Transmission electron microtomography without the "missing wedge" for quantitative structural analysis
Transmission electron microtomography without the "missing wedge" for quantitative structural analysis
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DOI：
10.1016/j.ultramic.2006.04.007
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发表时间：
2007-01-01
期刊：
影响因子：
2.2
通讯作者：
Jinnai, Hiroshi
中科院分区：
文献类型：
--
作者：
Kawase, Noboru;Kato, Mitsuro;Jinnai, Hiroshi
通过透射电子显微断层扫描（TEMT）对氧化锆/聚合物纳米复合材料的棒状样品进行了三维（313）可视化和结构分析，特别强调样品的完全旋转（倾斜角范围：+/- 90度）。为了达到这样一个理想的实验条件的TEMT，在试样以及样品保持器的改进。为了在倾斜到大角度时获得高透射率的样品，需要杆状样品。重建的断层图像的图像分辨率是各向同性的，与具有有限角度范围的常规TEMT的各向异性图像分辨率形成鲜明对比（“缺失楔形”问题）。氧化锆的体积分数，φ，从3D重建评估是在定量协议与纳米复合材料的已知组成。通过限制最大倾斜角α，从具有完全旋转的倾斜系列中进行一系列3D重建，从该倾斜系列中评估氧化锆的每单位体积的体积分数和表面积σ作为α的函数。从实际的实验数据证实，0和Z都随着α的增加而略微减小，并且在α = 80度左右达到恒定值，这表明为了进行真正的定量测量，样品可能必须倾斜到+/-80度。(c)2006 Elsevier B. V.保留所有权利。
A three-dimensional (313) visualization and structural analysis of a rod-shaped specimen of a zirconia/polymer natiocomposite material were carried out by transmission electron microtomography (TEMT) with particular emphasis on complete rotation of the specimen (tilt angular range: +/- 90 degrees). In order to achieve such an ideal experimental condition for the TEMT, improvements in the specimen as well as the sample holder were made. A rod-shaped specimen was necessary in order to obtain a high transmission of the specimen upon tilting to large angles. The image resolution of the reconstructed tomogram was isotropic, in sharp contrast to the anisotropic image resolution of the conventional TEMT with a limited angular range (the "missing wedge" problem). A volume fraction of zirconia, phi, evaluated from the 3D reconstruction was in quantitative agreement with the known composition of the nanocomposite. A series of 3D reconstructions was made from the tilt series with complete rotation by limiting the maximum tilt angle, alpha, from which a couple of structural parameters, the volume fraction and surface area per unit volume, Sigma, of the zirconia, were evaluated as a function of alpha. It was confirmed from actual experimental data that both 0 and Z slightly decreased with the increasing a and reached constant values at around alpha = 80 degrees, suggesting that the specimen may have to be tilted to +/- 80 degrees for truly quantitative measurements. (c) 2006 Elsevier B.V. All rights reserved.