Silicon, germanium, and compound semiconductors, among which silicon carbide, gallium arsenide and gallium nitride are the most representative examples, play a withstanding role in the world economy, since they were and still are the keys for the advancement of modern microelectronics and optoelectronics, with a wealth of sister technologies relevant for renewable energy solutions and advanced spectroscopy applications. This textbook will cover the synthesis, spectroscopic characterisation and optimisation of semiconductor materials, accounting for the most recent developments in the field of nanomaterials. It will be of great interest for scholars and instructors to have the chance to look at semiconductor science with a basic chemical approach. Homopolar semiconductors (silicon and germanium) are examined first, considering the role of these materials in modern microelectronics and in photovoltaics. Compound semiconductors (for example, carbides, arsenides, tellurides, nitrides) are also discussed in detail, considering that the chemistry of their preparation is even more critical and their role in photonic applications is strategic. Authored by a leading expert in the field, this easily accessible text is appropriate for advanced undergraduates and postgraduates studying materials science and technology.