高级sem和ebsd的Trip钢试样制备

O. Ambrož, Š. Mikmeková, Veronika Hegrová, T. Aoyama
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引用次数: 1

摘要

现代扫描电子显微镜(SEM)允许观察具有高表面灵敏度的标本。加速电压对表面灵敏度有显著影响。随着扫描电镜技术的发展,对样品表面质量的要求越来越高。最初用于光学显微镜的金相方法变得不够。这个问题尤其发生在具有细晶粒结构的多相材料上。所研究的TRIP钢由铁素体-贝氏体基体、残余奥氏体和马氏体相组成。最小相的尺寸为纳米单位。用x射线衍射法测定残余奥氏体的体积。所有测试样品的基本制备都涉及常规金相磨削和非常精细的机械抛光。在这种状态下分析了一个样本。其他样品随后进行化学抛光、电抛光和化学机械抛光。制备后立即使用SE和BSE检测器在低能量下对样品进行扫描电镜观察。在同一区域进行EBSD以表征残留的奥氏体。利用专用原子力显微镜(AFM)与扫描电镜(SEM)结合的形貌分析表明,机械抛光导致表面变形,残余奥氏体发生转变。所有其他方法都有其特点,对于现代灵敏的扫描电镜仪器,有必要优化个别程序。
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TRIP STEEL SPECIMEN PREPARATION FOR ADVANCED SEM AND EBSD
Modern scanning electron microscopy (SEM) allows observations of specimens with high surface sensitivity. The surface sensitivity is significantly affected by the accelerating voltages. With the development of the scanning electron microscopy, the requirements for the surface quality of samples increase. Metallographic methods originally intended for light microscopy become insufficient. The problem occurs especially with multiphase materials having a fine-grained structure. The investigated TRIP steel consists of a ferritic-bainitic matrix, retained austenite and martensite phases. The sizes of the smallest phases are nanometer units. The volume of residual austenite was determined by X-ray diffraction. The basic preparation of all tested samples involved conventional metallographic grinding and very fine mechanical polishing. One sample was analysed in this state. Other samples were subsequently chemically polished, electropolished and chemical-mechanically polished. The specimens were observed in the SEM using a SE and a BSE detector at low energies immediately after the preparation. An EBSD was performed in the same areas to characterize the retained austenite. Topographical imaging by special AFM, integrated into the SEM, demonstrated that the mechanical polishing results in surface deformation and residual austenite is transformed. All other methods have their specifics and for modern sensitive SEM instruments it is necessary to optimize individual procedures.
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