Impact of the electron beam on the thermal stability of gold nanorods studied by environmental transmission electron microscopy

Highlights: • An in-situ environmental TEM study of the thermal stability of CTAB-stabilized gold nanorods. • Upon electron irradiation the CTAB bi-layer transformed into a carbon layer stabilizing the anisotropic shape up to high temperatures. • Under ex-situ conditions the nanorods deformed at much lower temperatures. • This work demonstrates that in-situ TEM data need to be carefully assessed and accompanied by ex-situ experiments. - Abstract: In-situ transmission electron microscopy experiments are of great interest to nanoscience and nanotechnology. However, it is known that the electron beam can have a significant impact on the structure of the sample which makes it important to carefully interpret in-situ data. In this work, we studied the thermal stability of CTAB-stabilized gold nanorods under different gaseous environments in an environmental transmission electron microscope and compared the outcome to ex-situ heating experiments. We observed a remarkable influence of the electron beam: While the nanorods were stable under inert conditions when exposed to the electron beam even at 400°C, the same nanorods reshaped at temperatures as low as 100°C under ex-situ conditions. We ascribe the stabilizing effect to the transformation of the CTAB bi-layer into a thin carbon layer under electron beam irradiation, preventing the nanorods from deforming. When exposed to an oxidizing environment in the environmental transmission electron microscope, this carbon layer was gradually removed and the gold atoms became mobile allowing for the deformation of the rod. This work highlights the importance of understanding the phenomena taking place under electron beam irradiation, which can greatly affect in-situ experiments and conclusions drawn from these. It stresses that in-situ electron microscopy data, taken on measuring the temperature dependence of nanoparticle properties, should be carefully assessed and accompanied by ex-situ experiments if possible.