Zeolites mordenite (MOR) and β decorated with high dispersion degree and loading content of CuO composite (symbolized as CuO/zeolite) were prepared via a novel method-the stepped hydrothermal synthesis. The resultant composite were characterized with details by powder XRD, ICP-AES, H2-TPR and TEM techniques. Shown by experiment, the stepped hydrothermal synthetic method adopted in the present research using urea as alkali source as well as benefiting from the ultrasonic wash treatment hardly damages the zeolitic framework structure. Compared with ammonia, high dispersion degree and loading level of CuO are yielded as a consequence of the employment of urea as alkali source. Besides, the ultrasonic wash treatment not only removes some CuO precursors that deposit on the external surface of the porous support but also produces a uniform distribution of CuO particles with smaller dimension on the surface of zeolites: CuO are dispersed in nanoscale of about 4-8 nm on mordenite and 2-5 nm on zeolite β. The present synthetic strategy could be therefore applied as a novel general method for the manufacture of functional materials in a wide spectrum.