The partial transformation of crystal phase of micron-sized TiO2 powder from rutile to anatase was realized utilizing microwave irradiation in hydrogen peroxide solution. Afterwards, the ultrasound of low power was used as an irradiation source to induce the transition crystal TiO2 powder to perform the sonocatalytic activity through the degradation of azo fuchsine in aqueous solution. The results show that the sonocatalytic activity of the transition crystal TiO2 powder is obviously higher than that of pure micron-sized rutile and anatase TiO2 powders. The degradation ratio of azo fuchsine in the presence of the transition crystal TiO2 powder attains nearly 80% within 80 min ultrasonic irradiation.