Nickel-phosphorus (EN) deposited multi-walled carbon nanotubes (MWCNTs) were prepared using an electroless platingtechnique. The D.C and A.C magnetic behavior of the composites showed that pre-acid treatment of the MWCNTs prior toelectroless deposition greatly enhanced the magnetic susceptibility at 5 K producing a composite with antiferromagneticcorrelations and a superparamagnetic transition at 65.5 K. Raman scattering analysis suggests that there is no directinteraction of the nickel-phosphorus deposit and the MWCNTs.