Metallic material become interesting field for interconnect application that have high thermal stability and oxidation resistant at high temperature. The main problem is the agglomerates powder and grain growth of metallic material that lead to decrement of properties of interconnect material. Therefore, the main objectives of this research is to develop small size particle up to nano range size and even particle size. The methods of this research was performed though high energy ball milling for 60 h and ultrasonic bath for various holding time of 3 h, 3.5 h, 4 h, 4.5 h and 5 h. The analysis and characterization process will be conducted by Powder size analysis by particle size analyzer (PSA) and Scanning Electron Microscopy (SEM) with magnification of 1000 and 2000 times. The result shows that the particle size decreased gradually from UT samples, Milled 60 h samples and to milled 60 h and UT samples. Its shows that particle size of 38.67µm for raw material, 11.45µm for UT 4.5 samples, 6.27 µm for milled 60 h sample and 5.23 µm for milled 60 h and UT 4.5 h. Fine surface structed and even particle size was shown by UT samples and combination samples due to high energy bubbles through liquid media that collide the material.