探针扫描式液相原子力显微镜技术及系统研制
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摘要
纳米科技是近年来飞速发展的前沿学科领域之一。原子力显微镜(AFM)因具有极高的分辨率,并且可在大气和液体等多种环境下进行微纳米检测,而成为纳米科技领域的重要工具。目前,国内外已有的液相AFM系统大多采用样品扫描方式,仅适用于小样品、小区域及小扫描范围检测；同时,这些系统只在样品表面滴上一小滴液滴,仅有极小面积的样品表面浸润在液体中,并非全液相环境。为此,本文发展了一种基于探针扫描方式的大范围液相AFM新方法与新技术,克服了现有液相AFM的局限性,不仅具有重要的科学意义,而且在物理学、化学及电化学、材料学和生命科学等领域有着广泛的应用前景。
论文首先阐述了液相AFM的工作原理、成像特点以及国内外发展现状,对AFM探针在溶液中受到的固液界面相互作用进行了系统的理论研究,讨论了它们对液相AFM成像的影响。通过对探针扫描式AFM的传统探测光路进行分析,对光路中的扫描误差和反馈误差进行了理论推导与计算,讨论了这些误差对AFM成像造成的影响,并提出了消除扫描误差和反馈误差的关键因素。
在此基础上,提出和发展了一种探针扫描式液相AFM的新方法。开展了液相AFM成像理论的研究,分析了AFM的液相成像特性。提出了探针扫描式AFM的光路跟踪新方法,该方法可实现扫描过程中检测光对探针运动的追踪,消除扫描器的运动给光电探测信号引入的横向扫描误差和纵向反馈误差。此外,本文还提出了一种基于位置敏感元件的光路误差检测法,可对扫描误差进行直观的判断和分析,指导检测光路的进一步调试。
本文研究和发展了一种新型液相AFM探头系统。该探头采用探针扫描方式和开放式设计,消除了对样品尺寸和重量的限制。特殊的液相视窗和探针座的设计,可将样品和AFM探针完全浸入到液体中,实现全液相环境下的扫描检测。搭建了新型探针扫描式液相检测光路,切实解决了扫描过程中的光路跟踪问题,消除了因扫描器的运动所引起的XY向扫描误差和Z向反馈误差。设计制作了叠层式与管式组合型扫描与反馈控制器,该扫描器结合了叠层式压电陶瓷位移量大和管式压电陶瓷响应迅速的优点,可实现较大扫描范围和纳米级分辨率的XY向扫描和高精度的Z向反馈控制。采用二维步进移动台,既可以实现探针与样品之间的快速定位(扫描选区),又能实现更大范围的图像拼接。
在上述理论和技术研究的基础上,研制了探针扫描式液相AFM系统。该系统可测量最大尺寸300mm×300mm、最大重量10kg的样品,可实现液相和气相两种环境下的AFM扫描检测。压电陶瓷扫描器的XY方向最大扫描范围有4gm×4μm和20gm×20μm可选,分辨率可达纳米量级。二维步进移动台的步进移动范围为30mm×30mm,可实现探针在样品表面任意位置的快速定位。
为了研究考察探针扫描式液相AFM的性能,利用该系统气相及液相环境下全面开展了实验技术研究。首先,分别在液体和空气中对标准光栅和锗量子点等典型样品进行了扫描检测,成功获得了样品表面的纳米结构图像。其次,在草酸溶液中对多孔氧化铝模板进行了AFM图像的序列测量,通过图像拼接获得了较大范围的高分辨AFM图像。此外,对铝在NaOH溶液中的腐蚀和铁片基底铜的电化学沉积过程进行了实时观察,获得了这些反应过程的序列图像。实验结果表明,本文自主研发的液相型AFM,无论是在空气中还是在液相环境下,均可获得良好的图像分辨率、重复性和对比度,而且其液相成像性能突出,完全可满足科研及工业等领域对大样品进行大范围及高分辨扫描检测的要求。
最后,对论文的研究内容和研究成果进行了总结,阐述了探针扫描式液相AFM的新方法及本文研制的新型液相AFM系统的特点及创新之处。同时,提出了课题研究工作中的不足和需要改进之处,对未来的研究工作提出了展望。
Nanotechnology opens new frontier in scientific research. Atomic force microscope (AFM). a high-resolution imaging technique that can resolve atomic features, can be operated in various environments, such as ambient air and liquids. It makes AFM an important analytic tool for nanotechnology. Traditional liquid-AFMs usually adopt sample-scanning method, which promises a high stability and sensitivity but encounters challenges when imaging large and massive samples. Moreover, the liquid cell of commercial AFMs is available to immerse samples in liquid but only maintain a limited area of sample surface for their limited volume and closed design. In contrast, probe-scanning type AFM is not subject to this limitation and can obtain images with high speed either in air or in liquid.
