辐射CT(SR-CT)技术的原理以及目前国内外研究现状。在此基础上,利用相场法对陶瓷烧结过程进行了二维和三维的数值模拟,分析了利用SR-CT技术对陶瓷固相烧结过程进行实时观测的实验难点,提出了利用加窗傅立叶滤波提高SR-CT重建图像的质量的方法并进行了可行性分析,设计了实验方案,利用SR-CT技术对多种陶瓷样品固相烧结过程的微结构演化过程进行了实时的实验观测,并结合现有烧结理论和模型对实验的结果进行分析。
本文主要研究内容如下:
一、总结了固相烧结理论,对固相烧结过程的微观结构演化进行了二维和三维的数值模拟,其中三维的数值模拟目前国内尚未见到公开的报道,在国际上也仅见少数几篇报道。
1、对固相烧结过程进行了分析,探讨了关于固相烧结过程的热力学驱动力和物质传输机制以及致密化过程的一些经验方程和唯象动力学方程。
2、对固相烧结过程现有的数值模拟方法进行了综述。重点讨论了基于Cahn-Hilliard守恒参量和Ginzburg-Landau非守恒参量的扩散相场模型。
3、利用扩散相场模型,结合Cahn-Hilliard守恒参量和Ginzburg-Landau非守恒参量控制方程,对初始颗粒四方堆积情形和初始颗粒气孔耦合拓扑情形固相烧结过程的微结构形貌演化进行了二维的数值模拟,数值模拟结果展现了固相烧结过程的诸多微观结构演化现象,如颗粒和气孔的迁移等。
4、在二维模拟的基础上,进一步利用扩散相场模型对初始颗粒堆积情形和初始颗粒气孔耦合拓扑情形固相烧结过程的微结构形貌演化进行了三维的数值模拟,更加直观的反映了在固相烧结过程中的微观结构演化规律,通过对不同模拟时间的材料孔隙率的统计并结合烧结理论验证了模型的有效性。
二、提出了利用加窗傅立叶滤波提高SR-CT重建图像质量的方法,为将SR-CT技术应用于陶瓷固相烧结过程的研究提供了算法和技术支持。
1、以提高SR-CT技术重建图像质量为主线,对SR-CT技术进行了探讨,详细介绍了滤波反投影算法和加窗傅立叶变换技术。
2、通过对滤波反投影重建算法和同步辐射光场空间非均匀性的讨论,分析了滤波反投影算法中影响重建图像质量的因素,提出了利用加窗傅立叶滤波改进重建图像质量的方案并分析了方法的可行性。
3、利用基于加窗傅立叶变换的滤波反投影算法得到了两组实验重建图像,和未经过加窗傅立叶变换重建图像的对比,其重建图像质量有了明显提高,同步辐射光场空间非均匀性噪声得到了有效抑制。
三、在国内率先实现了利用SR-CT技术对陶瓷固相烧结过程的实时和无损的观测,为改进烧结模型和指导烧结提供了有效的实验支持。
1、设计实验方案并制备了系列具有代表性的陶瓷粉末和素坯样品。利用SR-CT技术完成了对几种样品固相烧结过程的观测实验,得到了样品在不同烧结时刻的内部微观结构的二维和三维重建图像,通过重建图像观测到了陶瓷固相烧结过程的三个阶段及诸多烧结现象(晶界形成、颗粒长大、气孔球化等)。
2、利用数字图像处理方法统计了样品在不同烧结时刻的孔隙率变化,得到了孔隙率随烧结时间和烧结时间对数的变化曲线。通过曲线分析了各样品在烧结过程中的致密化规律,得到了在不同烧结阶段致密化的特点。
3、根据孔隙率—烧结时间对数曲线得到了烧结中期孔隙率随烧结时间对数的线性关系,提出了相对致密化速率的概念,并根据一组不同初始孔隙率样品的孔隙率—烧结时间对数曲线分析了初始孔隙率对烧结开始时间、烧结中期致密化相对速率和烧结完成时间的影响。
最后,总结全文工作,给出本文研究的主要内容和尚需进一步深入的研究课题,提出今后研究思路和方案。
In this paper, the necessity and importance of investigating ceramic sintering process in real-time and non-destructive is firstly presented. The microstructure evolution process and phenomena, thermodynamic mechanisms and theoretical models, constitutive laws and governing equations about sintering process is globally reviewed. The principle and research status of Synchrotron radiation x-ray computed tomography (SR-CT) technique is generally summarized. The microstructure evolution of the sintering process is numerical simulated by phase-field method. In order to observe the microstructure evolution of sintering process by SR-CT technique, the technical difficulties of SR-CT technique was studied and a new method which can improve the quality of reconstructed images based on the windowed Fourier filter method was proposed. The sintering process of several groups of ceramic samples was investigated by SR-CT experimental and the experimental results were discussed according the sintering theory.
