This study assesses the wear performance of HVOF-sprayed nanostructured TiB2 composite coatings and the use of mechanical alloying for powder preparation. In order to prevent the formation of undesired secondary borides, TiB2 particles are processed with a nickel-base self-fluxing matrix alloy. XRD analysis shows that the minimum average TiB2 crystal size is 22 nm after high-energy milling and only slightly larger and uniformly distributed after HVOF spraying. The resulting TiB2 layers are characterized based on morphology and wear behavior and are shown to hold promise for abrasive wear applications. Paper includes a German-language abstract.