ULiège: Nanomaterials, Catalysis, Electrochemistry (NCE)

General expertise of the research group

The Nanomaterials, Catalysis, Electrochemistry (NCE) laboratory, which is part of the Research Unit in chemical Engineering of ULiège, has developed a wide expertise in the conception and set-up of devices linked to chemical engineering based on an integrated approach, from the preparation of materials and their extensive characterization to trials in prototype (continuous) reactors. The first part of the activities concerns the design and preparation of new materials with controlled pore texture at the nanoscale. The mastering of the synthesis process enables to perform scale-up studies. Activities about materials also deal with shaping or assembly for industrial applications. The second part of the activities concerns the building of test benches dedicated to the determination of the materials properties (activity of catalysts, performances of fuel cell or battery electrodes) and to the set-up of pilot devices for the production of a given material.

Since 2009, electrochemical engineering applications such as fuel cells constitute a major axis of the research at NCE, and is currently driven by its recognized expertise in the synthesis and study of carbon materials and catalysts. In all cases, the goal is to include new materials, often with specific nanostructuration, first in (composite) electrodes, then in full electrochemical devices. In addition, the competences in catalyst manufacturing and characterization acquired in the past in the framework of other applications is widely used here to combine the advantages of mastered pore texture and high metal dispersion. It is particularly critical in Proton Exchange Membrane fuel cells given that the cell performance is related to both the specific activity of the catalyst and the mass transport properties of the electrode.

In order to study fuel cells, the NCE laboratory has developed remarkable equipment for the manufacture and in situ characterization of Proton Exchange Membrane fuel cell components, among which fully automated house-built monocell and stack test benches, along with all the necessary equipment to manufacture electrodes and Membrane-Electrodes Assemblies from their components; those operations are performed in a very reproducible manner which allows for very accurate characterization.

Thanks to several large-scale projects and related investments, the laboratory is able to cover the complete manufacture chain, from basis materials (including catalysts) to the complete cell that can be further integrated in a user system.

Specific hydrogen- related expertise & research topics

• Research in the field of the constituent materials of PEM fuel cells (catalysts, membranes, bipolar plates), from their manufacturing to the study of their aging in representative conditions.
• Characterization of materials and assemblies for PEM fuel cells.
• Development of manufacturing techniques for PEM fuel cell components.
• Development of test-benches for the characterization of materials and cells, for mobile and stationary applications.

Available equipment/tools:

• All the necessary equipment to manufacture and characterize carbon-supported metal and alloy catalysts, from the carbon synthesis to the metal deposition
• Electrochemical characterization tools: 3-cell electrodes, rotating disk electrodes (RDEs), rotating ring disk electrodes (RRDEs), corrosion cells, dedicated (and adapted) potentiostats (4, among which 2 adapted for RRDEs)
• Tools for the manufacturing and characterization of Membrane-Electrodes Assemblies (MEAs– fuel cells) and electrodes: fully home-made (and versatile) automated spray-coater, one industrial spray-coater, two bar-coaters (one with heating platform), instrumented hot presses, high performance profilometer, cells for electrical and ionic conductivity measurements (adapted to composite electrodes madeof ionic and electronic conductors like in fuel cell MEAs)
• Equipment for the measurement of contact resistance between layers of materials (under pressurization)
• Fully instrumented fuel cell test benches: 2 hydrogen/air 5 cm x 5 cm benches. A third test-bench will be acquired in 2024
• One instrumented stack test bench, up to 10 kWel.

