基于超声显微镜的薄层材料多参量一体化定征关键技术研究
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摘要
薄层材料作为一种对现代工业和国民经济产生巨大影响的功能性材料,在其研发、制备和应用等过程中一直以来对无损定征技术具有强烈的需求。而超声无损检测技术由于具有其它方法难以媲美的优势,在薄层材料性能定征和质量监控中得到了广泛应用,呈现出定征内容日益丰富、多参量一体化定征成为主流的发展态势,特别是随着超声显微镜技术的飞速发展,由于其高分辨率的特点,使得精细化定征成为可能,并十分适合于薄层材料性能定征和质量监控中应用。因此,基于超声显微镜的薄层材料定征技术必将是该领域发展的主流,显示出巨大的发展潜力。基于以上背景,本论文结合国家自然科学基金资助项目,开展基于超声显微镜的薄层材料多参量一体化无损定征关键技术研究,根据薄层材料的结构特点以及超声波在薄层材料中的传播规律,在建立薄层材料反射系数理论模型、发展一种基于超声显微镜的二维反射系数测量技术的基础上,利用垂直入射的反射系数谱和双入射角的反射系数谱,通过多参量辨识技术同时确定薄层材料的厚度、密度、波速和衰减等特性参数,实现薄层材料的多参量一体化定征。具体的研究内容和创新成果体现在：
第一章,阐述薄层材料及其研发、制备和应用过程中实施无损定征技术的重要意义,系统总结薄层材料无损定征技术的研究现状及其发展趋势,全面概括基于超声显微镜的薄层材料定征技术的研究现状,明确目前该技术所存在的问题,为本文指明了研究方向。同时,对论文的研究内容及各章节进行了安排。
第二章,建立了超声波在均匀介质叠层结构中的传播模型,分别推导垂直入射和斜入射情况下任意结构的叠层材料声反射系数理论计算公式。在介绍传统Thomson-Haskell算法及其高频精度损失问题的基础上,提出了一种改进型Thomson-Haskell算法用于声反射系数的理论计算,建立了声反射系数与薄层材料属性及其结构参数,包括厚度、密度、声速和衰减等特性参量之间的定量关系,为薄层材料的特性定征奠定了必要的理论基础。
第三章,在建立超声显微镜声波传播模型的基础上,详细分析基于脉冲超声显微镜的二维反射系数测量原理,创建了一种基于宽频脉冲超声显微镜的二维反射系数测量方法,并简要描述了Z轴采样步距对测量结果的影响,为采样步距优化选择提供理论依据。然后,分别实测铝、有机玻璃和四种不同厚度薄钢片以及两类典型多层结构的声反射系数,并与利用第二章方法所计算的理论声反射系数进行比较,验证了该测量方法的有效性和可行性,为本文的后续工作提供了共性的技术保障。
第四章,提出了一种基于垂直入射超声反射系数谱的薄层材料多参量一体化定征方法。首先,根据聚焦探头和薄层的几何关系推导薄层材料厚度理论表达式,建立薄层材料厚度与探头聚焦在相应薄材上、下表面时回波信号之间的定量关系。其次,通过第三章所述V(z,t)技术测量薄层材料的声反射系数,并拾取探头聚焦在待检薄材上、下表面时的声回波信号,进而根据薄层材料的厚度表达式确定薄材的厚度。然后,在厚度已知的情况下,通过提取所测反射系数的垂直分量,并根据最小二乘反演算法确定其余参量,实现了薄层材料的多参量一体化定征。最后,使用50MHz的聚焦探头,对250μm厚度的不锈钢薄片属性进行定征,相关参数定征误差均在5%以内,验证了该方法的可行性和有效性。
第五章,提出了一种基于双入射角超声反射系数谱的薄层材料多参量一体化定征技术。首先,建立薄层结构声波传播模型,利用改进型Thomson-Haskell算法确定二维声反射系数与所需定征参量,即材料的密度和厚度、纵波和横波波速以及纵波和横波衰减等,之间的定量关系。其次,通过基于超声显微镜的V(z,t)技术测量薄层材料样本的反射系数,提取垂直入射和较优斜入反射系数谱,并引入两步逆解算法,将六维空间中的参数逆求问题转换为两步三维空间参数逆求问题,实现薄层材料特性参数的完整定征。然后,还对该方法进行了灵敏度函数分析和抗噪声的稳定性分析。最后,使用25MHz聚焦探头将该方法应用于250μm厚度不锈钢薄片的定征,所定征全部参数误差均在4%以内,验证了该方法的可行性和有效性。
第六章对本文的研究工作进行概括总结,并对以后的工作进行展望,明确未来的主要研究内容和方向。
As a functional material, thin layer plays an enormous impact on the modern industry and the national economy, thus the non-destructive characterization of thin layer has been strongly demanded during the processes of thin layer development, preparation and application. Ultrasonic nondestructive testing is widely used in the field of material property characterization and quality control of thin layer due to its unique advantages, and shows the trends of simultaneous characterization. With the rapid development of acoustic microscope technique, the high resolution characterization has been possible and it is very suitable for the characterization of thin layer. Therefore, the characterization technique based on the acoustic microscopy has shown great potential and would be the mainstream. Thus, with the support of National Natural Science Foundation-funded project, the simultaneous characterization of material and geometrical properties of thin layer with acoustic microscopy is studied.On the basis of theoretical model of wave propagation and the proposed reflection coefficient measurement technique, the material properties, including thickness, density, longitudinal and transverse velocities, and attenuation, are determined with an inverse algorithm utilizing least square method to minimize the sum of squared deviations between theoretical and measured reflection spectrum at normal and oblique incidence. The detailed context and innovative points of this dissertation are as following:
