The cubic zinc blende GaSb phase was produced by a mechanical alloying technique, which is a solid state route based on the action of non-hydrostatic pressures. The thermal stability of this phase was tested using the differential scanning calorimetry technique and, in order to clarify the results, an annealing process was performed. Comparing x-ray diffraction patterns for as-prepared and annealed samples, the improvement in crystallinity of the cubic phase and Sb segregation and/or crystallization can be easily seen. Optical phonons frequencies were measured for both as-milled and annealed samples by means of the Raman spectroscopy technique. Raman profiles of as-milled samples showed typical zinc blende GaSb optical modes and revealed new features that can be associated with multiphase states.