2015 : Modulated synthesis and characterization of Ni-UiO-66

Dra. Ratna Ediati MS., Ph.D

Abstract

Modulated synthesis of Ni-UiO66 is reported via direct conventional solvothermal method. Zirconium tetrachloride (ZrCl4), 1,4-benzen dicarbocarboxylic acid (H2BDC), and nickel (II) nitrate (Ni(NO3)2.6H2O) were dissolved in mixture of N-N’-dimethyl formamide (DMF) and variant concentrations of acetic acid (CH 3COOH). Acetic acid was used as modulator in which variants concentrations were 5eq, 10eq, and 20eq. All mixtures were heated at 140 °C for 6h. The structures of Ni-UiO66 obtained from modulated synthesis were confirmed to be isostructural to UiO-66 by powder X-Ray diffraction (PXRD). The data present a unique crystalline phase, which is in good agreement with the UiO-66 pattern by Cavka. The characterization PXRD pattern of Ni-UiO66 has main peak with a high intensity at 2θ of 7.3°, as well as other characteristic peaks with lower intensity at 2θ of 8.6, 10.3, 20.6 and 30.5°. The crystallinity of Ni-UiO66 can be enhanced by adding modulator to the reaction mixture. Ni-UiO66 with variant modulator is 20eq has the highest crystalline. The IR spectra of UiO-66 and Ni-UiO66 are almost the same, further confirming the isostructural to UiO-66. SEM images of UiO-66 and Ni-UiO66 show the modulator leads to the morphology of intergrown particles decreasing