The main content is as follows:
Firstly, by summarizes the sintering theories, the 2-D and 3-D microstructural evolution during sintering process was simulated by Phase field model while there are few reports on the 3-D results.
1、The material transmission mechanism, densificated process, empirical densification equation and phenomelogical densification equation about sintering process were studied.
2、A summary of the numerical simulating methods of sintering process was presented.The Phase field model based on Cahn-Hilliard equation for conserved field variables and Ginzburg-Landau equation for non-conserved variables was emphatically introduced.
3、By solving coupled time-dependent governing equations with Cahn-Hilliard equation for conserved field variables and Ginzburg-Landau equation for non-conserved variables, the 2-D microstructural evolution during sintering process, such as aggregation and migration of pores and grains is visually simulated.
4、The 3-D microstructural evolution during sintering process was futher simulated by the Phase field model and the Correctness of the Simulation Results was confirmed by the porosity-simulation time curves and sintering theories. Secondly, a new method of improving the quality of reconstructed images based on windowed Fourier filter method was proposed.
1、The SR-CT technique was discussed and the filter back-projection reconstruction algorithm was emphatically introduced.
2、By analysis the filter function of the filter back-projection reconstruction algorithm and the characteristics of the synchrotron radiation x-ray,the method of improving the quality of reconstructed images based on windowed Fourier filter method was proposed.The feasibility of the methods was analysised.
3、The effectiveness of the method was validated by the experimental results of two kinds of samples.Compaied with the reconstructed images that did not use Windowed Fourier filter method, the reconstructed images which use the Windowed Fourier filter method shows the high reconstruction quality. In addition, the real-time and non-destructice observation of the sintering process by Synchrotron radiation computed tomography technique was firstly realized in our country.
1、The experimental scheme was performed and several groups of sample according to different components and initial porosities were prepared, the SR-CT technique was employed to explore the microstructure evolution of the samples. From these cross-section images at different sintering time, the evolution process of grains and pores could be observed, and vertical-section and three-dimensional images could also be obtained.
2、The porosity of the compacted samples were obtained by treating the reconstructed images using digital image processing method.The desifacation Characteristics of different sintering stages could be clearly observed by the porosity-time and porosity- time-logarithm curves.
3、From the linear relationship between Porosity and Log time in the middle stage of sintering,the relative densification rate was performed. The beginning time of the sintering process, the relative densification rate in the middle stage of sintering and the end point of sintering was discussed by analyis the porosity- time-logarithm curve of the samples with different initial porosity.
At last, the whole works are summarized and the further researches are proposed.
本文主要研究内容如下:
一、总结了固相烧结理论,对固相烧结过程的微观结构演化进行了二维和三维的数值模拟,其中三维的数值模拟目前国内尚未见到公开的报道,在国际上也仅见少数几篇报道。
1、对固相烧结过程进行了分析,探讨了关于固相烧结过程的热力学驱动力和物质传输机制以及致密化过程的一些经验方程和唯象动力学方程。
2、对固相烧结过程现有的数值模拟方法进行了综述。重点讨论了基于Cahn-Hilliard守恒参量和Ginzburg-Landau非守恒参量的扩散相场模型。
3、利用扩散相场模型,结合Cahn-Hilliard守恒参量和Ginzburg-Landau非守恒参量控制方程,对初始颗粒四方堆积情形和初始颗粒气孔耦合拓扑情形固相烧结过程的微结构形貌演化进行了二维的数值模拟,数值模拟结果展现了固相烧结过程的诸多微观结构演化现象,如颗粒和气孔的迁移等。
4、在二维模拟的基础上,进一步利用扩散相场模型对初始颗粒堆积情形和初始颗粒气孔耦合拓扑情形固相烧结过程的微结构形貌演化进行了三维的数值模拟,更加直观的反映了在固相烧结过程中的微观结构演化规律,通过对不同模拟时间的材料孔隙率的统计并结合烧结理论验证了模型的有效性。
二、提出了利用加窗傅立叶滤波提高SR-CT重建图像质量的方法,为将SR-CT技术应用于陶瓷固相烧结过程的研究提供了算法和技术支持。
1、以提高SR-CT技术重建图像质量为主线,对SR-CT技术进行了探讨,详细介绍了滤波反投影算法和加窗傅立叶变换技术。
2、通过对滤波反投影重建算法和同步辐射光场空间非均匀性的讨论,分析了滤波反投影算法中影响重建图像质量的因素,提出了利用加窗傅立叶滤波改进重建图像质量的方案并分析了方法的可行性。
3、利用基于加窗傅立叶变换的滤波反投影算法得到了两组实验重建图像,和未经过加窗傅立叶变换重建图像的对比,其重建图像质量有了明显提高,同步辐射光场空间非均匀性噪声得到了有效抑制。
三、在国内率先实现了利用SR-CT技术对陶瓷固相烧结过程的实时和无损的观测,为改进烧结模型和指导烧结提供了有效的实验支持。
1、设计实验方案并制备了系列具有代表性的陶瓷粉末和素坯样品。利用SR-CT技术完成了对几种样品固相烧结过程的观测实验,得到了样品在不同烧结时刻的内部微观结构的二维和三维重建图像,通过重建图像观测到了陶瓷固相烧结过程的三个阶段及诸多烧结现象(晶界形成、颗粒长大、气孔球化等)。
2、利用数字图像处理方法统计了样品在不同烧结时刻的孔隙率变化,得到了孔隙率随烧结时间和烧结时间对数的变化曲线。通过曲线分析了各样品在烧结过程中的致密化规律,得到了在不同烧结阶段致密化的特点。
3、根据孔隙率—烧结时间对数曲线得到了烧结中期孔隙率随烧结时间对数的线性关系,提出了相对致密化速率的概念,并根据一组不同初始孔隙率样品的孔隙率—烧结时间对数曲线分析了初始孔隙率对烧结开始时间、烧结中期致密化相对速率和烧结完成时间的影响。
