面向微纳尺度实验力学分析的扫描电镜-拉曼光谱联用系统与分析方法

Confocal Raman spectroscopy and scanning electron microscopy are all robust instruments applied in the experimental study of mechanics at micro-to-nano scale. However, the measurements by using the two instruments respectively and independently is hard to satisfy the research requirement of in-situ and simultaneous correlative analysis. Hence it is necessary to develop a new Raman-SEM hyphenated system, and corresponding analyzing methods as well, specifically suitable to the mechanical investigation. This project is proposed to develop a set of SEM and confocal micro-Raman hyphenated system. It would be the first hyphenated system built through oblique interposing mode and it would be compatible to several advanced SEM system. Based on the existing tungsten filament SEM, the core components would be designed and developed, meanly including a four coaxial optical system of confocal Raman/fluorescence, an optical interposing module with multi degree of freedom, a universal docking module, and an angular resolution accessory. After the integral assembly and debugging, the hyphenated system would be operated on multi-spectral mode, and its key parameters would be calibrated. The kernel technical problems would be solved, such as the interference of different modules, multi-control outside the sample compartment, in situ multi-spectral measurement. Based on the hyphenated system, the in situ measurement method, considering the angle-resolved Raman and spectral size effect, would be proposed for the decoupling measurement of the stress tensor. Finally, the hyphenated system will be used in the in situ measurements and simultaneous correlative analyses for the multi-scale mechanical properties of some typical micro-nano materials and structures. Through the feedback of the application, the apparatus would be improved further.

共焦显微拉曼光谱仪与扫描电子显微镜均是目前微纳尺度力学实验研究广泛使用的大型仪器。然而采用二者进行分别、独立的测量难以满足多尺度、原位、协同力学分析的研究需求，亟需发展适于力学测量的联用系统及相应分析方法。本项目面向微纳尺度实验力学的原位精细表征，研发一套基于斜向介入模式、多平台兼容通用的扫描电镜-共焦显微拉曼联用系统。本研究在现有钨灯丝扫描电镜基础上，设计、研制共焦显微拉曼四同轴光路系统、多自由度光学介入与通用式对接装置等核心组件以及角度分辨附件，通过系统整体组装、调试实现系统联合运行和关键参数指标标定，解决模块干涉、仓外多重控制、多光谱原位测量等关键技术问题。在此基础上，提出基于角度分辨拉曼和考虑光谱尺寸效应的应力解耦表征模型与原位测量方法。最后将所研发系统与方法应用于典型微纳尺度材料与结构的多尺度力学性能原位测量与协同分析，并通过应用实验反馈改进所研发的联用系统。

共焦显微拉曼光谱仪与扫描电子显微镜均是目前微纳尺度力学实验研究广泛使用的大型仪器。然而采用二者进行分别、独立的测量难以满足多尺度、原位、协同力学分析的研究需求，亟需发展适于力学测量的联用系统及相应分析方法。面向微纳尺度实验力学的原位精细表征，本项目研发了一套基于斜向介入模式、多平台兼容通用的扫描电镜-显微共焦拉曼联用系统，通过系统整体组装、调试实现系统联合运行和关键参数指标标定，解决了模块干涉、仓外多重控制、原位测量等关键技术问题；提出了基于角度分辨拉曼和考虑光学折射、数值孔径等因素的应力解耦表征模型与测量方法；将所研发系统与方法应用于典型材料应力原位测量，实现了显微观察与光谱力学表征的协同分析。