We developed an experimental setup, which allows us to conduct correlative SEM, optical, and x-ray microscopy/tomography studies of active interfaces and working devices under realistic operating conditions (i.e., in liquids, high-pressure gases, and plasmas). The SEM setup is integrated with micro-Raman spectrometer; thus enabling Raman, fluorescence, reflectance spectra to be collected from the SEM field of view. The sample can be incased in a fluidic chamber which has a micro-fabricated electron/optically transparent SiN membrane with embedded microheater and electrical contacts. The fluidic chamber has an exchangeable modular design; thus, different environments liquids, gases, and plasma and sample sizes can be used.
This unique setup allows us to conduct real-time spectromicroscopy studies on charge transport inside nanodevices, reactive battery (or fuel cell) electrodes under cycling, thin-films nucleation and growth during CVD, ALD, PVD depositions, observing chemical or plasma etching processes, etc. under realistic conditions and with nanometer lateral resolution.
The fundamental aspect of this research is in experimental studies of electron beam interaction with solid and liquid interfaces exposed to gaseous and plasma environments that is not well understood.
Kolmakov A, Gregoratti L, Kiskinova M, Guenther S: Recent Approaches for Bridging the Pressure Gap in Photoelectron Microspectroscopy. Topics in Catalysis 59: 448-468, 2016
Al-Asadi AS, Zhang J, Li J, Potyrailo RA, Kolmakov A: Design and application of variable temperature setup for scanning electron microscopy in gases and liquids at ambient conditions. Microscopy and Microanalysis 21; 765-770, 2015
Tselev A, Velmurugan J, Ievlev AV, Kalinin SV, A. Kolmakov A: Seeing Through Walls at the Nanoscale: Microwave Microscopy of Enclosed Objects and Processes in Liquids. ACS Nano 10(3): 3562-3570, 2016
In situ SEM; Liquids; Gases; Microfluidics; Plasma; Devices; Nanoparticles; u-Raman; Electrochemistry;