最后,总结全文工作,给出本文研究的主要内容和尚需进一步深入的研究课题,提出今后研究思路和方案。
In this paper, the necessity and importance of investigating ceramic sintering process in real-time and non-destructive is firstly presented. The microstructure evolution process and phenomena, thermodynamic mechanisms and theoretical models, constitutive laws and governing equations about sintering process is globally reviewed. The principle and research status of Synchrotron radiation x-ray computed tomography (SR-CT) technique is generally summarized. The microstructure evolution of the sintering process is numerical simulated by phase-field method. In order to observe the microstructure evolution of sintering process by SR-CT technique, the technical difficulties of SR-CT technique was studied and a new method which can improve the quality of reconstructed images based on the windowed Fourier filter method was proposed. The sintering process of several groups of ceramic samples was investigated by SR-CT experimental and the experimental results were discussed according the sintering theory.
The main content is as follows:
Firstly, by summarizes the sintering theories, the 2-D and 3-D microstructural evolution during sintering process was simulated by Phase field model while there are few reports on the 3-D results.
1、The material transmission mechanism, densificated process, empirical densification equation and phenomelogical densification equation about sintering process were studied.
2、A summary of the numerical simulating methods of sintering process was presented.The Phase field model based on Cahn-Hilliard equation for conserved field variables and Ginzburg-Landau equation for non-conserved variables was emphatically introduced.
3、By solving coupled time-dependent governing equations with Cahn-Hilliard equation for conserved field variables and Ginzburg-Landau equation for non-conserved variables, the 2-D microstructural evolution during sintering process, such as aggregation and migration of pores and grains is visually simulated.
4、The 3-D microstructural evolution during sintering process was futher simulated by the Phase field model and the Correctness of the Simulation Results was confirmed by the porosity-simulation time curves and sintering theories. Secondly, a new method of improving the quality of reconstructed images based on windowed Fourier filter method was proposed.
1、The SR-CT technique was discussed and the filter back-projection reconstruction algorithm was emphatically introduced.
2、By analysis the filter function of the filter back-projection reconstruction algorithm and the characteristics of the synchrotron radiation x-ray,the method of improving the quality of reconstructed images based on windowed Fourier filter method was proposed.The feasibility of the methods was analysised.
3、The effectiveness of the method was validated by the experimental results of two kinds of samples.Compaied with the reconstructed images that did not use Windowed Fourier filter method, the reconstructed images which use the Windowed Fourier filter method shows the high reconstruction quality. In addition, the real-time and non-destructice observation of the sintering process by Synchrotron radiation computed tomography technique was firstly realized in our country.
1、The experimental scheme was performed and several groups of sample according to different components and initial porosities were prepared, the SR-CT technique was employed to explore the microstructure evolution of the samples. From these cross-section images at different sintering time, the evolution process of grains and pores could be observed, and vertical-section and three-dimensional images could also be obtained.
2、The porosity of the compacted samples were obtained by treating the reconstructed images using digital image processing method.The desifacation Characteristics of different sintering stages could be clearly observed by the porosity-time and porosity- time-logarithm curves.
3、From the linear relationship between Porosity and Log time in the middle stage of sintering,the relative densification rate was performed. The beginning time of the sintering process, the relative densification rate in the middle stage of sintering and the end point of sintering was discussed by analyis the porosity- time-logarithm curve of the samples with different initial porosity.
At last, the whole works are summarized and the further researches are proposed.
引文
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[1]施剑林,固相烧结—Ⅰ气孔显微结构模型及其热力学稳定性,致密化方程,硅酸盐学报,1997,25(5):499-513.
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