High-Throughput Materials Discovery by Inkjet-Printing of Composition Spread Libraries
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High-Throughput Materials Discovery by Inkjet-Printing of Composition Spread Libraries Klaus Stoewe, Wilhelm F. Maier, Boris Weidenhof Technische Chemie, Universitaet des Saarlandes, Campus C4.2, 66123 Saarbruecken, Germany ABSTRACT High-throughput synthesis and screening rely on structurally diverse catalyst libraries. As a consequence of increased parallelization and integration of reactor and analysis systems, the requirements for new synthesis methodologies include even smaller amounts of samples, e.g. different multi-component mixed oxides in the mg or even µg-range have to be prepared reproducibly and fully automated. We tried to bring solution chemistry, composition spread libraries and a very high sample density together within one approach and tested inkjet printing of materials libraries using sol-gel recipes as synthesis method. Inkjet printing allows the deposition of liquid volumes in the pL range thus enabling the deposition of very small catalyst amounts. For the application of this technique in sol-gel chemistry several restrictions have to be handled, such as viscosity limitations of the printing head. Parameters as solvent, solvent amount, metal precursors, metal salt concentrations, deposition sequences etc. as well as gelification procedures have to be optimized. Catalytic screening relies on porous samples with high surface area to get conversions, which can be detected by HT screening methods. Thus, additionally the recipe itself as well as the support structure has to be optimized. In our first tests we used emission corrected IR thermography for screening. . INTRODUCTION High-throughput technologies (HTT) are now widely accepted for speeding up the discovery and optimization of new materials and catalysts.1 By iteration of design of experiment (DoE), parallel library synthesis, high-throughput screening of the libraries and data mining a specific objective criterion such as a desired conversion or selectivity can be approached. The workflow of high-throughput experimentation (HTE) offers automation, investigation of large parameter spaces as well as a high degree of reproducibility. As for catalysts a high surface area is indispensable, most synthesis methods focus on solution based methods, such as impregnation of porous or nano-scaled solid supports or sol-gel syntheses leading to porous mixed oxide or nitride powders. The number of samples to be synthesized using pipetting robots is limited only by rack size or screening capacity. For compositional optimization of leads so-called compositions spread libraries can be prepared. Here, the catalyst compositions can be varied over the whole phase space of multinary systems in analogy to thin film library synthesis by physical or chemical vapour deposition techniques, where masking and annealing are used to produce continuous composition gradient libraries. These masking techniques allow the generation of high sample density limited only by the spatial resolution of the analysis techniques used to characterize the composition spread library. Wit
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