The effect of the preparation conditions on the physicochemical characteristics, operating life, and reactivity of Fe/Cu bimetallic particles was studied significantly by using a model pollutant (p-nitrophenol), scanning electron microscopy-energy dispersive spectrometry, and X-ray diffraction spectrometry. The results suggest that the higher reactivity and longer operating life of Fe/Cu bimetallic particles were obtained under the optimal preparation conditions. Furthermore, under the optimal preparation conditions, Cu was not easily dropped from the Fe particle, and the weight ratio of Cu on the surface of the Fe/Cu bimetallic particles increased significantly. Moreover, their optimal theoretical Cu mass loading could be decreased from 0.89 to 0.41 g Cu/g Fe, which favors the reduction of production costs. In addition, two batch experiments with Fe/Cu bimetallic particles prepared under optimal and nonoptimal conditions were set up to comparatively investigate the improvement of operating life and reactivity of Fe/Cu particles when optimized preparation conditions were carried out. As a result, it was proven that the reactivity and operating life of Fe/Cu bimetallic particles could be improved significantly through the optimization of preparation conditions.