Nano-Structural Elucidation in Carbon Black Loaded NR Vulcanizate by 3D-TEM and In Situ WAXD Measurements
Nano-Structural Elucidation in Carbon Black Loaded NR Vulcanizate by 3D-TEM and In Situ WAXD Measurements
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通过 3D-TEM 和原位 WAXD 测量阐明炭黑负载的 NR 硫化橡胶的纳米结构
DOI：
10.5254/1.3539405
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发表时间：
2007
影响因子：
1.5
通讯作者：
B. Hsiao
中科院分区：
文献类型：
--
作者：
Y. Ikeda;A. Kato;J. Shimanuki;S. Kohjiya;M. Tosaka;S. Poompradub;S. Toki;B. Hsiao
本文成功地研究和报道了炭黑在橡胶基体中分散体纳米结构的三维可视化。使用3D-TEM，这是计算机断层扫描结合透射电子显微镜（TEM），使我们能够重建天然橡胶（NR）矩阵中的炭黑聚集体的3D图像。TEM测量是在没有任何电子染色的薄样品上通过明场方法进行的。样品在样品室中经受单轴倾斜（+65度至-65度，增量为2度），并且对每个样品拍摄66张TEM图像。这些TEM图像用于计算机断层扫描以重建3D图像。该技术被称为3D-TEM。透射电子显微镜观察到的纳米结构特征与电子电导率的结果一致，证实了纳米材料的渗流行为。这些结果通过原位广角X射线衍射（WAXD）进一步补充，即，同时对样品进行WAXD和拉伸测量，以观察NR硫化胶中的应变诱导结晶。在拉伸伸长率时，在炭黑存在下的WAXD中清楚地观察到结晶，并且其有助于拉伸性能。为了了解填充NR硫化胶的性能，更有必要了解混合纳米填料的结构状态和伸长时产生的微晶。«少
Three dimensional (3D) visualization of nanometer structure of carbon black dispersion in rubbery matrix has successfully been studied and reported in this paper. Use of 3D-TEM, which is computerized tomography combined with transmission electron microscopy (TEM), enabled us to reconstruct 3D images of carbon black aggregates in natural rubber (NR) matrix. The TEM measurements were conducted by a bright-field method on thin samples without any electron staining. The sample was subject to uni-axial tilting (+65 degree to -65 degree with 2 degree increment) in the sample chamber, and 66 TEM images were taken on each sample. These TEM images were used for computerized tomography to reconstruct the 3D image. This technique is designated as 3D-TEM. The nano-structural features observed by 3D-TEM were in conformity with the electron-conductivity results, and the percolation behavior was recognized. These results were further supplemented by in situ wide-angle X-ray diffraction (WAXD), i.e., simultaneous WAXD and tensile measurements on the sample to observe the strain-induced crystallization in NR vulcanizate. Upon tensile elongation, the crystallization was clearly observed in WAXD in the presence of carbon black, and it contributed to the tensile properties. In order to understand the performances of filled NR vulcanizates, it surely is necessarymore » to know the structural states of the mixed nano-filler and the crystallites produced upon elongation.« less