The work of this dissertation is centered on two non-conventional synthetic approaches to ferromagnetic nanomaterials: high-throughput experimentation (HTE) (polyol process) and continuous flow (CF) synthesis (aqueous reduction and the polyol process). HTE was performed to investigate phase control between FexCo1-x and Co3-xFexOy. Exploration of synthesis limitations based on magnetic properties was achieved by reproducing Ms=210 emu/g. Morphological control of FexCo1-x alloy was achieved by formation of linear chains using an Hext. The final study of the FexCo1-x chains used DoE to determine factors to control FexCo1-x, diameter, crystallite size and morphology. [Ag] with [Metal] provide statistically significant control of crystallite size. [OH]/[Metal] predict 100 % FexCo1-x at > 30. To conclude section 1, a morphological study was performed on synthesis of Co3-xFexOy using the polyol process. Co3-xFexOy micropillars were synthesized at various sizes. The close proximity of the particles in the nanostructure produced an optical anisotropy and was magnetically induced which is evidence for the magneto-birefringence effect. The second non-conventional synthetic approach involves continuous flow (CF) chemistry. Co nanoparticles (Ms=125 emu/g) were newly synthesized by aqueous reduction in a microreactor and had 30 ±10 nm diameter and were produced at >1g/hr, a marker of industrial-scale up viability. The final work was the CF synthesis of FexCo1-x. The FexCo1-x was synthesized with limitation to the composition. The maximum FexCo1-x phase composition at 20 % resulted from the aqueous carrier solvent triggering oxide formation over FexCo1-x.