In chapter one, the importance of non-destructive testing on the development, preparation and application of thin layer is briefly described. Then, The current research status of non-destructive testing associating with thin layer and its development in the further are summarized. Finally, the characterization of thin layer with acoustic microscopy is systematically generalized. Meanwhile, the problems are clarified and the research direction is pointed out. The content and chapter arrangement of the dissertation are also given.
In chapter two, the theoretical reflection spectrum of layered structure at normal incidence is firstly established by analyzing wave propagation. A reformulation of the Thomson-Haskell method is presented to calculate the acoustic reflection coefficients of layered structures of arbitrary configurations. Finally, the simulation studies verify the validity and feasibility of the proposed method.
In Chapter three, the spatial and temporal structure of the acoustic field is analyzed on the basis of wave propagation model, and an experimental method based on angular spectrum to evaluate the acoustic coefficient as a function of the incident angle θ and frequency co is presented with acoustic microscopy. Then, the Z-axis sampling interval is briefly discussed. The measurements of the reflection coefficients of the layered structures based on the proposed technique with self-developed scanning acoustic microscopy are performed. Two substrates of aluminum and Plexiglas, four stainless plates with various thicknesses of100μm,150μm,200μm, and250μm, and two typical multilayer structure are applied. The measured results are consistent with the corresponding theoretical calculations to verify the validity and feasibility of the proposed technique.
In chapter four, a kind of simultaneous measurement method for the thickness, density, sound velocity and attenuation using V(z,t) data recorded by time-resolved acoustic microscopy is proposed. The theoretical reflection spectrum of thin layer at normal incidence is established as a function of three dimensionless parameters. The measured reflection spectrum R(θ,ω) is obtained from V(z,t) data and the measured thickness is derived from the signals when the lens focusing on the front and back surface of thin layer, which are picked up from the V(z,t) data.The density, sound velocity and attenuation are then determined by the measured thickness and inverse algorithm utilizing least squares method to fit the theoretical and measured reflection spectrum at normal incidence. Thus, the proposed method allows to simultaneously measuring the thickness, density, sound velocity and attenuation of thin layer. An experimental example using a point-focusing transducer with nominal frequency of around50MHz is conducted with250μm stainless steel plate. The measurement results validate the proposed method. The results demonstrate that the thickness, density and sound velocity can be measured with a percentage biases less than5%and the sound attenuation is close to true value.
