@PhdThesis{dbt_mods_00026038, author = {Hahn Dr.-Ing., Sebastian}, title = {Grundlagenuntersuchungen zur Wirkweise und Kontrolle von Katalysatoren in autokatalytischen B{\"a}dern zur Metallabscheidung}, year = {2015}, month = {May}, day = {21}, keywords = {Str{\"o}mungszelle; RDE; QCM; NiP; autokatalytische Abscheidung; Stabilisatoren; Blei; Thioharnstoff; galvanostatische Aufl{\"o}sung}, abstract = {In this work, a flow cell for in-situ microgravimetrical and electrochemical investigationsis introduced and characterized. The well understood homogeneous diffusionboundary layer of a rotating disk electrode (RDE) is well suited for the study of electrochemicalprocesses, but the in-situ measurement of layer thickness is not possible.This parameter is important for the characterization of deposition processes and canbe measured with a quartz crystal microbalance (QCM), but rotation for generating ahomogenous flow and diffusion boundary layer is hardly feasible. Instead, we builda combination of a flow cell with a QCM to allow the investigation of diffusioneffects on electrochemical metal deposition speed.For the flow cell design and optimization, the ``Comsol Multiphysics`` software wasused to calculate flow conditions and concentration gradients at the electrode. Calculationresults were checked by measuring current limiting density values of theredox system Hexacyanoferrat II/III in our flow cell/QCM combinations and comparingthem to values obtained with an RDE.The main application of the experimental assembly is the characterization of theautocatalytic NiP-deposition. In this process, stabilizers are used to prevent the spontaneousdecomposition of the electrolyte. The inhibition of the deposition rate as afunction of stabilizer concentration and its dependence on flow conditions is examined.Lead and thiourea are used as stabilizers in this work.In the same experimental arrangement, the electrochemical dissolution potential ofthe previously deposited NiP-layer was measured in a variety of dissolution electrolytes.It was found that the NiP-layer's dissolution potential is influenced by the typeof stabilizer, its concentration and the flow conditions during the deposition step.After optimizing the dissolution electrolyte, the measurement of the dissolutionpotential allowed the estimation of the thiourea concentration in the depositionelectrolyte in a range between 0-0,5 ppm and >1 ppm.}, url = {https://www.db-thueringen.de/receive/dbt_mods_00026038}, url = {http://uri.gbv.de/document/gvk:ppn:825836867}, file = {:https://www.db-thueringen.de/servlets/MCRZipServlet/dbt_derivate_00031780:TYPE}, language = {de} }