This work describes the preparation of alloy films by multitarget, triode sputtering. An apparatus designed to sputter two or three targets simultaneously onto a rotating substrate holder is described. The sputtering parameters necessary to vary and reproduce alloy composition are discussed. Changes in alloy composition are obtained by voltage variation of the several targets. Reproducible film compositions are assured by maintaining target voltage, geometry, and sputtering atmosphere constant. Zero or a constant partial pressure of hydrogen is required to obtain reproducible alloy properties. Composition, resistance, and thickness data are presented for the alloy systems Nb–Zr and Nb–Zr–Mo. Sheet resistance values for these films are reproducible to ±2%.