Abstract: The structural transitions of the NiAs-type Mn0.52Sb0.48 magneto-ordered compound, ball milled to different periods, have been characterized by X-ray diffraction and DSC analysis. On the basis of lattice parameter results a structural evolution mode with three stages is proposed. In the first stage lattice parameters keep nearly unchanged with the refinement of grains and increase of lattice strain. In the second stage, microstrain shows a lowering tendency accompanying the successive decreases of grain size. The X-ray revealed internal strain is found to be strains inside the lattice, which can be relaxed with new grain formation. The change of Tc is shown to be affected by the dimension of c axis, however the overall magnetization is continuously decreased with milling, due to the disordering process occurred in milling. Correspondent disordering mechanisms have been tentatively postulated and discussed according to the changes of lattice para meters.