ZnFe₂O₄/ZnO composites built from plenty of ZnFe₂O₄nanoparticles decorated on the surfaces of ZnO microflowers were successfully prepared by a simple mild solution method combined with a subsequent calcination process. The morphologies and microstructures of the as-prepared samples were characterized by various techniques. In addition, a comparative sensing performance investigation between the two kinds of sensing materials manifested that the sensing properties of ZnFe₂O₄/ZnO microflowers were obviously enhanced compared with those of single ZnO microflowers component. For instance, the response of ZnFe₂O₄/ZnO microflowers to 50 ppm acetone was similar to 8.3 at 250℃, which was nearly 5.4-fold higher than that of primary ZnO microflowers at the same conditions. The synergetic effect and the formation of the heterojunction between ZnO and ZnFe₂O₄along with the well-dispersed structures were believed to be the sources of the improvement of gas sensing properties.