In chapter five, an ultrasonic technique for simultaneous determination of the complete set of acoustical and geometrical properties of thin layer using two incident angles is presented.The theoretical model of the two-dimensional spectrum of the thin layer is calculated as a function of six parameters:thickness, density, longitudinal and transverse velocities and attenuation, using the reformulation of Thomson-Haskell method.Then, The experimental spectrum can be measured by V(z,t) technique with acoustic microscopy. The full set of the properties can be derived inversely with minimization of the difference between the calculated and experimentally measured reflection spectrum of the thin layer at two angles:one at normal incidence and the other at oblique incidence. By introducing a two-step inversion algorithm, the searching process in six-dimensional space is transformed to two searching processes in three-dimensional space. The sensitivity of the two-dimensional spectrum to individual properties and its stability against experimental noise are studied. Meanwhile, an experimental example is performed with250μm stainless steel plate. The measured errors are less than4%, validating the proposed method.
In chapter six, the research results and the innovative points of this dissertation were summarized, and the future research works are also forecast.
第一章,阐述薄层材料及其研发、制备和应用过程中实施无损定征技术的重要意义,系统总结薄层材料无损定征技术的研究现状及其发展趋势,全面概括基于超声显微镜的薄层材料定征技术的研究现状,明确目前该技术所存在的问题,为本文指明了研究方向。同时,对论文的研究内容及各章节进行了安排。
第二章,建立了超声波在均匀介质叠层结构中的传播模型,分别推导垂直入射和斜入射情况下任意结构的叠层材料声反射系数理论计算公式。在介绍传统Thomson-Haskell算法及其高频精度损失问题的基础上,提出了一种改进型Thomson-Haskell算法用于声反射系数的理论计算,建立了声反射系数与薄层材料属性及其结构参数,包括厚度、密度、声速和衰减等特性参量之间的定量关系,为薄层材料的特性定征奠定了必要的理论基础。
第三章,在建立超声显微镜声波传播模型的基础上,详细分析基于脉冲超声显微镜的二维反射系数测量原理,创建了一种基于宽频脉冲超声显微镜的二维反射系数测量方法,并简要描述了Z轴采样步距对测量结果的影响,为采样步距优化选择提供理论依据。然后,分别实测铝、有机玻璃和四种不同厚度薄钢片以及两类典型多层结构的声反射系数,并与利用第二章方法所计算的理论声反射系数进行比较,验证了该测量方法的有效性和可行性,为本文的后续工作提供了共性的技术保障。
第四章,提出了一种基于垂直入射超声反射系数谱的薄层材料多参量一体化定征方法。首先,根据聚焦探头和薄层的几何关系推导薄层材料厚度理论表达式,建立薄层材料厚度与探头聚焦在相应薄材上、下表面时回波信号之间的定量关系。其次,通过第三章所述V(z,t)技术测量薄层材料的声反射系数,并拾取探头聚焦在待检薄材上、下表面时的声回波信号,进而根据薄层材料的厚度表达式确定薄材的厚度。然后,在厚度已知的情况下,通过提取所测反射系数的垂直分量,并根据最小二乘反演算法确定其余参量,实现了薄层材料的多参量一体化定征。最后,使用50MHz的聚焦探头,对250μm厚度的不锈钢薄片属性进行定征,相关参数定征误差均在5%以内,验证了该方法的可行性和有效性。
第五章,提出了一种基于双入射角超声反射系数谱的薄层材料多参量一体化定征技术。首先,建立薄层结构声波传播模型,利用改进型Thomson-Haskell算法确定二维声反射系数与所需定征参量,即材料的密度和厚度、纵波和横波波速以及纵波和横波衰减等,之间的定量关系。其次,通过基于超声显微镜的V(z,t)技术测量薄层材料样本的反射系数,提取垂直入射和较优斜入反射系数谱,并引入两步逆解算法,将六维空间中的参数逆求问题转换为两步三维空间参数逆求问题,实现薄层材料特性参数的完整定征。然后,还对该方法进行了灵敏度函数分析和抗噪声的稳定性分析。最后,使用25MHz聚焦探头将该方法应用于250μm厚度不锈钢薄片的定征,所定征全部参数误差均在4%以内,验证了该方法的可行性和有效性。
第六章对本文的研究工作进行概括总结,并对以后的工作进行展望,明确未来的主要研究内容和方向。
As a functional material, thin layer plays an enormous impact on the modern industry and the national economy, thus the non-destructive characterization of thin layer has been strongly demanded during the processes of thin layer development, preparation and application. Ultrasonic nondestructive testing is widely used in the field of material property characterization and quality control of thin layer due to its unique advantages, and shows the trends of simultaneous characterization. With the rapid development of acoustic microscope technique, the high resolution characterization has been possible and it is very suitable for the characterization of thin layer. Therefore, the characterization technique based on the acoustic microscopy has shown great potential and would be the mainstream. Thus, with the support of National Natural Science Foundation-funded project, the simultaneous characterization of material and geometrical properties of thin layer with acoustic microscopy is studied.On the basis of theoretical model of wave propagation and the proposed reflection coefficient measurement technique, the material properties, including thickness, density, longitudinal and transverse velocities, and attenuation, are determined with an inverse algorithm utilizing least square method to minimize the sum of squared deviations between theoretical and measured reflection spectrum at normal and oblique incidence. The detailed context and innovative points of this dissertation are as following:
In chapter one, the importance of non-destructive testing on the development, preparation and application of thin layer is briefly described. Then, The current research status of non-destructive testing associating with thin layer and its development in the further are summarized. Finally, the characterization of thin layer with acoustic microscopy is systematically generalized. Meanwhile, the problems are clarified and the research direction is pointed out. The content and chapter arrangement of the dissertation are also given.