The objective of this dissertation is to develop a novel liquid-AFM system capable of imaging large samples in liquid environment with a high resolution. With a unique optical detection method, the laser beam can reflect from the same point on the cantilever during scanning. It can overcome the limitations of current liquid-AFM systems described above, and shows its broader potential applications in the fields of physics, chemistry, electrochemistry, materials and biology.
Firstly, the principle, features and state-of-the-art of liquid AFM system are briefly reviewed and presented. Then the probe-sample interactions in liquid environment and their influences have been detailed analyzed. Besides, the scanning-and feedback-induced errors in traditional probe-scanning AFMs and their influences on AFM measurements have been theoretical analyzed and calculated. Based on these theoretical analyses, the research plan for this project will be demonstrated.
Secondly, a novel optical detection method for probe-scanning AFM is designed. With a new beam tracking method, the laser beam can reflect from the same point on the cantilever throughout raster scan over the entire scan area. This method has enabled elimination of the scanning- and feedback-induced errors in the optical path of current probe-scanning AFMs. To estimate the scanning-induced error, a detection method based on position sensitive detector (PSD) is developed. With the aid of this method, the optical path of the detection system can be easily adjusted.
On the basis of the new optical detection method, a liquid-AFM probe unit has been designed and fabricated. In the liquid-AFM head, the laser adjustment can be eliminated regardless of the measuring environment. Thanks to the special designed window, the beam shift that normally occurs upon immersion into liquid is completely absent in the AFM head, which makes the measurements in liquid environment as simple as measuring in air. Additionally, a new kind of three-dimensional piezoelectric scanner is designed. The new compound scanner uses two stacked piezoelectric actuators in the X and Y directions for their large displacements, and a piezoelectric tube in Z-axis for its fast response. It combines the advantages of these two kind of piezoelectric actuators. With the help of the two-dimensional step scanner, our AFM probe unit is able to locate on the sample surface rapidly and scan AFM images in adjacent regions successively.
Based on above theoretical analyses and developed novel methods, a liquid-AFM system is established to address measurements in liquid environment of both the research lab and industrial applications. It enables imaging large sample in liquid with high resolution and high performances. Furthermore, image stitching method has been developed to build a wider AFM image with range from micrometers to millimeters.
Below is a summary of the key features of this AFM. The system is designed to image samples with size up to 300mm×300mm and weight up to 10kg. To satisfying different measurement needs, two kinds of piezo scanner are fabricated. The smaller scanner has a scan range of 4μm×4μm with spatial resolution of 0.1 nm. The compound scanner, which combines the advantages of stacked piezo and piezo tube, has a scan range of 20μm×20μm and spatial resolution of nanometer. The two-dimensional step scanner with an X-Y travel range of 30mm×30mm, allows fast travelling and location of AFM probe on large sample surface in X-Y plane and scanning AFM images in adjacent regions successively. Combined with the Z-axis piezo tube, it can also realize larger-size AFM measurements. In addition, an image stitching method is utilized to build a broad merged microscopic image with range up to millimeters while keeping nanometer order resolution. This function enables us to obtain wide AFM images with high resolution, which satisfies the rising scientific and industrial demands in micro- and nano-measurements.
