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Various aqueous citrate electrolyte compositions for the Ni-Mo electrodeposition are explored in order to deposit Ni-Mo alloys with Mo-content ranging from 40 wt% to 65 wt% to find an alloy composition with superior catalytic activity towards the hydrogen evolution reaction (HER). The depositions were performed on copper substrates mounted onto a rotating disc electrode (RDE) and were investigated via scanning electron microscopy (SEM), X-ray fluorescence (XRF) and X-ray diffraction (XRD) methods as well as linear sweep voltammetry (LSV) and impedance spectroscopy. Kinetic parameters were calculated via Tafel analysis. Partial deposition current densities and current efficiencies were determined by correlating XRF measurements with gravimetric results. The variation of the electrolyte composition and deposition parameters enabled the deposition of alloys with Mo-content over the range of 40-65 wt%. An increase in Mo-content in deposited alloys was recorded with an increase in rotation speed of the RDE. Current efficiency of the deposition was in the magnitude of <1%, which is characteristic for the deposition of alloys with high Mo-content. The calculated kinetic parameters were used to determine the Mo-content with the highest catalytic activity for use in the HER.
For this study gas diffusion electrodes (GDE) with low platinum loading are prepared for the application as anode in polymer electrolyte membrane fuel cell (PEMFC) systems based on hydraulic compression. As catalyst support material, carbon nanofibers (CNF) are investigated because of their high specific surface area and high graphitization degree. The electrode preparation is optimized by an economic and environmental friendly pre-treatment process in oxygen plasma. For GDE manufacture an ink containing oxygen plasma activated CNFs as well as hydrophilic polymer is used. After spray coating of this CNF ink on a graphitic substrate, platinum is deposited using the pulse plating technique. Preliminary results showed a considerable improvement of CNF dispersibility as well as an increased amount and an optimized morphology of the deposited platinum. Morphology and microstructure are observed by scanning electron microscopy as well as transmission electron microscopy. Platinum loading is determined by thermogravimetric analysis to be in the range of 0.01 mg cm-2 to 0.017 mg cm-2. Furthermore, MEAs are prepared from these GDEs and testing is performed in a novel modular fuel cell test stack based on hydraulic compression. Technical information about stack design and functions is given in this work.
This work deals with the preparation and investigation of PEM fuel cell electrodes, which are obtained using graphene related material (GRM) serving as catalyst support for platinum nanoparticles. Applied GRM are used for the preparation of suspensions in four distinct mixing ratios. Two sorts of GRM have been investigated: carbon nanofibers (CNF) and graphene oxide (GO). Utilized CNFs provide a superior graphitization degree of about 100%, which leads to both high corrosion resistance and low ohmic resistance in PEM fuel cells.
For electrode preparation a GRM containing layer serving as catalyst support is applied onto a gas diffusion layer (GDL). Prior to GRM suspension and deposition onto a GDL, the graphene structures are functionalized by plasma treatment. Due to this step, an improved hydrophilic behavior for facilitating suspension preparation is achieved. In addition, a subsequent platinum nanoparticle deposition by pulsed electrodeposition process is optimized.
In polymer electrolyte membrane fuel cells (PEMFC) noble metal nano particles are deposited on graphitic supports serving as electrocatalysts for devices with high power density. In this study anodes are analysed with low platinum loading of about 0.1 mg cm-2. These electrodes are prepared by carbon nano fibres (CNF) decorated with platinum nano particles. For electrode manufacturing two sorts of fibres, which are produced in an industrial scale, are used with different graphitisation degree and surface area. CNF layers are applied on commercially available graphitic substrate by spray coating which leads to a porous structure with high surface area. Subsequently, platinum deposition is achieved by pulsed electroplating for an improved platinum utilisation in PEMFC electrodes. Spray coating and platinum deposition are assisted by a previous oxygen plasma activation process. Prepared anode material is characterised by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction spectroscopy (XRD), X-ray fluorescence spectroscopy (XRF) and thermogravimetry (TGA). Electrochemical analyses (cyclic voltammetry and corrosion test) are carried out in 0.5 M sulphuric acid. The effect of graphitisation degree of carbon nano fibres on the performance of prepared electrodes is investigated in-situ in a PEM fuel cell test bench.
