Winiarski B, Gholinia A, Mingard K, Gee M, Thompson G E, Withers P J
School of Materials, University of Manchester, Manchester M13 9PL, UK; Materials Division, National Physical Laboratory, Teddington TW11 0LW, UK.
School of Materials, University of Manchester, Manchester M13 9PL, UK.
Ultramicroscopy. 2017 Jan;172:52-64. doi: 10.1016/j.ultramic.2016.10.014. Epub 2016 Nov 11.
Here we examine the potential of serial Broad Ion Beam (BIB) Ar ion polishing as an advanced serial section tomography (SST) technique for destructive 3D material characterisation for collecting data from volumes with lateral dimensions significantly greater than 100µm and potentially over millimetre sized areas. Further, the associated low level of damage introduced makes BIB milling very well suited to 3D EBSD acquisition with very high indexing rates. Block face serial sectioning data registration schemes usually assume that the data comprises a series of parallel, planar slices. We quantify the variations in slice thickness and parallelity which can arise when using BIB systems comparing Gatan PECS and Ilion BIB systems for large volume serial sectioning and 3D-EBSD data acquisition. As a test case we obtain 3D morphologies and grain orientations for both phases of a WC-11%wt. Co hardmetal. In our case we have carried out the data acquisition through the manual transfer of the sample between SEM and BIB which is a very slow process (1-2 slice per day), however forthcoming automated procedures will markedly speed up the process. We show that irrespective of the sectioning method raw large area 2D-EBSD maps are affected by distortions and artefacts which affect 3D-EBSD such that quantitative analyses and visualisation can give misleading and erroneous results. Addressing and correcting these issues will offer real benefits when large area (millimetre sized) automated serial section BIBS is developed.
在此,我们研究了连续宽离子束(BIB)氩离子抛光作为一种先进的连续切片断层扫描(SST)技术的潜力,该技术用于破坏性三维材料表征,以从横向尺寸显著大于100μm且可能超过毫米大小区域的体积中收集数据。此外,所引入的相关低损伤水平使BIB铣削非常适合以非常高的索引率进行三维电子背散射衍射(EBSD)采集。块面连续切片数据配准方案通常假定数据由一系列平行的平面切片组成。我们量化了在使用BIB系统(比较Gatan PECS和Ilion BIB系统用于大体积连续切片和三维EBSD数据采集)时可能出现的切片厚度和平行度变化。作为一个测试案例,我们获得了WC-11%wt.Co硬质合金两相的三维形态和晶粒取向。在我们的案例中,我们通过在扫描电子显微镜(SEM)和BIB之间手动转移样品来进行数据采集,这是一个非常缓慢的过程(每天1-2片),然而即将出现的自动化程序将显著加快这一过程。我们表明,无论切片方法如何,原始大面积二维EBSD图都会受到影响三维EBSD的畸变和伪像的影响,从而使得定量分析和可视化可能给出误导性和错误的结果。在开发大面积(毫米大小)自动化连续切片BIB系统时,解决和纠正这些问题将带来实际益处。