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.

  • 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.

Thermogravimetric Analysis (TGA)

  • TA Instruments Discovery TGA 5500
  • Autosampler attachment
  • Low mass IR furnace, Differential Thermal Analysis (DTA) signal
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