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Pulsed Electrodeposition Of Nano… enhanced mechanical properties, and improved corrosion resistance when the Nanocrystalline films are dense and defect free. 1.1. PROBLEM STATEMENT REGARDING EXPERIMENT –Major obstacle regarding the experimental research was that we were unable to get a uniform co- deposition of the diamond particles on the annealed copper substrate (due to very early settling down of diamond particles owing to their higher density) during the pulsed electro deposition of nickel on the annealed Cu substrate using potentiostat and hence we cannot get effective simultaneous deposition of both Ni and diamond. 1.2. STRATEGY USED TO OVERCOME- We used a ultrasonicator during the pulsed deposition which sent ultrasonic waves into solution and woúld not allow the diamond particles to settle down and we can get an uniform coating with uniform deposition of diamond particles. II. EXPERIMENTAL DETAILS Nanocrystalline nickel was deposited on annealed copper substrate of unit surface area (1 cm 2 ) via pulsed electro deposition technique using potentiostat (model 263A, Princeton Applied Research, USA) from Watts bath containing nickel (NiSO4.7H2O), nickel chloride (NiCl2.6H2O), boric acid and citrate complexing agent sodium citrate( Na3C6H5O7.2H2O). Diamond particles of three different dimensions, viz., 1, 3, and 6 micron were added separately (5 g/L) to the watts bath and co-deposited along with Nanocrystalline nickel. The temperature was kept constant at 55 °C. The solution was sonicated for 45-60 minutes prior to deposition to disperse the diamond particles uniformly the bath. Electrolyte Bath Compositions Utilized for the Co-deposition of Ni-Diamond film Composition Concentration Parameters NiSO4.7H2O, g/L - 250 NiCl2.6H2O,g/L - 40 Temp. = at 55 °C H3BO3, g/L - 40 Sodium citrate, g/L - 25 Depositions were carried out at different current densities, viz., in 50, 100 and 200 mA/ cm 2 for different durations, i.e., 7, 14 and 21 minutes. One cycle of deposition corresponds to 1 minute. Scanning electron micrographs show uniform deposition of Microstructure of micron diamond on the surface of copper embedded in the nickel matrix. Elemental mapping confirmed uniform deposition of nickel and diamond with almost no cracks or pits. The analysis of the electrodeposited surfaces were done using SEM, and micromechanical properties, such as, Vicker’s hardness . Improved microstructural and mechanical properties were found in the case of electrodeposited surfaces containing 6 micron diamond followed by 3 and 1 micron diamond. The mechanical properties were also found better than those processed via stirring the solution during deposition. 2.1. POTENTIOSTAT USED FOR PULSED ELECTRODEPOSITION :- (MODEL 263A, PRINCETON APPLIED RESEARCH, USA) www.<strong>ijcer</strong>online.com ||May ||2013|| Page 90
Pulsed Electrodeposition Of Nano… OBSERVATIONS AND RESULTS – Experimental parameter I –3 micron diamond, (5 g/L), 60 ml solution , 30 min prior to sonication , 3 min deposition + 3 min sonication , Temperature 50-55 degree Celsius 21 cycles intermittent (electrodes kept dipped while sonication intervals) no deposition while sonication THE Images on the right hand side are the S.E.M images of the equiaxed NANOCRYSTALL- INE DEPOSITED NICKEL( with uniformly deposited 3 MICRON DIAMOND OVER IT) on the annealed Cu substrate ABOVE SHOWN IS THE ELEMENTAL MAPPING which shows two spectrums viz: SPECTRUM 1 and SPECTRUM 2 From elemental mapping we can clearly see that the CARBON WEIGHT % at SPECTRUM 2 is very high around 80 % and presence of very low Ni % which indicates and proves the presence of diamond particle over there www.<strong>ijcer</strong>online.com ||May ||2013|| Page 91
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