Ingots of the quasi-binary GaSb-A1Sb alloy were prepared by progressive casting and zone casting at various rates of crystallization. Results of x-ray diffraction studies, metallographic studies, hardness determinations, and chemical analyses indicate that, with the possible exception of a narrow composition range between 10 and 30 mole % A1Sb which was not investigated, solid solution prevails in the system. Bulk specimens of single phase, solid solution alloy were obtained by use of low linear rates of crystallization (0.05 in./hr), while at higher rates of crystallization (1/a to 1z/4 in./hr) two intermingled solid phases were characteristically obtained.Vegard's law was found to be at least roughly applicable; with lattice constants for the alloys ranging between values of 6.0963A for pure GaSb and 6.1361A for pure A1Sb. Optical energy gaps determined for alloy specimens increased regularly with cell size from a value of 0.68 ev for GaSb to a value of 1.74 ev for A1Sb. Values of electrical resistivity and hole mobility for the relatively impure alloy specimens were also intermediate between those for the compounds in a like state of purity.Liquidus data are also presented for the system.