Abstract: Standard samples for spectral analysis have gradually dominated the development of standard samples, and the standard samples of precious metals are difficult to be prepared due to compositional segregation and other factors. Powder metallurgy technology can prepare alloys with uniform composition, fine grain size, and the preparation of high-quality powder can provide raw material basis for the preparation of standard samples. With the help of ultrasonic cleaning machine on the silver alloy vibration, this study investigates whether the silver alloy powder can be produced, and explores whether the method can achieve the effect of grain refinement through the test analysis results. Experiments were carried out to compare and illustrate the three aspects of morphology, particle size and grain, and chemical composition. Polarizing microscope, scanning electron microscope and energy spectrometer were used to observe and test the silver alloy and silver alloy powder, X-ray fluorescence spectrometer was used for the verification of the chemical composition of the results. The use of ultrasonic vibration of silver alloys to prepare silver alloy powders is a new method of preparing silver alloy powders, which can produce powders with an average grain size of 9.54 μm when the ultrasonic power reaches 600 W, of which more than 70% are less than 10 μm. The average grain size of silver alloys is 22.5 μm, which indicates that ultrasonic vibration of silver alloys has the conditions for grain refinement, and the combination of the morphology and composition of the test results show that it is possible to both refine the grains and improve the tissue homogeneity by preparing the powder.