用Ｈ２ＷＯ４和ＮｉＣｌ２碱性水溶液与ＦｅＣｌ２和Ｙ２Ｏ３的酸性水溶液快速混合方法，在超声喷雾热转换装置中制备ＷＮｉＦｅＹ系纳米级复合氧化物粉末。通过Ｘ射线衍射及透射电镜分析，研究了复合粉末的物相组成、颗粒形貌及粒径范围．结果表明，采用上述两种溶液快速混合及超声喷雾热转换的方法，可以制备成分均匀的复合氧化物粉末。其物相组成为ＷＯ３，ＮｉＯ，Ｙ２Ｏ３，粉末的千粒平均粒径为３２ｎｍ，颗粒形貌近似球形，用ＢＥＴ法测定的粒径为３０ｎｍ。 WNiFeY nanowire composite oxide powders were prepared by ultrasonic mixing with H2WO4 and aqueous solution of NiCl2 and acidic aqueous solution of FeCl2 and Y2O3. By X-ray diffraction and transmission electron microscopy analysis of the phase composition, particle morphology and particle size range of the composite powder. The results show that composite powder with uniform composition can be prepared by the rapid mixing of the two solutions and the ultrasonic spray thermal conversion. The phase composition of WO3, NiO, Y2O3, the average particle size of one thousand particles of the powder is 32nm, the particle morphology is approximately spherical, the particle size determined by the BET method is 30nm.