This paper deals with characterization and synthesis of zinc fluoroborate from zinc fluoride and boron by mechanochemical reaction. Zinc fluoroborate is widely used in high technological areas such as textile, chemical reaction, plating solution, and glass. In this study, zinc fluoroborate has been synthesized via high-energy ball milling method. The effect of reactant mol ratio (B/ and ball milling period was investigated on the product yield. After completion of the reaction, the product in the reaction mixture (including excess reactant and side products) was purified by the extraction with water. The samples were characterized by FT-IR and ion-selective electrode. SEM and EDX analyses were took place. Decomposition of sample was characterized by TG-DTA. The sample was sintered at 300- to compare the data with TG-DTA. The results showed that decomposition of B-F bond started at . As a result of these experiments, maximum yield was obtained at 0.8 molar ratio and 3000 min. of mechanochemical reaction duration with the use of ball milling. Eighty-three percentage pure zinc fluoroborate was produced by adding the purification step.