Material preparation

Highlights:

  • Fully equipped synthesis laboratory
  • Tube furnaces for synthesis or catalyst calcination under controlled gas atmosphere and flow
  • Physical characterization of synthesized materials (TGA-MS, DSC, BET, SEM/EDX, XPS, XRD)

References:

  • Hartig-Weiss, A.; Miller, M.; Beyer, H.; Schmitt, A.; Siebel, A.; Freiberg, A. T. S.; Gasteiger, H. A.; El-Sayed, H. A. / ACS Appl. Nano Mater., 2020, 3, 2185-2196, -  DOI
  • Geppert, T. N.; Bosund, M.; Putkonen, M.; Stühmeier, B. M.; Pasanen, A. T.; Heikkilä, P.; Gasteiger, H. A.; El-Sayed, H. A. / J. Electrochem. Soc., 2020, 167, article # 084517 (Open Access) - DOI
  • Stühmeier, B. M.; Selve, S.; Patel, M. U. M.; Geppert, T. N.; Gasteiger, H. A.; El-Sayed, H. A. / ACS Applied Energy Materials, 2019, 2, 8, 5534-5539 (Open Access) – DOI
  • Madkikar, P.; Menga, D.; Harzer, G. S.; Mittermeier, T.; Siebel, A.; Wagner, F. E.; Merz, M.; Schuppler, S.; Nagel, P.; Munoz-Garcia, A. B.; Pavone, M.; Gasteiger, H. A.; Piana, M. / J. Electrochem. Soc., 2019, 166(7), F3032-F3043 (Open Access) - DOI

Highlights:

  • In-house electrode fabrication starting from solvent-based catalyst inks using an RK Control Coater
  • Coating process via the Mayer-rod and "doctor-blade" techniques adapted for the desired wet film thickness
  • Tuning of the catalyst layer properties by varying the solid and liquid composition of the ink

References:

Ink Solvent Dependence of the Ionomer Distribution in the Catalyst Layer of a PEMFC / Orfanidi, A.; Rheinländer, P. J.; Schulte, N.; Gasteiger, H. A. / J. Electrochem. Soc., 2018, 165, F1254–F1263 (Open Access) – DOI

Highlights:

  • Decal Transfer Method for fabrication of membrane electrode assemblies (MEAs)
  • Automatic program for hot-pressing of catalyst coated membrane (CCM)  
  • Defined hot-pressing conditions (temperature, pressure)
  • Improved interface between membrane and ionomer-containing catalyst layer

Testing equipment

The cryo cross section polisher (IB-19520 CCP, JEOL) is the ideal device to prepare samples for scanning electron microscopy (SEM). An argon ion beam allows for smoother cross sections with less distortion compared to mechanical polishing methods for various kind of samples. Sensitive samples can additionally be cooled down with liquid nitrogen during polishing. To achieve the best results, varying polishing settings can be adjusted to the sample type.

Highlights:

  • Clean polished cross section of hard, soft, and composite material
  • Preparation of LIB electrode and MEA cross sections for SEM analysis
  • Cryo-polishing to minimize beam damage for sensitive materials (e.g., binder etc.)

Highlights:

  • Fully automated test station
  • Gamry Potentiostat with 30 A booster
  • High pressure operation up to 30 bar (differential or symmetric)
  • 5 cm² single cell hardware for high pressure operation
  • Evaluation of the influence of pressure, catalyst loading and ionomer content on electrolyzer performance

Publication:

Influence of Ionomer Content in IrO2/TiO2 Electrodes on PEM Water Electrolyzer Performance / Bernt, M.; Gasteiger, H. A. / J. Electrochem. Soc., 2016, 163(11), F3179-F3189 (Open Access)  - DOI

Via physical adsorption/desorption of inert gases (Kr, N), the surface and the porosity of the measured material can be determined.

Highlights:

  • Portable gas flow/humidification system with Biologic VSP-300 Potentiostat (2 channels, 20 A)
  • Water pump for electrolysis operation
  • Custom-made operando 5 cm2 single cell with x-ray windows
  • Designed for mechanistic studies of noble- and transition-metal catalysts using x-ray absorption spectroscopy (XAS) in operando mode

References:

  • A. Siebel, Y. Gorlin, J. Durst, O. Proux, F. Hasché, M. Tromp, H. A. Gasteiger, ACS Catalysis, 6, 7326-7334 (2016) - DOI

Highlights:

  • Fast screening of different synthesized catalysts based on their activity for the hydrogen oxidation/evolution (HOR/HER) and oxygen reduction/evolution (ORR/OER) reactions
  • Setups adapted for acidic, alkaline and aprotic electrolytes
  • Small-scale testing with few mg of material
  • Investigation of different electrochemical deposition reactions

References:

  • Hartig-Weiß, A.; Tovini, M. F.; Gasteiger, H. A.; El-Sayed, H. A. / ACS Applied Energy Materials, 2020 - DOI

Mercury intrusion porosimetry (MIP) is used to examine the pore structure of a sample. Since mercury does not wet most substances (shows a contact angle greater than 90°), it has to be forced to fill open pore space by applying an external pressure. According to the Washburn equation, this pressure correlates inversely to the pore diameter, which can be accessed from roughly 200 µm down to 3 nm by MIP. The more-than-five-decade span of pore sizes enables the application for a wide range of powders (e.g., cathode active materials for lithium-ion batteries) and solids (e.g. battery electrodes, catalyst layers and gas diffusion media of fuel cells and electrolyzers). Targeted parameters are the pore size and its distribution, pore volume, bulk and skeletal density, and finally the porosity of the sample.

The picture shows the table-top SEM Jeol JCM6000 (left-side) with the possibility of gold-sputtering with Jeol JFC-1300 (right side). The SEM is a useful tool to visualize the micron-sized active-material particles in battery electrodes. Additionally the composition of the electrode can be determined via elemental analysis using the built-in EDX probe.

X-ray photoelectron spectroscopy (XPS) is a surface-sensitive quantitative spectroscopic technique. With this method, it is possible to quantify the elemental composition, empirical formula, chemical state and electronic state of the elements that are within a range of ~5 nm of the surface.