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The autocatalytic nickel bath uses sodium hypophosphite as a reducing agent, sodium citrate as a complexing agent and sodium acetate as an accelerator. The effect of calix[4]arene molecule type H4L named (dicarboxylic acid p-tert-butylcalix[4]arene) was studied and used at various concentrations of 10-3 to 10-6 M to improve the microstructure, the microhadness and properties of nickel deposit obtained. The effect of varying the concentration of H4L, on the deposition rate, the composition, the microstructure and morphology of chemical deposition was studied. The results showed that depending on the concentration of calix[4]arene, the deposition rate decreases from 11, to 7.75 μm/h. The microstructure and microhardness improves significantly at a concentration of 10-6 M of additive. It was also shown that the coating obtained is adherent and compact and the chemical bath has become more stable in the presence of calix[4]arenic additives. Indeed, in both cases, the nickel content decreased with the addition of concentration. This decrease of nickel content might be related to the increase of deposition rate depending on the concentration. The X-ray diffraction analysis revealed peak intensification in the {111} orientation of plane in the presence of a concentration of 10-6 M; this may be in agreement with the results of metallographic study which showed that the coatings are adherent and have a good resistance. Hence, the Vickers microhardness of deposited coatings has a better value (376 HV) at the concentration 10-6 M. The corrosion resistance in 3% NaCl solution has been proven at the same concentration as found. Finally, the cyclic voltammetry and electrochemical impedance spectroscopic studies revealed that the additive strongly influences the cathodic process and affects slightly oxidation of hypophosphite.