This paper presents a novel strategy to prepare Cu3(BTC)2@SiO2 core-shell nanoparticles in the size range of 200-400 nm using a new one-pot strategy under ultrasonic irradiation at room temperature. In this approach, the silica shell thickness could be finely tuned in the size range of 12-60 nm for various reaction times. Nanocomposite thin films were fabricated on the glass substrates by Sol-Gel spin coating using the products for 1.5 h, 2 h and 2.5 h, respectively, and heat treated using an infrared lamp heating system in air. The photocatalytic degradation of phenol in aqueous solution using Cu2(BTC)3@SiO2 thin films was investigated under visible light irradiation at pH 4. After a 45 min reaction with phenol, the degradation rate was up to 93.1%. Moreover, the thin film photocatalysts could be reused 5 times without appreciable loss of photocatalytic activity for degradation of phenol. The present work clearly shows that the films as photocatalysts showed higher photocatalytic performance.