Nanomaterials, Catalysis, Electrochemistry

Equipment

In case you are interested in having measurements/experiments done with our equipement, please get in touch with Jérémy Geens .

General Characterization Equipment

DSC
Differencial Scanning calorimetry, TPD/R/O 1100 Fisons Instrument, Setaram TG-DSC 111 coupled with mass spectrometer Balzers Omnistar.
adsorption_desorption
Three volumetric mono-sampler adsorption-desorption devices Sorptomatic 1990 from Fisons Instruments .
adsorption_desorption micromeritics
A multi-sampler adsorption-desorption volumetric device from Micromeritics .
mercury porosimetry
Three Pascal 140 (low pressure) and three Pascal 240 (high-pressure, up to 2000 bars) mercury porosimeters from Thermo Scientific .
pycnometer
Helium pycnometer.
Dektak profilometer
Dektak 150 profilometer from Bruker for thin-film characterization (thickness and roughness).
viscosimeter
Two Brookfield viscosimeters for measuring the viscosity of sols.

Electrochemical Characterization Equipment

The Electrochemistry team of the NCE has become specialized in the full characterization of electrochemical performances of novel materials for Li-ion batteries. These include new compounds for anodes, cathodes as well as solid electrolytes. Such characterizations cover the preparation of the materials, their processing and shaping as well as their characterizations in half-cells.

For the deposition on current collectors, coatings on different substrates are realized starting from precursor sols either by dip-coating, spin-coating or a home-made robotic spray.

dip coater spin coater inkspray robot
Dip coater (KSV NIMA), Spin coater (MB SC 200), Homemade robotic spray

When starting from pre-synthesized particles, the deposition on current collectors is realized either by spray coating or by bar-coating (with or without heating the substrate).

electrochemistry equipment electrochemistry equipment
Barcoaters (Elcometer 4340) without and with heating table

The electrochemical performance of the developed materials is assessed upon assembling half-cells, with metallic lithium as reference electrode. For that purpose, the assemblies are realized either in coin-cells (using a crimping machine) or in home-made Swagelok-type battery bodies that feature a controlled torque, so a controlled pressure on the electrode-separator-electrode assemblies.

crimping machine Swagelok cells
Crimping machine for coin cell MSK-110 (MTI) and homemade cylindrical Swagelok type cells

The electrochemical characterizations (charge/discharge curves, cycling stability, internal resistance,...) of the developed materials are realized using high-performance potentiostats. For routine and screening measurements, the laboratory possesses two 16-channels multipotentiostats that allow for the characterization either inside the glovebox (controlled inert atmosphere) or inside a climate chamber (controlled temperature and humidity).

glove box coin cells coin cells potentiostat
Glove box (Mbraun MB 200B), coin cells cycling in glove box, coin cells cycling in climate chamber (Vötsch VC 4018) and 16 channels potentiostat (Bio-Logic VMP3)

Fuel cells

The NCE is involved in several projects dealing with the preparation and characterization of novel materials as different elements of low temperature PEM fuel cells. These studies require the characterization of their performance when integrated in a single cell fuel cell or a fuel cell stack.

Pt-based electrocatalysts on novel carbon supports are prepared via modified impregnation methods so as to achieve enhanced performance for both the anode and cathode reactions at lower catalyst loadings. Highly dispersed carbon xerogel supported Pt nanoparticles catalysts can be prepared by the strong electrostatic adsorption (SEA) method or the charge enhanced dry impregnation (CEDI) method using various reduction methods such as hydrogen reduction or borohydride reduction.

The physicochemical characterization of these catalysts is performed by ATG-DSC, ICP-AES, XRD and TEM. These measurements provide information concerning Pt loading and particle size and dispersion.

The electrochemical characterization of the prepared catalysts is performed in a three-electrode cell with a rotating disk electrode, where several electrochemical measurements are carried out in order to determine the catalyst specific activity or the electroactive surface area.

tree-electrode cell wuth rotating electrode
Three-electrode cell with rotating disk electrode

For the electrode fabrication process, the prepared catalysts are deposited by bar-coating or spray coating, either on a plain polymer film so as to assess the homogeneity of the deposition process with the use of a profilometer, or on the electrolytic polymer membrane so as to prepare a catalyst coated membrane (CCM). The CCM is then compressed together with the Gas Diffusion Layers (GDL) on either side in order to prepare a Membrane Electrode Assembly (MEA). The MEA can be then inserted in a single cell fuel cell assembly for further characterization of its performance.

inkspray robot barcoater
Custom-built robotic spray and Bar coating with Elcometer 4340
presses
Instrumented presses used for the MEA fabrication.

Other elements of a PEM fuel cell are also characterized, such as the electrolytic polymer membrane or the bipolar plates. In order to estimate the corrosion resistance of stainless steel and coated stainless steel bipolar plates and their stability in the corrosive environment of a fuel cell, corrosion tests are conducted in a Biologic corrosion cell. Modifications on the surface of the bipolar plates due to corrosion can also be identified by estimating the Interfacial Contact Resistance (ICR) between the bipolar plates and the GDL before and after the corrosion tests, by means of Electrochemical Impedance Spectroscopy (EIS). The same technique (EIS) is used in order to measure the conductivity of commercial and prepared electrolytic membranes before the MEA fabrication.

corrosion kit
EL-FLAT BioLogic corrosion cell kit.

The final step of the characterization of the different fuel cell elements is performed with their integration in a fuel cell assembly. For these exdperiments, two setups are available, one where the assembly operates in a controlled temperature environment and one where the fuel cell is heated externally. Gas flow rates, humidification and temperature, as well as the assembly operating temperature and pressure are controlled and monitored by custom-built test stations and the cell performance under various operating conditions is monitored by high-performance potentiostats.

single-cell assembly paxitech BioLogic VMP3
Single-cell fuel cell assembly, Paxitech fuel cell, and BioLogic VMP3 potentiostat.
fuel cell in oven fuel cell heating cartridge
FC assembly in a controlled temperature oven (Binder) and with cartridges heating.

A test station that will allow for the realization of performance tests of fuel cell stack assemblies up to 5 kW is currently under construction.

General equipment for Synthesis and shaping of materials

glove box
Glove box.
ball miller
Ball miller.

Chemical reactors

nitridation reactor
Nitridation reactor.
photocatalysis reactor
Photocatalysis reactor 1.
photocatalysis reactor
Photocatalysis reactor 2.
CCVD nanotube reactor
Rotary kiln reactor for the kg-scale synthesis of carbon nanotubes by catalytic CVD.
tar catalytic reforming reactor
Experimental installation for catalytic reforming of tars.