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A Novel Method for Specimen Preparation and Analysis of CVD Diamond Coated Tools Using Focussed Ion Beams (FIB) and Scanning Electron Microscopy (SEM)

机译:利用聚焦离子束(FIB)和扫描电子显微镜(SEM)进行CVD金刚石涂层工具的样品制备和分析的新方法

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Investigations of the microscopic properties of chemical vapor deposited diamond coatings on tungsten carbide tools are important to understand the coating-substrate interface (Uhlmann et al. in Prod Eng Res Dev ll(2):83-86, 2004; Surf Coat Technol 131, 395-399, 2000), the coating morphology, and the properties of cracks. Commonly the microscopic properties are analyzed in the transmission electron microscope (TEM). This paper presents a novel investigation method that includes a faster specimen preparation and that offers new analyzing possibilities. It applies a well-established device combining a scanning focused ion beam (FIB) column for the preparation of the specimens and a scanning electron microscope (SEM) for the analysis of the specimen. The aim of the paper is to verify preparation parameters for which the microscopic properties of the diamond coating are preserved during the FIB preparation and to show that the SEM analysis provides the same results of microstructure and element distribution compared to the TEM analysis. Furthermore, the feasibility of new analysis methods is studied. The FIB/SEM method traces and images defects in the nanometer range like cracks, crack propagation directions, delaminations, and layer inhomogeneities directly. The bulk FIB-prepared specimens are suitable for a precise standard-based element quantification and distribution analysis using energy or wavelength (WDX) dispersive X-ray spectroscopy. Moreover, the WDX analysis distinguishes between graphite-like carbon and diamond.
机译:研究碳化钨工具上化学气相沉积金刚石涂层的微观特性对于理解涂层与基体的界面非常重要(Uhlmann等人,Prod Eng Res Dev ll(2):83-86,2004; Surf Coat Technol 131, 395-399,2000),涂层的形态,以及裂纹的性质。通常,在透射电子显微镜(TEM)中分析微观性质。本文提出了一种新颖的调查方法,该方法包括更快的标本制备过程,并提供了新的分析可能性。它使用了完善的设备,该设备结合了用于制备样品的扫描聚焦离子束(FIB)柱和用于分析样品的扫描电子显微镜(SEM)。本文的目的是验证在FIB制备过程中保留金刚石涂层微观特性的制备参数,并表明SEM分析与TEM分析相比提供了相同的微观结构和元素分布结果。此外,研究了新分析方法的可行性。 FIB / SEM方法可直接在纳米范围内跟踪和成像缺陷,例如裂纹,裂纹扩展方向,分层和层不均匀性。 FIB制备的大量样品适用于使用能量或波长(WDX)色散X射线光谱学进行基于标准元素的精确定量和分布分析。此外,WDX分析可区分类石墨碳和金刚石。

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