ABSTRACTFe3O4/CNT hybrids have been successfully synthesized through simple one-step methods. The resulting composites were characterized via transmission electron microscopy (TEM), X-ray diffractometry (XRD), Fourier transform infrared (FTIR) and vibration and sample magnetometry (VSM) approaches. It was found that those Fe3O4/CNT nanocomposites were superparamagnetic. TEM observation indicated that the produced Fe3O4 particles were decorated the external walls of CNTs. The increasing of the ultrasonic times result in the changes in the average particle sizes of the Fe3O4 particles. For the Fe3O4/CNT composites, larger particle sizes lead to the greater magnetic responses.