The 3D microstructure of Ni4Ti3 precipitates growing in different Ni-Ti alloys have been investigated in a Dual-Beam FIB/SEM system via the Slice-and-View procedure. From the optimized cross-section image sequence, the mean volume, specific surface area, sphericity and aspect ratio of the Ni4Ti3 precipitates are calculated based on pixel counting, while the morphology is quantitatively determined by the equivalent ellipsoids and classified according to the Zingg scheme. Also, the Pair Distribution Functions of the precipitates are obtained from the coordinates of the mass center of the precipitates. The present work indicates that slice-and-view is a valuable tool for the investigation of the 3D distribution and related parameters of technologically important precipitates in alloys such as Ni-Ti.