In chapter two, the theoretical reflection spectrum of layered structure at normal incidence is firstly established by analyzing wave propagation. A reformulation of the Thomson-Haskell method is presented to calculate the acoustic reflection coefficients of layered structures of arbitrary configurations. Finally, the simulation studies verify the validity and feasibility of the proposed method.
In Chapter three, the spatial and temporal structure of the acoustic field is analyzed on the basis of wave propagation model, and an experimental method based on angular spectrum to evaluate the acoustic coefficient as a function of the incident angle θ and frequency co is presented with acoustic microscopy. Then, the Z-axis sampling interval is briefly discussed. The measurements of the reflection coefficients of the layered structures based on the proposed technique with self-developed scanning acoustic microscopy are performed. Two substrates of aluminum and Plexiglas, four stainless plates with various thicknesses of100μm,150μm,200μm, and250μm, and two typical multilayer structure are applied. The measured results are consistent with the corresponding theoretical calculations to verify the validity and feasibility of the proposed technique.
In chapter four, a kind of simultaneous measurement method for the thickness, density, sound velocity and attenuation using V(z,t) data recorded by time-resolved acoustic microscopy is proposed. The theoretical reflection spectrum of thin layer at normal incidence is established as a function of three dimensionless parameters. The measured reflection spectrum R(θ,ω) is obtained from V(z,t) data and the measured thickness is derived from the signals when the lens focusing on the front and back surface of thin layer, which are picked up from the V(z,t) data.The density, sound velocity and attenuation are then determined by the measured thickness and inverse algorithm utilizing least squares method to fit the theoretical and measured reflection spectrum at normal incidence. Thus, the proposed method allows to simultaneously measuring the thickness, density, sound velocity and attenuation of thin layer. An experimental example using a point-focusing transducer with nominal frequency of around50MHz is conducted with250μm stainless steel plate. The measurement results validate the proposed method. The results demonstrate that the thickness, density and sound velocity can be measured with a percentage biases less than5%and the sound attenuation is close to true value.
In chapter five, an ultrasonic technique for simultaneous determination of the complete set of acoustical and geometrical properties of thin layer using two incident angles is presented.The theoretical model of the two-dimensional spectrum of the thin layer is calculated as a function of six parameters:thickness, density, longitudinal and transverse velocities and attenuation, using the reformulation of Thomson-Haskell method.Then, The experimental spectrum can be measured by V(z,t) technique with acoustic microscopy. The full set of the properties can be derived inversely with minimization of the difference between the calculated and experimentally measured reflection spectrum of the thin layer at two angles:one at normal incidence and the other at oblique incidence. By introducing a two-step inversion algorithm, the searching process in six-dimensional space is transformed to two searching processes in three-dimensional space. The sensitivity of the two-dimensional spectrum to individual properties and its stability against experimental noise are studied. Meanwhile, an experimental example is performed with250μm stainless steel plate. The measured errors are less than4%, validating the proposed method.
In chapter six, the research results and the innovative points of this dissertation were summarized, and the future research works are also forecast.
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