Our laboratory is equipped with techniques for fundamental and applicative electrochemical tests, as well as methods for advanced material characterization. In addition to our equipment, we collaborate with other departments and institutions for access to additional techniques.
Synthesis and electrocatalyst characterization
- High-temperature furnaces with quartz tubes
- X-ray powder diffractometer (PANalytical X'Pert PRO) (In collaboration with the Department of Inorganic Chemistry and Technology)
- BioLogic: SP-200
- Ivium Technologies: Compact.Stat.e
- Nordic Electrochemistry: 2×ECi200 in Eci100
- Princeton Applied Research: PARSTAT 2273
- BioLogic: SP-300
- DropSens: μStat 400
- Rotators for rotating disk electrodes (3×OrigaLys, Radiometer Analytical, EG&G PARC)
- Rotators for rotating ring disk electrodes (Pine)
- High temperature disk electrode setup
- Floating electrode setup
- Gas diffusion electrode setup
Characterization of electrocatalysts with the floating electrode method is in between fast screening tests with a rotating electrode and more application-imitating membrane-electrode assembly. Using commercial TEM grids as floating electrodes in a custom build setup enables rapid electrochemical characterization of promising electrocatalysts under high mass transport of gaseous products or reactants and at the same time local nanoscale and even atomic scale characterization in the TEM.
More about the method in this publication.
Advanced electrochemical techniques
- Electrochemical cell, coupled to an MS detector for detection of volatile compounds (financed by ARRS Paket 18, NATO SPS OFICeR and ERC 123STABLE projects)
Electrochemistry – Mass Spectrometry (EC-MS) is a coupled technique that combines an electrochemical experiment with a mass spectrometry detector. The technique provides a platform for detecting electrochemically formed gaseous and volatile species as a function of applied voltage/current, which opens up a window into electrocatalytic processes such as water electrolysis and CO2 reduction. It is also an essential tool for studying degradation of carbon materials as electrodes in all types of electrochemical processes.
In an instrument by Spectro Inlets, a working electrode in a three-electrode electrochemical cell is assembled parallel to a membrane chip at a well-defined distance. All volatile analytes formed at the electrode diffuse across the thin film of electrolyte and equilibrate across the perforated membrane with an atmosphere of a carrier gas in the volume below the membrane. The carrier gas not only limits the evaporation of the solvent, thus enabling lower detection limits, but it also saturates the electrolyte in the cell. The analytes and carrier gas travel at a well-defined flux through a narrow capillary to the vacuum system of the mass spectrometer for ionization, separation and detection. The system design ensures that all the analyte species from the electrolyte are eventually detected at the MS, thus enabling quantitative detection.
- Electrochemical flow cell, coupled to and ICP-MS detector (Agilent Technologies 7900 ICP-MS) (In collaboration with the Department of Analytical Chemistry)
A flow cell is used to carry out typical electrochemical experiments while at the same time performing a mass-spectrometric analysis of the electrolyte. This enables determining the concentration of metals that have dissolved from the sample into the electrolyte as a result of the electrochemical manipulation. Even ppb-level concentration can be accurately determined and the obtained concentration profiles enable direct comparison of the dissolved metals with the electrochemical changes imposed to the sample.
- Atomic resolution scanning transmission electron microscope (JEOL, ARM 200CF) (Department of Materials Chemistry)
- In situ heating TEM holder (Aduro Protochips)
- Identical location setup
- Scanning electron microscope (Zeiss Supra 35 VP) (Department of Materials Chemistry)
Electron microscopy enables precise studies of materials structure, but it is very localized to a small location. To be able to reliably study the structural changes that are caused by electrochemical action, it is important to find the same location in the material (e.g. the same nanoparticle) before and after electrochemical tests. This is identical location electron miscroscopy, which enables atomically precise determination of structural changes of electrocatalytic materials.
- Ozonator (A2Z Ozone, MP-3000 Multi-Purpose Ozone Generator)