The ever-increasing desire for more energy attainable from a smaller volume of matter has driven researchers to explore advanced materials at the molecular size. Magnetic materials at the nanometer size scale have been the subject of enormous research effort worldwide for more than half a century. Different magnetic nanoparticles have shown different behavior in the absence and presence of an external magnetic field, which has led them to be categorized as soft or hard magnets. Applications range from medical and biomedical devices to magnetic recording media and magnetic sensing have emphasized the importance of this class of materials. Soft magnetic phases have found application in power generation and magnetic targeted drug delivery, while hard magnets have been subject of extensive research for application as energy storage media. Discovery of the exchange-coupling phenomenon between two adjacent hard and soft magnetic phases has attracted scientists to develop advanced materials for energy storage with no usage of fossil fuels: clean energy. In this Dissertation, synthesis of pure phase, soft FeCo nanoparticles with high magnetic moment and hard phase CoxC nanoparticles possessing high coercivity is reported. The polyol method (chemical co-precipitating at polyhydric alcohol as reducing agent) is used to make FeCo and CoxC nanoparticles and the effects of important reaction kinetics parameters on the structure and magnetic properties of the products are studied. Careful analysis of correlations between these parameters and the properties of the magnetic particles has made synthesis of FeCo and CoxC nanoparticles with desired properties possible. Fabrication of MnAlC-FeCo heterostructures as a rare earth-free alternative for high-performance permanent magnet is also reported. To synthesize MnAlC-FeCo, mechanical alloying and dry mixing of MnAlC and FeCo nanoparticles are accomplished followed by annealing in a furnace. Overall, the achieved results in this work enable synthesis of high moment FeCo and high coercivity CoxC with desired structure and magnetic properties obtained through polyol method. In particular, this Dissertation provides the technique to fabricate cobalt carbide nanoparticles without using rare earth elements as a catalyst or as heterogeneous seed nuclei at any stage of the processing.