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The synthesis of magnetic Cu1-xNix nanoparticles was carried out in cationic water-in-oil (w/o) microemulsions of water/cetyl-trimethyl-ammonium bromide (CTAB), n-butanol/isooctane by the reduction of nickel and copper chlorides with hydrazine and NaOH. The synthesized Cu1-xNix particles were heat treated to maintain their proper homogeneity and Curie temperature. Some alloy particles with the composition CU27.5M72.5 were coated with silica prior to the thermal homogenization in order to retain the pristine morphology. The magnetic particles were characterized using XRD, transmission electron microscopy (TEM) and magnetic measurements. The thermal demagnetization in the vicinity of the Curie temperature of the nanoparticles was studied using a modified TGA/SDTA method.