Nano-sized sodium bicarbonate (NaHCO3) will be prepared by utilizing the method of bubble liquid membrane interfaces. Nano-sized sodium bicarbonate (NaHCO3) of high quality will be successfully produced with 100 mL distilled water, 10 g NaHCO3, 12 g nano-SiO2, 6 mL thickener and 8 mL foaming agent blended evenly and mixed together. NaHCO3 is soluble in the high-quality prepared bubble liquid membranes, where more smaller bubbles are formed in large quantity. The separation by crystallization of NaHCO3 is achieved at the interface of drying thin liquid membranes. The smaller bubbles between the liquid membranes hinder the growth of NaHCO3, thus making it easy to obtain particles of even smaller sizes. The microscopic analysis results show that the prepared NaHCO3 particles, 80 nm in width and 280 nm in length, are much smaller than those commercial NaHCO3 particles of 5 to 100 m in size.