Departamento de Química Inorgánica I, Universidad Complutense, 28040 Madrid, Spain.
Inorg Chem. 2011 May 16;50(10):4640-6. doi: 10.1021/ic2004112. Epub 2011 Apr 14.
A novel synthetic strategy based on the combination of the chlorination of an organometallic precursor followed by solvothermal treatment is found to be successful in the synthesis of tetragonal nano-ZrO(2) or nano-ZrO(2), embedded in an amorphous carbon matrix, depending on the solvent employed in the solvothermal step. The chemical and structural features (chemical composition, size and surface defects) of the intermediate and final materials have been determined experimentally mainly by high resolution transmission electron microscopy, electron energy loss spectroscopy, and Z-contrast images. These local techniques reveal that the nanoparticles consist of tetragonal ZrO(2) with an average size of 1.7 ± 0.4 and 6.2 ± 0.9 nm for the embedded in carbon and the free nano-ZrO(2), respectively.
一种新的合成策略，基于有机金属前体的氯化反应，然后进行溶剂热处理，被发现成功地合成了四方纳米 ZrO(2)或纳米 ZrO(2)，嵌入在无定形碳基质中，这取决于溶剂热步骤中使用的溶剂。中间和最终材料的化学和结构特征（化学成分、尺寸和表面缺陷）主要通过高分辨率透射电子显微镜、电子能量损失光谱和 Z 对比度图像实验确定。这些局部技术表明，纳米粒子由四方 ZrO(2)组成，嵌入碳中的纳米粒子的平均尺寸为 1.7±0.4nm，自由纳米 ZrO(2)的平均尺寸为 6.2±0.9nm。
