We report magnetic properties of macroporous magnetic materials with highly ordered spherical voids prepared by an electrochemical technique. The interstitial sites in close‐packed arrays of colloidal silicas were filled by the electrodeposition of Fe, Co, and Fe3O4. The silica templates were removed by soaking the deposited templates into a 2% HF solution. SEM images of the template‐free macroporous magnetic materials clearly exhibit spherical voids arranged in a three dimensionally ordered structure. The magnetization curves of the Fe and Co films show a decreasing tendency with decreasing temperature, which might be associated with magnetic polarization and domain wall propagation. On the other hand, the Fe3O4 film exhibits a typical ferromagnetic behavior but has the reduced Curie temperature, which is due to the 2D Heisenberg type of the Fe spins. (© 2004 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)
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