In the framework of XRD diffractometry we identified two-phases (2223 and 2212) in our Bi1.8Pb0.3Sr2Ca2(Cu1-xNix)3.3Oy superconductor samples. The percent of 2223-phase depend on Ni doping: 78.37 % for x=0.002; 70.29 % for x=0.005; 51.13 % for x=0.015; 47.75 % for 0.02; 26.11 % for x=0.03. The unit cell of 2223 phase was indexed as tetragonal structure having the following lattice constants: a=b=5.39 Å and c=37.05 Å [1]. On cooling to 77 K, the plots of resistance versus temperature (four points method) evidenced that the critical transition temperature to the superconductor phase, Tc, is decreasing from 106.21 to 93.47 K when the Ni content is varying from x=0.002 to x=0.03. From the log-log plots of the excess-conductivity we calculated the 3D-2D cross-over temperature, the coupling factor and the coherence length for all the samples. Thermal measurements were performed with a horizontal “Diamond” Differential/Thermogravimetric Analyzer from PerkinElmer Instruments in dynamic air atmosphere (150 cm3 min-1), choosing an increasing rate of 10 K/min, from room temperature to 940 °C. Thermal behaviors (TG, DTA, DSC, DTG diagrams) show a strong dependence on Ni content. The results of the specific heat capacities calculated from DSC plots [2], are presented in Fig. 1 for three samples (x=0.002, 0.005 and x=0.01). The contribution of crystal lattice to the estimated specific heat capacity was in conformity with the Einstein model [2]. The Einstein temperature values depend on Ni content.