To demonstrate the imaging ability and stability of the developed liquid-AFM system, serials of experimental measurements were carried out. Results show that the overall shape, size, and contrast are nearly identical in those images. Furthermore, by studying the corrosion behavior of aluminum surface in NaOH solution, as well as copper plating on silicon wafer in real time with the developed liquid-AFM system, we also show that the system can observe the solid-liquid interface of the electrochemical reactions and processes in the atomic level. The superior performance of the system renders its great prospect in research and industry applications among chemical, electrochemical and biological studies, where large-size scanning and high-resolution imaging are required for large, heavy samples in liquid environment.
论文首先阐述了液相AFM的工作原理、成像特点以及国内外发展现状,对AFM探针在溶液中受到的固液界面相互作用进行了系统的理论研究,讨论了它们对液相AFM成像的影响。通过对探针扫描式AFM的传统探测光路进行分析,对光路中的扫描误差和反馈误差进行了理论推导与计算,讨论了这些误差对AFM成像造成的影响,并提出了消除扫描误差和反馈误差的关键因素。
在此基础上,提出和发展了一种探针扫描式液相AFM的新方法。开展了液相AFM成像理论的研究,分析了AFM的液相成像特性。提出了探针扫描式AFM的光路跟踪新方法,该方法可实现扫描过程中检测光对探针运动的追踪,消除扫描器的运动给光电探测信号引入的横向扫描误差和纵向反馈误差。此外,本文还提出了一种基于位置敏感元件的光路误差检测法,可对扫描误差进行直观的判断和分析,指导检测光路的进一步调试。
本文研究和发展了一种新型液相AFM探头系统。该探头采用探针扫描方式和开放式设计,消除了对样品尺寸和重量的限制。特殊的液相视窗和探针座的设计,可将样品和AFM探针完全浸入到液体中,实现全液相环境下的扫描检测。搭建了新型探针扫描式液相检测光路,切实解决了扫描过程中的光路跟踪问题,消除了因扫描器的运动所引起的XY向扫描误差和Z向反馈误差。设计制作了叠层式与管式组合型扫描与反馈控制器,该扫描器结合了叠层式压电陶瓷位移量大和管式压电陶瓷响应迅速的优点,可实现较大扫描范围和纳米级分辨率的XY向扫描和高精度的Z向反馈控制。采用二维步进移动台,既可以实现探针与样品之间的快速定位(扫描选区),又能实现更大范围的图像拼接。
在上述理论和技术研究的基础上,研制了探针扫描式液相AFM系统。该系统可测量最大尺寸300mm×300mm、最大重量10kg的样品,可实现液相和气相两种环境下的AFM扫描检测。压电陶瓷扫描器的XY方向最大扫描范围有4gm×4μm和20gm×20μm可选,分辨率可达纳米量级。二维步进移动台的步进移动范围为30mm×30mm,可实现探针在样品表面任意位置的快速定位。
为了研究考察探针扫描式液相AFM的性能,利用该系统气相及液相环境下全面开展了实验技术研究。首先,分别在液体和空气中对标准光栅和锗量子点等典型样品进行了扫描检测,成功获得了样品表面的纳米结构图像。其次,在草酸溶液中对多孔氧化铝模板进行了AFM图像的序列测量,通过图像拼接获得了较大范围的高分辨AFM图像。此外,对铝在NaOH溶液中的腐蚀和铁片基底铜的电化学沉积过程进行了实时观察,获得了这些反应过程的序列图像。实验结果表明,本文自主研发的液相型AFM,无论是在空气中还是在液相环境下,均可获得良好的图像分辨率、重复性和对比度,而且其液相成像性能突出,完全可满足科研及工业等领域对大样品进行大范围及高分辨扫描检测的要求。
最后,对论文的研究内容和研究成果进行了总结,阐述了探针扫描式液相AFM的新方法及本文研制的新型液相AFM系统的特点及创新之处。同时,提出了课题研究工作中的不足和需要改进之处,对未来的研究工作提出了展望。
Nanotechnology opens new frontier in scientific research. Atomic force microscope (AFM). a high-resolution imaging technique that can resolve atomic features, can be operated in various environments, such as ambient air and liquids. It makes AFM an important analytic tool for nanotechnology. Traditional liquid-AFMs usually adopt sample-scanning method, which promises a high stability and sensitivity but encounters challenges when imaging large and massive samples. Moreover, the liquid cell of commercial AFMs is available to immerse samples in liquid but only maintain a limited area of sample surface for their limited volume and closed design. In contrast, probe-scanning type AFM is not subject to this limitation and can obtain images with high speed either in air or in liquid.
