Ammonium perrhenate (APR) is an intermediate product in rhenium extraction process, by which it is possible to produce rhenium powder. The main purpose of this research is to investigate the behaviour of APR in different atmospheres as a part of reduction process. In this research, differential thermal analysis and thermo gravimetric analysis are used to peruse the APR behaviour in nitrogen, argon and hydrogen atmospheres. Also for further validation, X-ray diffraction analysis and the scanning electron microscopy were used. The results indicate that APR behaves almost the same in the argon and nitrogen atmospheres. In these conditions, APR decomposes to rhenium oxides during thermal decomposition. However, APR in hydrogen reductive atmosphere is reduced to pure rhenium powder without any reactions. SEM images showed that hydrogen reduced APR had a spherical morphology, but on the other hand the directly reduced rhenium powder in hydrogen atmosphere showed flake morphology.