Thermal reduction has been applied to the preparation of copper nanoparticles (Cu-NPs) using three kinds of nonionic surfactants (Triton X-100, Tween-80, and dodecylamine). The Cu-NPs were formed by decomposition of copper(II) oxalate in presence of triphenylphosphine. The effect of the surfactants on the formation of the Cu-NPs was studied via X-ray diffraction, scanning electron microscopy, energy dispersive analysis of X-rays, transmission electron microscopy, thermogravimetric differential thermal analyses, and Fourier transform infra-red spectroscopy. It is shown that the Cu-NPs have an fcc crystal structure. Depending on the surfactant used, Cu-NPs with diameters between 8 and 20 nm can be prepared. The smallest Cu-NPs (8 nm) were formed in the presence of micelles of dodecylamine (yield 49%), while the largest particles (20 nm) were obtained with Triton X-100 (yield 99%). The use of Triton X-100 results in the highest yield and most uniform Cu-NPs.