A porous coordination polymer, Zn3(BTC)2·12H2O (Zn-BTC) upon silk yarn, has been synthesized under ultrasound irradiation of identical reaction mixtures of Zn(II) and H3BTC (BTC = 1,3,5-benzenetricarboxylate). Effects of temperature, sequential dipping steps and sonication on the growth of Zn-BTC upon silk yarn were investigated. These systems depicted a decrease in the particles size accompanying a decrease in the sequential dipping steps. Results showed a decrease in the particles size as decreasing frequency of ultrasound irradiation. The antimicrobial activity of Zn-BTC upon fiber was tested against the Gram positive strain Micrococcus sp. and Gram negative bacterial strain Escherichia coli. The samples were characterized with X-ray powder diffraction (XRPD), Fourier transform infrared spectroscopy spectra and scanning electron microscopy. XRPD analyses indicated that the prepared Zn-BTC nanostructures on silk fibers were crystalline.