Atomic-scale electron microscopy at ambient pressure

Ultramicroscopy. 2008 Aug;108(9):993-8. doi: 10.1016/j.ultramic.2008.04.014. Epub 2008 May 2.

Abstract

We demonstrate a novel nanoreactor for performing atomic-resolution environmental transmission electron microscopy (ETEM) of nanostructured materials during exposure to gases at ambient pressures and elevated temperatures. The nanoreactor is a microelectromechanical system (MEMS) and is functionalized with a micrometer-sized gas-flow channel, electron-transparent windows and a heating device. It fits into the tip of a dedicated sample holder that can be used in a normal CM microscope of Philips/FEI Company. The nanoreactor performance was demonstrated by ETEM imaging of a Cu/ZnO catalyst for methanol synthesis during exposure to hydrogen. Specifically, the nanoreactor facilitated the direct observation of Cu nanocrystal growth and mobility on a sub-second time scale during heating to 500 degrees C and exposure to 1.2 bar of H(2). For the same gas reaction environment, ETEM images show atomic lattice fringes in the Cu nanocrystals with spacing of 0.18 nm, attesting the spatial resolution limit of the system. The nanoreactor concept opens up new possibilities for in situ studies of nanomaterials and the ways they interact with their ambient working environment in diverse areas, such as heterogeneous catalysis, electrochemistry, nanofabrication, materials science and biology.