The objective of this dissertation is to develop a novel liquid-AFM system capable of imaging large samples in liquid environment with a high resolution. With a unique optical detection method, the laser beam can reflect from the same point on the cantilever during scanning. It can overcome the limitations of current liquid-AFM systems described above, and shows its broader potential applications in the fields of physics, chemistry, electrochemistry, materials and biology.
Firstly, the principle, features and state-of-the-art of liquid AFM system are briefly reviewed and presented. Then the probe-sample interactions in liquid environment and their influences have been detailed analyzed. Besides, the scanning-and feedback-induced errors in traditional probe-scanning AFMs and their influences on AFM measurements have been theoretical analyzed and calculated. Based on these theoretical analyses, the research plan for this project will be demonstrated.
Secondly, a novel optical detection method for probe-scanning AFM is designed. With a new beam tracking method, the laser beam can reflect from the same point on the cantilever throughout raster scan over the entire scan area. This method has enabled elimination of the scanning- and feedback-induced errors in the optical path of current probe-scanning AFMs. To estimate the scanning-induced error, a detection method based on position sensitive detector (PSD) is developed. With the aid of this method, the optical path of the detection system can be easily adjusted.
On the basis of the new optical detection method, a liquid-AFM probe unit has been designed and fabricated. In the liquid-AFM head, the laser adjustment can be eliminated regardless of the measuring environment. Thanks to the special designed window, the beam shift that normally occurs upon immersion into liquid is completely absent in the AFM head, which makes the measurements in liquid environment as simple as measuring in air. Additionally, a new kind of three-dimensional piezoelectric scanner is designed. The new compound scanner uses two stacked piezoelectric actuators in the X and Y directions for their large displacements, and a piezoelectric tube in Z-axis for its fast response. It combines the advantages of these two kind of piezoelectric actuators. With the help of the two-dimensional step scanner, our AFM probe unit is able to locate on the sample surface rapidly and scan AFM images in adjacent regions successively.
Based on above theoretical analyses and developed novel methods, a liquid-AFM system is established to address measurements in liquid environment of both the research lab and industrial applications. It enables imaging large sample in liquid with high resolution and high performances. Furthermore, image stitching method has been developed to build a wider AFM image with range from micrometers to millimeters.
Below is a summary of the key features of this AFM. The system is designed to image samples with size up to 300mm×300mm and weight up to 10kg. To satisfying different measurement needs, two kinds of piezo scanner are fabricated. The smaller scanner has a scan range of 4μm×4μm with spatial resolution of 0.1 nm. The compound scanner, which combines the advantages of stacked piezo and piezo tube, has a scan range of 20μm×20μm and spatial resolution of nanometer. The two-dimensional step scanner with an X-Y travel range of 30mm×30mm, allows fast travelling and location of AFM probe on large sample surface in X-Y plane and scanning AFM images in adjacent regions successively. Combined with the Z-axis piezo tube, it can also realize larger-size AFM measurements. In addition, an image stitching method is utilized to build a broad merged microscopic image with range up to millimeters while keeping nanometer order resolution. This function enables us to obtain wide AFM images with high resolution, which satisfies the rising scientific and industrial demands in micro- and nano-measurements.
To demonstrate the imaging ability and stability of the developed liquid-AFM system, serials of experimental measurements were carried out. Results show that the overall shape, size, and contrast are nearly identical in those images. Furthermore, by studying the corrosion behavior of aluminum surface in NaOH solution, as well as copper plating on silicon wafer in real time with the developed liquid-AFM system, we also show that the system can observe the solid-liquid interface of the electrochemical reactions and processes in the atomic level. The superior performance of the system renders its great prospect in research and industry applications among chemical, electrochemical and biological studies, where large-size scanning and high-resolution imaging are required for large, heavy samples in liquid environment.
引文
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