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A non-vacuum, two-step process has been used to prepare a series of nanocrystalline CuIn1−xGaxSe2 (x = 0, 0.25, 0.5, 0.75, 1) materials. An open-air solvothermal preparation in triethylenetetramine solvent was followed by annealing at 500 °C in a nitrogen atmosphere for 20 min. All materials have mixed clustered plate, spherical particle, and nanorod morphologies with the smallest particle diameters ranging between 20 and 40 nm. Raman spectroscopy and X-ray diffraction (XRD) confirm that indium/gallium ratio control is possible over a wide range. The solvothermal reaction step yields a mixture of chalcopyrite and Cu2−xSe. This is converted to pure chalcopyrite product by annealing at 500 °C.