| AVS 63rd International Symposium & Exhibition | |
| In-Situ and Operando Spectroscopy and Microscopy for Catalysts, Surfaces, & Materials Focus Topic | Thursday Sessions |
| Session IS-ThP |
| Session: | In-Situ and Operando Spectroscopy and Microscopy for Catalysts, Surfaces, & Materials Poster Session |
| Presenter: | Hongxuan Guo, National Institute of Standards and Technology (NIST) |
| Authors: | H.X. Guo, National Institute of Standards and Technology (NIST) A. Yulaev, National Institute of Standards and Technology A. Kolmakov, National Institute of Standards and Technology |
| Correspondent: | Click to Email |
For applications such as electrochemistry, environmental science or (photo-) catalysis it is important to characterize materials and interfaces in reactive liquid or aquatic environments. However, interface sensitive characterization techniques, such as X-ray photoelectron spectroscopy (XPS), XAS, Auger electron spectroscopy (AES), SEM, electron microscopies require high or ultrahigh vacuum environments for their operation. To circumvent these pressure gap challenges, the graphene membrane based environmental cells have been recently developed 1, 2, 3 Graphene is the strongest materials with one molecularly impermeable atomic layer thick and it is transparent to electrons and x-rays in a wide energy range. Therefore, it is the best separating membrane material so far for fabrication of liquid cell for thein-situ studies of liquid samples in high or ultra-high vacuum environments.
We report on high yield fabrication of double layer graphene capped multichannel matrix which can be impregnated with a large variety of liquids and electrolytes for in-situ SEM, EDS, SAM, XPS. The liquid life time inside a cell can reach many hours and is limited by the defects density in the graphene and interfacial diffusion between the graphene membrane and MCA matrix. Using SEM, in combination with EDS and XAS spectroscopies we analyzed the electronic structure and dynamics of water-graphene interface. Auger spectroscopy was used to analyzed the attenuation of the water generated Auger electrons by double layer graphene. Electrochemical graphene liquid cells have been fabricated via Pt electrodes atomic layer deposition deep in to the MCA matrix. , We performed first feasibility tests via electroplating and stripping of Cu on the surface of double layer graphene from CuSO4 solution. This new sample platform provides a new experimental ground for characterization of liquid materials for energy, catalysis, biomedical and environmental research.
1 1. J. Kraus, R. Reichelt, S. Guenther, L. Gregoratti, M. Amati, M. Kiskinova, A. Yulaev, I. Vlassiokiv and A. Kolmakov, Nanoscale, 2014. 6, 14394-14403
2. J. D. Stoll and A. Kolmakov, Nanotechnology, 2012, 23, 505704.
3. Andrei Kolmakov, Luca Gregoratti, Maya Kiskinova, Sebastian Günther, Topics in Catalysis, 2016, 59, 448–468