Application of a novel Split&Pool-principle for the fully combinatorial synthesis of functional inorganic materials

Abstract

In the field of high throughput experimentation (HTE) related to materials sciences and catalysis a large number of test methods and analytical tools have been developed in the last years. As a consequence of the increasing parallelization and integration of the reactor and analysis systems, the requirements for the synthesis methodologies are rising extremely: smallest amounts of material samples of, i.e. different multi component mixed oxides in the μg- or gram-range have to be synthesized reproducibly and fully automated. In order to meet these challenges, the combination of different expert skills in the fields of inorganic synthesis, robotics, automation and related fields are of major importance. Real combinatorial chemistry, meaning the combinatorial permutation of element combinations or synthesis parameters involving statistical synthetic approaches leading to true combinatorial libraries of new functional materials supported by computer aided designs, was not presented yet in scientific community of inorganic solid state chemistry. We present here for the first time a tool for synthetic chemistry, originally developed with the application focus on molecular libraries, to produce inorganic solid state materials. With the so-called Split&Pool (S&P)-principle, it is possible to produce highly diverse materials libraries in the range of 10 3–10 8 samples with a very simple workflow. Characterization with μ-XRF, optical microscopy and other analysis tools prove the potential of the presented synthesis technique. A powerful enhancement of this synthesis tool is our recently presented “single bead reactor” (SBR), allowing efficient testing of the libraries created by the Split&Pool methodology.