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This new type nanocomposite powder was prepared with electroless plating enhanced by ultrasonic wave. High-resolution transmission electron microscopy (HRTEM) showed that As-plated particles have nanometer scale average size. X-my diffraction (XRD) analysis showed the presence of a noncrystalline structurein the plating layer on the nano-Al2 Os matrix. The content of the plating layer was analyzed by energy dispersive X-ray spectroscopy (EDX) technology. The plating layer content was adjustable by changing the solutionconcentration.