Abstract: Since the current synthesis of UiO-66 requires harsh conditions of high temperature and long term, the electrochemical method was applied to quickly synthesize UiO-66 under the conditions of no zirconium salt, normal temperature and 2 h in this paper. UiO-66/glassy carbon electrode（GCE） was prepared to construct an electrochemical sensor for detecting Cd²⁺. Through the characterization and analysis of scanning electron microscopy（SEM）, X-ray diffraction（XRD）, Fourier infrared spectroscopy（FTIR） and specific surface area（BET）, it could be seen that the synthesized UiO-66 had a rhombohedral dodecahedron structure with good crystallization and large specific surface area of 1 054. 455 m~2/g, and the total pore volume was 0. 709 cm~3/g. The optimal detection conditions were determined. pH value of NaAc-HAc buffer solution was 5, enrichment voltage was-1. 0 V, and enrichment time was 120 s.Under the optimal conditions for Cd²⁺ detection, the detection sensitivity of the electrochemical sensor was 4. 10 AM^-1 and the lowest detection limit was 0. 037 μM, showing good Cd²⁺ detection performance. It also had good reproducibility, stability and anti-interference. The recovery experiment showed that the effect of testing the actual Fen River water sample is good.