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A MgCl2-based Ziegler–Natta catalyst was characterized using X-ray diffraction (XRD) patterns, scanning electron microscopy (SEM) and transmission electron microscopy (TEM) and IR spectra. We focused on the XRD reflection at 2θ = 50° to determine the thickness of MgCl2crystals, and validated these results with TEM pictures. SEM pictures were taken in order to measure the size of the nanoparticles formed by the MgCl2crystals. Several compounds were synthesized for comparison and to aid interpretation of the infrared (IR) spectra. The catalysts were prepared by precipitating MgCl2, which was used as support material and subsequently treated with TiCl4. The thickness of the catalyst crystals was calculated from the XRD reflection at 2θ = 50°. Changing the precipitation temperature within a range from 40 to 90 °C altered the thickness of the MgCl2crystal plates. The maximum thickness of 7 nm was achieved at a precipitation temperature of 60 °C. The SEM pictures showed that the nanoparticles had a diameter of ~200 nm. A crystal base unit had a volume that corresponded to that of a sphere of 3.5 nm radius. Thus, we estimated that a typical catalyst particle with a diameter of 20 μm contained about one million nanoparticles, each of which consisted of about 25,000 MgCl2crystal units.