α-FeO samples were manufactured by means of the polymeric precursor method. The powders were sintered and calcined at temperatures of 300-700 °C for 2 h, respectively. In the X-ray diffraction results, the formation of the rhombohedral phase without secondary phases was exhibited. The size of the particle increased after calcination at 700 °C, exhibiting a slightly more irregular morphology for the samples calcined with the addition of NHOH in the synthesis process. From the field-emission scanning electron microscopy measurements, the particle size was determined, showing a smaller size for the samples without NHOH in the synthesis process. The samples calcined at 600 °C had a size of 100 nm, with the sizes for lower temperatures being smaller. The size of the nanoparticle agglomerates was largest for the samples with NHOH; however, the zeta potential was slightly lower over time for these samples. The phase study of the α-FeO nanoparticles was confirmed by means of Raman spectroscopy, without additional bands of another crystal structure. In addition, the synthesized nanoparticles exhibited good photocatalytic activity in the degradation of rhodamine B (RhB) and atrazine (ATZ) within 40 min, with a maximum degradation of 59% for ATZ and 40% for rhodamine. The best responses in the degradation were for the samples without the addition of NHOH in the synthesis process and in proportions lower than 0.1 g. The cytotoxic effects of the nanoparticles obtained at 600 °C were evaluated in apical cells of onion roots. The results are promising for future applications because no changes were observed in the mitosis of the cells.