Looking at the energy crisis, installation of nuclear power station is become need of the world. But the harmful effects of these technique has already evidenced by the event happened in Japan. So it is very much necessary to monitor the leakages or flow of the radiations from the plant to the outer environment. In today's world, radiation measurements using thermo luminescence (TL) or optically stimulated luminescence (OSL) has become an important tool in nuclear & medical research. However the monitoring using TL/OSL depends on the sensitivity of materials used. Till date, very few materials have found the commercial value and are very costly. So it becomes very necessary to get alternative to those materials. in this book, we proposed synthesis techniques of some new rare earth activated TL/OSL materials and studied them. However, the materials suggested in the book have sensitivity more than the commercial material and may found importance in personal as well as environmental radiation monitoring. This book helps a lot to the researchers who are currently engaged in the field of research on radiation monitoring and synthesis of TL/OSL materials.