Abstract. Different sizes and shapes of BaSiF 6 were synthesized by a low temperature hydrothermal method using citric acid (CA) as a chelating agent and cetyltrimethylammonium bromide (CTAB) as a surfactant. The sizes and morphologies of the BaSiF 6 could be altered by controlled the molar radio of CA to Ba
2+. And the CTAB could help to fabricate nanoscale crystals. The as-synthesized BaSiF 6 's properties were studied using XRD, SEM, TEM and Raman. Finally, the mechanism for CA and CTAB coactive hydrothermal synthesis of the BaSiF 6 is discussed.