Participating in FL/B/EU funded projects with H2 related research:

• 2012-2018: European project FCH-JU-2011-1- SWARM (“Demonstration of Small 4-Wheel fuel cell passenger vehicle Applications in Regional and Municipal transport”). Collaboration between 20 European partners (public and private); Coordinator: PLANET (Planungsruppe Energie & Technik GbR, Germany). Total budget: €19,665,734 (EC contribution: €6,978,279)- ULiège-NCE budget: €330,420 (EC contribution: €216,630).
• 2014-2018: ENERGINSERE call– HYLIFE project (agreement no. 1410135): “Long-life materials for PEM hydrogen-air fuel cells”. Promoter: N. Job (ULg-LGC), in partnership with ULB (Pr. F. Reniers), UNamur (Pr. J.-J. Pireaux), Materia Nova (M. Poelman) and INP-Grenoble (F. Maillard). Overall budget: €2,431,118.44. ULiège-NCE budget: €906,707.50.
• 2014-2017: IDS-FunMat project 2014/04, doctoral thesis under joint supervision ULg– INP-Grenoble. Promoters: N. Job, F. Maillard (INP-Grenoble): “Hollow nanoparticles for low cost, high activity and durability PEMFC electrocatalysts (HOLLOW)”. Doctoral scholarship (3 years).
• 2014-2021: FEDER, “Multifunctional films” portfolio- INOXYPEM project: “Prototyping of coated steel bipolar plates for PEM fuel cells”. Promoter: N. Job (ULg-LGC) in partnership with CRM-Group (A. Lafort), UNamur (J.-J. Pireaux), ULiège-LTAS (P. Duysinx), CENAERO (C. Goffaux). Overall budget: €1,831,257ULiège-NCE budget: €675,279.
• 2016-2019 : Walloon Region ENERGIE– HYSTACK (agreement n°1550260) : « Design of a fuel cell test bench for stacks up to 10 kW ». Budget : €396.037,65.
• 2018-2021 : F.R.S.-FNRS– HOLCAT (PDR/OL T.0247.18) : « Hollow PtCo catalysts supported on carbon xerogels for Proton Exchange Membrane fuel cell cathode ». Budget : €204.000.
• 2021-2026: Energy Transition Fund Project, ETF-BE-HYFE– Belgian Hydrogen Fundamental Expertise. Structuring hydrogen research network in Belgium: funding of 16 collaborative doctoral theses across the entire hydrogen value chain. Coordinator: UGent. Participants: KULeuven, UC Louvain, UAntwerpen, UHasselt, VITO, IMEC, VKI, VUB, ULB, ULiège, UMons, WaterstofNet, TWEED. 1 thesis funded at NCE, 0.5 thesis funded at PEPs (UR ChemEng). Total budget: €4,507,809. ULiège-NCE budget: €324,300.

