The present study is focused on the synthesis and investigation of anodic aluminum oxide (AAO) films and magnetic nanocomposites Ni/AAO obtained by Ni electrodeposition into porous matrix. AAO membranes and magnetic nanocomposites were investigated by HRSEM, EDX microanalysis, XRD, nitrogen capillary adsorption method, SQUID magnetometry, and polarized small-angle neutron scattering (SANS). The influence of synthesis conditions and form factor effect on the magnetic properties of nanowire arrays is reported.