Cu-Fe alloys (CFAs) are much anticipated for use in electrical contacts, magnetic recorders, and sensors. The low cost of Fe has inspired the investigation of these alloys as possible replacements for high-cost Cu-Nb and Cu-Ag alloys. Here, alloys of Cu and Fe having compositions of Cu100-xFex (x = 10, 30, and 50 wt.%) are prepared by gas atomization and characterized microstructurally and structurally based on composition and powder size with scanning electron microscopy (SEM) and X-ray diffraction (XRD). Grain sizes and Fe-rich particle sizes are measured and relationships among composition, powder size, and grain size are established. Same-sized powders of different compositions yield different microstructures, as do differently sized powders of equal composition. No atomic-level alloying is observed in the CFAs under the experimental conditions.