In this research barium carbonate nanoparticle with composition BaCO3 (Witherite) was prepared by using the gel-combustion (sol - gel) method. A precursor sol was obtained from barium nitrate. The molar ratio of citrate/nitrate=1.3 (CA/NO-3 =1.3) was used to prepare very fine powders of barium carbonate. The gels resulting from these sols were transformed into powders by an auto-combustion process at ≤400oC. The powders consisted of orthorhombic BaCO3 and one another additional phase. The barium carbonate nano-particles produced by the gel-combustion method were calcined in three different calcination temperatures T = 450 °C, T = 600 °C and T =750 °C. The pure orthorhombic phase was found at 450oC X–Ray diffraction. The effect of calcination temperature was studied in three various temperatures. The crystallite size XRD was estimated from the broadening of XRD peaks, using Scherrer\\\'s formula. Transmission electron microscope (TEM) and X–Ray diffraction (XRD) of the samples were used for characterization of the obtain products. The size of particles were produced by this method are between 1nm to 10nm.

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