Electrodeposition provides a cost-effective means of producing fully dense nanocrystalline metals, alloys, and metal-matrix composites as coatings or freestanding forms (foil, sheet, wire, complex shapes). Fabrication of nanocomposite coating can be achieved by codeposition of nanometer-sized particles during electrodeposition of the matrix material. Since materials that can be electrodeposited include metals, alloys, oxides, semiconductors and electrically conducting polymers, this approach can be used to synthesize a wide range of nanocomposite materials. Electrodeposition of composite coatings, based on second phase hard particles dispersed in a metallic matrix, is gaining importance for potential engineering applications 1 such as wear-resistant coatings, 2‐4 corrosion-resistant coatings, 5 selflubricating films 6 and thermally graded structures. 7 TiC reinforced Cu and Fe based composites have been extensively used in electrical contacts, resistance welding electrodes and electrode for automatic welding. 8 Ni-TiC, finds their main use as cutting tools and in wear resistant applications because of their superior hardness and reasonable fracture toughness. Generally, hard metals are produced by conventionalsinteringmethodswhichareproductiveandproducefullydense parts. However, conventional techniques limit complexity in geometry. Therefore, a very economical and conventional technique is used here for the production of composites of scientific interest in the present investigation. Although TiC reinforced Ni metal matrix composites possess potential applications in cutting tools and as hard materials nevertheless less attention has been paid as very limited work has been reported 9‐12 on the electrodeposition of Ni-TiC. Moreover the nanocomposite of Ni-TiC has scarcely been reported. It is known that the properties of materials significantly change once the materials are transformed into nanomaterials. Therefore the present work focuses on this aspect in view of the interesting results obtained on metal matrix composites using micron sized particles. 13 It has been noticed that the electrodeposition of nano sized particles from aqueous medium has limitation of agglomeration and low degree of incorporation due to surface hydrophobicity. 10 In an attempt to overcome these problems, in the present investigation an unconventional bath (organic solvent) has been used. In view of the potential advantages offered by N-methylformamide i.e. very high dielectric constant which permits the highest probability of dissociation of electrolytes and its solubility, allowing high tolerance of electrolyte in the bath, high boiling point with good chemical stability permitting wide temperature range for bath operation and comparable viscosity and density to water; electrodeposition of metal matrix composites using N-methylformamide in conjunction with a common and cheap metal salt (nickel acetate) was undertaken for the first time in our laboratory