The homogeneity and luminescence properties of undoped bulk GaSb have been studied by the cathodoluminescence ͑CL͒ technique in the scanning electron microscope. CL images have revealed a nonuniform distribution of native defects in GaSb wafers prepared from as-grown single crystals. Postgrowth annealing in vacuum, gallium, and antimony atmospheres has been performed to obtain more accurate information about the defect structure in this material. In general, on annealing, homogeneous distribution of impurities is observed throughout the wafers. CL spectra show that a luminescence band ͑centered at 756 meV͒ is enhanced by annealing in a gallium atmosphere, suggesting that Ga atoms play an important role in the formation of this acceptor center. The 756 meV peak has been attributed to a transition from conduction band to an acceptor center comprised of Ga Sb or a related complex. Interestingly, localized crystallization at the subgrain boundaries seems to occur by annealing in Ga atmosphere. © 1995 American Institute of Physics.Recently, ZrF 4 -based fluoride glass optical fibers have been predicted to have intrinsic minimum losses one or two orders of magnitude lower than those of conventional silica fibers.1 The loss minima for the next generation fibers are expected to occur in the 2-4 m wavelength regime. These estimations have stimulated considerable interest on materials for mid-IR sources and detectors. GaSb is the most suitable substrate material for various lattice-matched optoelectronic devices in the range of 0.3 eV ͑InGaAsSb͒-1.58 eV ͑AlGaAsSb͒.2-4 There are several reports on the growth of bulk GaSb single crystals employing various techniques.5-7 However, there are very few reports on the characterization of defects in the grown crystals. For defect characterization, the cathodoluminescence ͑CL͒ technique has been found to be highly sensitive and is extensively used for the spatial defect mapping. To the best of our knowledge, CL microscopy has not been applied to defects studied in GaSb. In this letter, we present the results of CL investigation of defects in bulk GaSb generated during growth and postgrowth annealing treatments.The GaSb samples used in our studies were vertical Bridgman grown single crystals.8 Undoped GaSb is always p type in nature with the acceptor concentration of approximately 10 17 cm Ϫ3 at room temperature. The acceptor is intrinsic and is due to a vacant gallium site (V Ga ) and gallium antisite (Ga Sb ). The acceptor concentration can be reduced either by nonstoichiometric melt growth or by employing low-temperature growth techniques. 9,10 In this work we have performed postgrowth annealing in vacuum, gallium, and antimony atmospheres to examine the evolution and nature of the native acceptors. The wafers were prepared by conventional chemomechanical polishing. Prior to annealing, the samples were etched in CH 3 COOH:HNO 3 :HF ͑20:9:1͒ to remove any damaged layer left behind after polishing, dipped in HCl, and rinsed in methanol. Thermal annealing of the samples was carried ...