Nowadays clean and renewable energy supply is one of the biggest challenges for the mankind. Hydrogen is often proposed as a prospective fuel of the future, but there are numerous scientific and technological problems to be solved on the way to the hydrogen economy. One of them is hydrogen production. The most efficient way of hydrogen production would be direct water splitting using solar energy. Photoelectrode materials for solar water splitting cells must fulfill a number of requirements: an appropriate band gap, band edge positions, high specific surface area, long term chemical and mechanical stability, low cost of fabrication. In this work, porous thin film electrodes for photoelectochemical solar water splitting were developed by the dealloying approach. The search for materials with optimal physical and photoelectrochemical properties inevitably involves fabrication and characterization of a large number of samples. In order to accelerate this search, combinatorial and high-throughput methods were used for fabrication and investigation of the thin film materials libraries.