A MEMS Reactor for Atomic-Scale Microscopy of Nanomaterials Under Industrially Relevant Conditions

We present a microelectromechanical systems (MEMS) nanoreactor that enables high-resolution transmission electron microscopy (TEM) (HRTEM) of nanostructured materials with atomic-scale resolution during exposure to reactive gases at 1 atm of pressure. This pressure exceeds that of existing HRTEM systems by a factor of 100, thereby entering a pressure range that is relevant to industrial purposes. The nanoreactor integrates a shallow flow channel (35 ??m high) with a microheater and with an array of electron transparent windows of silicon nitride. The windows are only 10 nm thick but are mechanically robust. The heater has the geometry of a microhotplate and is made of Pt embedded in a silicon nitride membrane. To interface the nanoreactor, a dedicated TEM specimen holder has been developed. The performance is demonstrated by the live formation of Cu nanoparticles in a catalyst for the production of methanol. At 120 kPa and for temperatures of up to 500??C , the formation of these nanoparticles can be observed clearly and with an exceptionally low thermal drift. HRTEM images of the nanoparticles show atomic lattice fringes with spacings down to 0.18 nm.