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A composite of powders of semi-Heusler ferromagnetic shape memory and pure titanium was successfully prepared by spark plasma sintering at the temperature of 950 °C. Sintering resulted in the formation of small precipitates and intermetallic phases at the heterogeneous interfaces. Various complementary experimental methods were used to fully characterize the microstructure. Imaging methods including transmission and scanning electron microscopy with energy dispersive X-ray spectroscopy revealed a position and chemical composition of individual intermetallic phases and precipitates. The crystalline structure of the phases was examined by a joint refinement of X-ray and neutron diffraction patterns. It was found that Co38Ni33Al29 decomposes into the B2-(Co,Ni)Al matrix and A1-(Co,Ni,Al) particles during sintering, while Al, Co and Ni diffuse into Ti forming an eutectic two phase structure with C9-Ti2(Co,Ni) precipitates. Complicated interface intermetallic structure containing C9-Ti2(Co,Ni), B2-(Co,Ni)Ti and L21-(Co,Ni)(Al,Ti) was completely revealed. In addition, C9-Ti2(Co,Ni) and A1-(Co,Ni,Al) precipitates were investigated by an advanced method of small angle neutron scattering. This study proves that powder metallurgy followed by spark plasma sintering is an appropriate technique to prepare bulk composites from very dissimilar materials. [ABSTRACT FROM AUTHOR]