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The effect of ultrasonic treatment parameters, including ultrasonic treatment duration, frequency resonance, and treatment temperature, on the degassing of Mg-3.03Ca alloys was investigated. The results indicated that the optimum degassing efficiency could be obtained under the ultrasonic resonant condition. When applying ultrasonic treatment for 90 s with 150 W at 700 °C, the minimum hydrogen content and the highest degassing efficiency are obtained, respectively (42.8 cm³/100 g and 27.5%). The ultrasonic treatment can remove the gas from the melt and refine the microstructures. Finally, the mechanism of ultrasonic degassing and refinement was analyzed.