研究采用简捷化学浴和超声波辅助液相化学合成技术，制备出了2种非化学计量比的三元高阶Bi_3.64Mo_0.36O_6.55纳米光催化剂通过X-射线衍射分析（XRD）、场发射扫描电子显微镜（FESEM）和固体紫外-可见光学吸收光谱（Uv-Vis DRS）对所制得的样品进行了物相、形貌和光学性质的测试与表征。结果表明，经超声波辅助反应得到的Bi_3.64Mo_0.36O_6.55纳米晶（BMO-1）为纯立方相准立方体形的纳米颗粒，粒径约为30~50 nm。以有机染料亚甲基蓝（MB）为分子探针，以氙灯为可见光光源，光催化降解实验表明BMO-1的表观速率常数分别是化学浴法制得的纳米晶（BMO-2）和商业化纳米TiO₂（P25）的1.8倍和15.5倍，体现了更优的可见光催化降解有机污染物性能。

The nonstoichiometric Bi_3.64Mo_0.36O_6.55 photocatalysts were synthesized by a chemical bathing method and a wet ultrasonic-assisted chemical synthesis method respectively. The phase, morphology and optical property of asprepared products were investigated by X-ray diffraction(XRD), field emission scanning microscopy(FESEM) and optical absorption spectrum. The results showed that BMO-1 products obtained by sonochemistry reaction are single cubic crystal quasi-cubric nanoparticles with about 30~50 nm in diameter. The photocatalytic performance was evaluated by the degradation organic dye MB under the xenon lamp irradiation. Findings suggested that BMO-1 samples display the superior photocatalytic activity, of which the apparent reaction rate constant is 1.8 and 15.5 times that of BMO-2 and commercial nano TiO₂ (P25) respectively.