Catayst Surface Analysis
A variety of surface analysis techniques are used routinely to characterise the surfaces of catalyst and working electrode synthesis. This ranges from ex situ (electron microscopy, ultra-high vacuum systems) to in situ/operando conditions. For more instrumentation details, use the links provided.
Microscopy
Characterisation of catalyst surface morphorlogy, elemental analysis, estimation of active surface area of catalyst-loaded surface, with the possibility of in situ observation of catalytic activity.
- SEM
- Hitachi S-3400N
- Thermo Scientific Apreo SEM
- AFM
- Bruker Multimode 8 AFM (electrochemical cell available)
- Asylum Research Cypher ES AFM (electrochemical AFM)
- TEM
- service provided by the Electron Microscopy group in the Inorganic Chemistry (AC) department
- JEOL JEM-ARM200F
- FEI Talos F200X
- FEI TITAN 80-300
Spectroscopy
Characterisation of surface chemical functionalities of the catalyst, frequently done in operando conditions.
- Fourier-Transform Infrared Spectroscopy (FTIR)
- Bruker Vertex 80v FT-IR spectrometer
- Raman spectro-microscopy
- Renishaw inVia Raman confocal microscope
- X-ray Photoelectron Spectroscopy (XPS)
- Multiple in-house built instruments (Moke, Orlando, NAP-XPS etc.)
- Both monochromatic (Bochum, Oraldno) and non-monoschromatic (Moke) X-ray sources available, depending on need
- Powder and planar samples commonly analysed
- Mg and Al X-ray sources available
- Moke system: quasi-in situ XPS available, where sample can be analysed directly after electrochemical reaction, without atmospheric exposure
- X-ray Absorption Spectroscopy (XAS)
- Regular beamtime arrangement between BESSY and the ISC
- XAS: XANES, EXAFS used to track catalyst structure and morphorlogy during electrochemical reactions (operando conditions)
- State-of-the-art structural model and data-fitting techniques
Bruker D8 Advance X-ray diffractometer (left) and TA Instruments Discovery TGA 5500 (right) for catalyst crystallinity and chemical analysis
X-ray Crystallography
Determination of catalyst bulk and surface crystallinity, in relation to catalytic activity and catalyst degredation.
- X-ray Diffraction (XRD)
- Bruker D8 Advance
Thermogravimetric Analysis (TGA)
- TA Instruments Discovery TGA 5500
- Autosampler attachment
- Low mass IR furnace, Differential Thermal Analysis (DTA) signal