Department of Materials, University of Oxford, Parks Road, Oxford OX1 3PH, UK.
Ultramicroscopy. 2010 Apr;110(5):506-16. doi: 10.1016/j.ultramic.2009.12.010. Epub 2009 Dec 23.
Recently designed advanced in-situ specimen holders for transmission electron microscopy (TEM) have been used in studies of gold nanoparticles. We report results of variable temperature TEM experiments in which structural transformations have been correlated with specimen temperature, allowing general trends to be identified. Transformation to a decahedral morphology for particles in the size range 5-12nm was observed for the majority of particles regardless of their initial structure. Following in-situ annealing, decahedra were found to be stable at room temperature, confirming this as the equilibrium morphology, in agreement with recently calculated phase diagrams. Other transitions at low temperature in addition to surface roughening have also been observed and correlated with the same nanoscale phase diagram. Investigations of gold particles at high temperature have revealed evidence for co-existing solid and liquid phases. Overall, these results are important in a more precise understanding of the structure and action of catalytic gold nanoparticles and in the experimental verification of theoretical calculations.
最近设计的用于透射电子显微镜(TEM)的原位样品支架在金纳米粒子的研究中得到了应用。我们报告了变温 TEM 实验的结果,其中结构转变与样品温度相关联,从而可以确定一般趋势。对于尺寸范围为 5-12nm 的大多数粒子,无论其初始结构如何,都观察到粒子向十面体形态的转变。在原位退火后,发现在室温下十面体稳定,这与最近计算的相图一致,证实了这是平衡形态。除了表面粗糙化之外,还观察到低温下的其他转变,并与相同的纳米级相图相关联。对高温下的金粒子的研究揭示了共存的固-液两相的证据。总的来说,这些结果对于更精确地理解催化金纳米粒子的结构和作用以及实验验证理论计算都很重要。