Numerous studies have been performed in the field of Nd-Fe-B based permanent magnets since they possess excellent hard magnetic properties. The magnetic properties are closely related to the structure, phases present, processing route etc. High performance hard magnets can obtain their desired large energy product by interaction of magnetic moments at the nanoscale. Therefore, developing nanostructured Nd-Fe-B based magnets requires the study of novel synthesis techniques, microstructure and properties. Conventional physical techniques have limitations of inhomogeneity, contamination, poor control of microstructure and high cost due to the use of elemental rare earth metals. On the other hand, bottom-up chemical methods offer better control of structure at the nanoscale. The use of metal salts as precursors significantly reduces the cost. Hence, a cost-effective, bottom-up, microwave synthesis method is promising to produce homogenous particles by uniform microwave heating. The main objective of this project is the study of the microwave synthesis of Nd-Fe-B based magnets. The processing parameters, reaction mechanisms, characterization and property evaluation of these materials were carried out. Nanostructured Nd-Fe-B particles were prepared by microwave combustion and reduction diffusion. Microwave combustion resulted in a transformation from metal salts to mixed metal oxides consisting of CoFe2O4, NdFeO3, Nd3FeO6 and Fe2O3. Nd2(Fe,Co)14B nanoparticles were obtained by the reduction diffusion process, in which the mixed metal oxide was reduced by CaH2. The effects of processing parameters on properties and structure were studied. It was found that the structure and magnetic properties can be controlled by the microwave power. Higher microwave power resulted in larger grain size. The coercivity of the particles increased from ~ 6 kOe to ~9 kOe when the grain size increased from ~ 20 nm to ~ 60 nm. A range of reduction-diffusion annealing times was also tested. The highest energy product was obtained for reduction diffusion at 800 °C for 2 h. The CaO byproduct was removed by different chemicals. The optimum chemical was found to be NH4Cl (dissolved in methanol), which eliminated the use of water, thus avoiding the vigorous reaction between CaO and water.