This study focuses on how the partial substitution of copper by nickel nanoparticles affects the electrical and structural properties of the Bi2Ba2Ca2Cu2.9Ni0.1O10+δ, Bi2Ba2Ca2Cu2.8Ni0.2O10+δ and Bi2Ba2Ca2Cu2.6Ni0.4O10+δ compounds. Approximate values of crystallization size and crystallization percentage for the three compounds were calculated using the Scherer, modified Scherer, and Williamson-Hall methods. A great similarity was observed in the crystal size values from the Scherer method, 243.442 nm, and the Williamson-Hall method, 243.794 nm for the second sample. At the same time this sample exhibited the highest crystal size value for the three methods. In the examination of electrical properties, the sample with 0.1 partial substitution, Bi2Ba2Ca2Cu2.9Ni0.1O10+δ was determined to be the best with a critical temperature of 100 K and an energy gap of 6.57639 × 10-21 MeV. Using the SEM technique to analyze the structural morphology of the three phases, it was discovered that the size of the granular forms exceeds 25 nm. It was determined that the samples’ shapes alter when nickel concentration rises. The patterns that reveal the distribution of the crystal structure also exhibit clear homogeneity.