Hollow carbon spheres containing Fe3N nanocrystals (Fe3N/HCSs) are synthesized by ferrocene and ammonium chloride in high pressure argon at 500 °C. The structure, morphology and properties of the products are characterized by X-ray diffraction (XRD), field-emission scanning electron microscopy (SEM), transmission electron microscopy (TEM), thermogravimetric analysis (TG) and vibrating sample magnetometry (VSM). The hollow carbon spheres have diameters of 1-10 µm and shell thickness of hundreds of nanometers. The dimensions of the acicular Fe3N nanocrystals have diameters of ca. 100 nm and lengths of 600-800 nm. The weight percent of Fe3N nanocrystals in Fe3N/HCSs is about 37.8%. The saturation magnetization value of the hollow carbon spheres containing Fe3N nanocrystals is 10.61 emu/g.