Tribomechanics is a part of physics that is concerned with the study of phenomena that appear during milling under dynamic conditions. Tribomechanical micronization and activation (TMA) of whey protein concentrates (WPC) and zeolites (type clinoptilolite) were carried out. Samples of powdered WPC and zeolite were treated with the laboratory TMA equipment. The treatment was carried out at two various rotor speeds: 16,000 and 22,000 r.p.m. at ambient temperature. Analyses of the particle size and distribution as well as the specific area and scanning electron microscopy were carried out on the powdered WPC and zeolite, before and after the TMA treatment. Suspensions of the WPC and zeolite were treated with ultrasound, just before determining the particle size distribution, at 50 kHz. The results showed that tribomechanical treatment causes significant decrease in particle size, change in particle size distribution and increase in specific area of WPC and zeolite. These changes of the treated materials depend on the type of the material, the level of inserting particles, the planned angle of the impact, internal rubbing and the planned number of impacts. The effects found became stronger as the rotor speed of the TMA equipment increased (16,000 to 22,000 rpm). Ultrasonic treatment of suspension of tribomechanically treated WPC resulted infurther breakdown of partly damaged protein globules as proved with the statistic analyses. No further changes in their granulometric composition were caused by ultrasonic treatment of a suspension of tribomechanically treated zeolite.