In this work, we investigated the size and elemental composition of a binary of aluminum/zinc nanoparticles synthesized in a gas discharge generator. AlxZn1–x nanoparticles were produced in inert atmosphere by simultaneous  erosion of aluminum hole cathode and a zinc anode. Mass fractions of aluminum x were varied from 0.05 to 0.29 by changing the surface area of the aluminum electrode. It was found that the mass fraction of aluminum in binary composition increased 2.6 times when erosion surface of the Al cathode dropped from 188.5 to 37.7 mm2. The average sizes of primary nanoparticles were in the range from 12.8 to 18.6 nm, which formed submicron agglomerates.  Also, when the erosion process occurred in an air atmosphere, we produced zinc aluminate AlZn2O4 with luminescence in ultraviolet (UV) range.