Controlling the oxidation state of iron and the crystal structure of iron containing compounds is the key to improved materials such as iron oxide nanoparticles for cancer treatment or heterogeneous catalysis. Iron oxides contain iron in different oxidation states and form different phases for one valence state (α-Fe3+ 2O2- 3, β- Fe3+ 2O-3 2, etc.). Chemical vapor synthesis (CVS) allows the reproducible production of pure nanocrystals with narrow size distribution where particle formation and growth take place in the gas phase. Through the controlled variation of synthesis parameters CVS enables the synthesis of diverse iron oxide phases. In this study the energy for the CVS process is supplied by a hot wall furnace and a microwave plasma. The advantage of an plasma reactor as the first CVS stage is the fast and complete precursor decomposition at low temperatures. This results in a larger process window for the hot wall reactor in the second stage. The nanoparticles are examined regarding their structure, surface and valence by XRD and TEM.