Magnetic sub-micron sized particles (with diameters in the range 100–600 nm) of Co, Ni and Co-Ni alloys, protected with polyvinylpyrrolidone have been prepared in gram quantities using the polyol process. Experiments carried out with different metal precursors and starting compositions have yielded reliable routes to produce particles of the desired diameters in the 100–600 nm range. The particles were characterized with X-ray diffraction, scanning electron microscopy, energy dispersive X-ray analysis, thermogravimetric analysis and magnetic measurements. The particles are found to be stable under ambient conditions indefinitely. The coercivity values of the Co and Ni particles are ∼50% higher compared to the corresponding bulk values. The alloy particles follow a trend similar to the bulk alloys.