Platinum is one of the most effective electro catalysts for PEMFCs (proton exchange membrane fuel cells), but because of its prohibitive price, the use of this metal in industrial purposes is limited. As a consequence, during last years, several materials have been investigated, in order to obtain an efficient catalyst for both ORR (oxygen reduction reaction) and HOR (hydrogen oxidation reaction), which can replace the expensive platinum but preserving the same properties: high electrical conductivity, structural stability and good corrosion resistance. Moreover, one of the most important parameters for catalyst materials is the electrochemical surface area (real surface area), which has a strong influence on the reaction rate and also on the current density.
CNFs (carbon nanofibers) are considered to be a promising catalyst support material due to their unique characteristics, excellent mechanical, electrical and structural properties, high surface area and nevertheless, good interaction with platinum particles.
The possibility of preparing CNFs decorated with platinum by electrochemical methods was tested, using a hexachloroplatinic solution bath. The experiments were carried out with the aid of a Potentiostat/Galvanostat MMate 510, in a three – electrode cell.
The aim of the present work was to determine the electrochemical surface area of the CNFs – Pt catalysts, using an electrochemical method. The obtained results correlate very well with the particles size and distribution of platinum, analyzed by SEM (scanning electron microscopy) respectively with the quantity of deposited platinum determined by TG (thermo gravimetrical analyses). Cyclic voltammetry is a suitable method for estimation of the real surface area for catalyst particles.
In state of the art polymer electrolyte membrane fuel cells (PEMFC) rare and expensive platinum group metals (PGM) are used as catalyst material. Reduction of PGM in PEMFC electrodes is strongly required to reach cost targets for this technology. An optimal catalyst utilisation is achieved in the case of nano-structured particles supported on carbon material with a large specific surface area. In this study, graphitic material in form of carbon nanofibres (CNFs) is decorated with platinum (Pt) particles serving as catalyst material for PEMFC electrodes with low Pt loading. For electrode preparation CNFs have been previously activated by means of radio frequency induced oxygen plasma. This kind of treatment results in formation of functional groups on the CNF’s surface which directly influences the characteristics of subsequent Pt particle deposition. Different plasma parameters (plasma power, gas flow or exposure time) have to be set in order to achieve formation of oxygen containing functional groups (hydroxylic, carboxylic or carbonylic) on the CNF’s surface. In the frame of this experimental work, electrodes are investigated in respect of optimal morphology, microstructure as well as electrochemical properties. Therefore, samples were characterised by means of scanning electron microscopy combined with energy dispersive X-ray analysis, transmission electron microscopy, thermogravimetry, X-ray diffraction, X-ray fluorescence as well as polarisation measurements.
To further increase platinum utilisation in PEM fuel cells CNFs are investigated as catalyst support material due to the CNF’s high specific surface area. Furthermore, CNFs provide suitable properties concerning corrosion resistance as well as electrical conductivity in contrast to conventional carbon supports.
This work presents the results of an electrode preparation procedure based on O2 plasma activated CNFs. The plasma treatment leads to CNF dispersibility in alcohol/water for a spray coating process. Furthermore, O2 plasma activation enhances metal deposition on the CNF’s surface. Pulse plating procedure as well as wet chemical metal synthesis have been used for particle deposition. For pulse plating a potentiostat/galvanostat type MMates 510 AC from Materials Mates, Italy has been used. Electrode morphology has been determined in SEM type XL 30 ESEM from Philips, The Netherlands.
The membrane electrode assemblies (MEA) for polymer electrolyte membrane fuel cells (PEMFC) developed at the Westphalian Energy Institute are based on oxygen plasma activated carbon nanotubes (CNT) doped with platinum particles. For electrode preparation an ink is used containing the activated CNTs as well as hydrophobic and hydrophilic material in solved form. After this ink is sprayed onto a graphitic substrate platinum particles are deposited by pulse plating method, where the plasma activation enhances CNT dispersibility as well as platinum deposition. This materials mixture is structured in nanoscale with the aim to increase the catalyst particles’ specific surface. For low reactance at operation, homogeneous compression of the MEA’s layers is necessary within a PEMFC. A novel stack architecture for electrochemical cells, especially PEMFC as well as PEM electrolysers, has been developed in order to achieve ideal cell operation conditions. Single cells of such a stack are inserted into flexible slots that are surrounded by a hydraulic medium which is pressurised during operation in order to achieve an even compression and cooling of the stack’s cells. With this stack design it has been possible to construct a test facility for simultaneous characterisation of several MEA samples. As compression and temperature conditions of every single sample are the same, the effects of e.g. different electrode configurations can be investigated with the novel test system.