We report here the formation of nanocomposite of Bromargyrite doped in Prussian blue composite in the matrix of silica i.e. AgBr@KNi [FeC₆N₆]_0.7[CoC₆N₆]_0.3/SiO₂. This was successfully synthesized by the wet chemical precipitation procedure. The as-prepared sample and sample sintered at 500, 700, 900, and 1100 °C were structurally analysed by XRD. The result of XRD and Rietveld Refinement showed that the as-prepared sample was converted into the AgBr@Fe₂O₃/SiO_2. The refinements of the prepared samples were done by Fullprof Suite Software. With the Rietveld Refinement and XRD analysis, we achieved some microstructural and structural parameters like intensity, hkl planes, Wyckoff positions of atoms (x/a, y/b, z/c), size of the crystal, and R-factors (χ², R_p, R_wp, R_exp). The size of crystal of as-prepared sample and AgBr@Fe₂O₃/SiO₂ nanocomposite (1100 °C) was obtained as 3.89 nm and 34.64 nm respectively. The value of goodness fit factor was also achieved from the Rietveld Refinement.