Main relevant publications

1. Book chapters:
   1. M. Chatenet, N. Job, F. Maillard. Basics of PEMFC including the use of carbon-supported nanoparticles. In: New and Future Developments in Catalysis; Catalysis by Nanoparticles. S. Suib (Ed.), 1st edition, Elsevier, 2013, pp. 401-423, ISBN: 9780444538741.
   2. F. Maillard, N. Job, M. Chatenet. Approaches to synthesize carbon-supported platinum-based electrocatalysts for proton-exchange membrane fuel cells. In: New and Future Developments in Catalysis. Batteries, Hydrogen Storage and Fuel Cells; S. Suib (Ed.), 1st edition, Elsevier, 2013, pp. 407-428, ISBN: 9780444538802.
   3. N. Job. Carbon gels for electrochemical applications. In: Organic and carbon gels: from laboratory synthesis to applications, M. Aegerter, M. Prassas (Eds.), Series Advances in Sol-Gel Derived Materials and Technologies, Springer International Publishing, 2019, pp. 149- 189. ISBN: 978-3-030-13897-4.
2. Articles in international journals (selected):
   1. F. L. Deschamps, J. G. Mahy, A.F. Léonard, N. Job. Rotating disk electrode measurements on low and high loading catalyst layers: Diffusion limitations and application to Pt catalysts supported on porous micrometric carbon xerogel particles designed for proton exchange membrane fuel cells. Journal of Electroanalytical Chemistry 933 (2023) 117279.
   2. F. L. Deschamps, J. G. Mahy, A.F. Léonard, S.D. Lambert, A. Dewandre, B. Scheid, N. Job. A practical method to characterize PEMFC catalyst layer topography: application to two coating techniques and two catalyst supports. Thin Solid Films 695 (2020) 137751.
   3. A. Zubiaur, N. Job. Streamlining of the synthesis process of Pt/carbon xerogel electrocatalysts with high Pt loading for the oxygen reduction reaction in proton exchange membrane fuel cells applications. Applied Catalysis B 225 (2018) 364-378.
   4. P.Y. Olu, N. Job, M. Chatenet. Evaluation of anode (electro)catalytic materials for the direct borohydride fuel cell: methods and benchmarks. Journal of Power Sources 327 (2016) 235-257.
   5. P.-Y. Olu, F. L. Deschamps, G. Caldarella, M. Chatenet, N. Job. Investigation of platinum and palladium as potential anodic catalysts for direct borohydride and ammonia-borane fuel cells. Journal of Power Sources 297 (2015) 492-503.
   6. N. Job, S. D. Lambert, A. Zubiaur, C. Cao, J.-P. Pirard. Design of Pt/carbon xerogel catalysts for PEM fuel cells. Catalysts 5 (2015) 40-57. A. Zubiaur, M. Chatenet, F. Maillard, S. Lambert, J.-P. Pirard, N. Job. Using the Multiple SEA method to synthesize Pt/Carbon xerogel electrocatalysts for PEMFC applications. Fuel Cells 14 (2014) 343-349.
   7. N. Job, M. Chatenet, S. Berthon-Fabry, S. Hermans, F. Maillard. Efficient Pt/carbon electrocatalysts for Proton Exchange Membrane fuel cells: avoid chloride-based Pt salts! Journal of Power Sources 240 (2013) 294-305.
   8. N. Job, S. Lambert, M. Chatenet, C.J. Gommes, F. Maillard, S. Berthon-Fabry, J.R. Regalbuto, J.-P. Pirard. Preparation of highly loaded Pt/carbon xerogel catalysts for PEM fuel cells by the Strong Electrostatic Adsorption method. Catalysis Today 150 (2010) 119-127.
   9. N. Job, F. Maillard, J. Marie, S. Berthon-Fabry, J.-P. Pirard, M. Chatenet. Electrochemical characterization of Pt/carbon xerogel and Pt/carbon aerogel catalysts- first insights into the influence of the carbon texture on the Pt nanoparticles morphology and catalytic activity. Journal of Materials Science 44 (2009) 6591–6600.
   10. N. Job, S. Berthon-Fabry, M. Chatenet, J. Marie, M. Brigaudet, J.-P. Pirard. Nanostructured carbons as catalyst supports for PEM fuel cell electrodes. Topics in Catalysis 52 (2009) 2117-2122.
   11. N. Job, J. Marie, S. Lambert, S. Berthon-Fabry, P. Achard. Carbon xerogels as catalyst supports for PEM fuel cell cathode. Energy Conversion and Management 49 (2008) 2461-2470.
3. PhD thesis:
   1. P.-Y. Olu (2015), Study of the anode for the Direct Borohydride Fuel Cell, 201. Co-supervision with M. Chatenet (INP-Grenoble, France), IDS-FunMat program. https://hdl.handle.net/2268/188808
   2. T. Asset (2017). Hollow nanoparticles for low cost, high activity and durability PEMFC electrocatalysts. Co-supervision with F. Maillard (INP-Grenoble, France), IDS-FunMat program. https://hdl.handle.net/2268/214971
   3. A. Zubiaur (2017). Development of new catalysts for Proton Exchange Membrane Fuel Cells (PEMFCs). https://hdl.handle.net/2268/216303
   4. Deschamps (2022). Mise au point de méthodes d’étude de catalyseurs supportés sur carbones nanostructurés pour piles à combustible à membrane échangeuse de protons. https://hdl.handle.net/2268/289356