Recently, barium carbonate nanomaterial has been shown to be a proven versatile candidate for the catalysis and sensor applications. The catalytic and sensing efficiency can be improved by making barium carbonate composite with a suitable transition element. In this regard, the preparation of barium carbonate and its composite with nickel during the synthesis process is presented with the composite-hydroxide-mediated method, an effective, feasible, and low-temperature synthesis route. The nanomaterial produced is monitored for the structural and optical properties with various diagnostic methods. The X-ray diffraction results show the presence of orthorhombic structure of barium carbonate in both pure and 5% nickel samples. A mixed structure is formed with the phases of barium carbonate, Ba(NO 3 ) 2 , and Ni(NO 3 ) 2 for the sample with 15% nickel. The average crystallite size estimated is in the range of 14-22 nm. The scanning electron microscope pictures captured on silicon (Si) covered with the product material reveal interesting rods, needle, and flower-type morphological features. The bandgap energy obtained by diffused reflectance spectroscopy is in the expected range of 5.48-5.71 eV. The proposed method seems effective to provide a feasible route for the synthesis of a broad range of nanomaterials for research purposes.