Annexure - II

Electrochemical Study of Mg-Ti-V-X (Nb/Zr/Fe/Ni/W) alloy synthesized by mechanical

alloying
The aim of this project is to store the hydrogen reversibly in solid state form by forming the metal
hydrides. Magnesium is chosen as major element because of its high storing capacity of 7.6 wt% of
hydrogen. In order to improve the hydrogen absorption kinetics, it was planned to synthesis magnesium
based alloy by adding transition elements such as Nb, Zr, Fe, Ni, and W by high energy ball milling under
optimized parameters
Since hydrogen have low volumetric density, it requires large volume to store it in gaseous form.
Similarly there are series of problems in storing it in liquid form. So storing it in solid state by forming
the
hydrides is the cheapest way.
Initially, mechanical alloying of powder particles for 10 hours have been carried out. The essence
of the process is the solid state alloying by repetitive cold welding and fracture of constitutive powder
particles. With prolonged milling, various reactions take place, which lead to the formation of
intermetallic
compounds like Ti0.89V0.11 typically, with nanocrystalline structure. Then the formed nanocrystals were
compacted. In order to improve the conductivity of the sample, Ni is added in the ratio of 7:3
X-ray diffraction (X-RD) pattern of alloys before and after 10 hours of milling has obtained. By
comparing these two peaks, there is a shift in the peak. Using Xpert software, the peaks were analyzed
and found that V0.89Ti0.11 compound formed near the 2 value of 62 degrees. The formed compound will
enhance the absorption and desorption rates.
Scanning Electron Microscope (SEM) images helped to understand the mechanical alloying
mechanism, particle morphology. During milling, powder particles experience several forces like shear,
impact, attrition, compression. Due to these forces, deformation, cold welding fracturing occurs. In the
alloys Mg0.8Ti0.1V0.1, Mg0.8Ti0.05V0.05Ni0.05 particle size reduced and in Mg0.8Ti0.05V0.05W0.05 alloy, the particles
agglomerated and particle size growth occurred. Remaining alloys have the intermediate particle size.
Energy Dispersive X-ray analysis (EDAX) results shown that all the elements are presented in the
respective alloy.
Potentiometer having three electrode setup. They are reference electrode, working electrode,
counter electrode. The compacted sample were placed in working electrode and all three electrodes
placed in 6M KOH solution.
Cyclic voltammetry studies helped to understand the redox reactions i.e. oxidation and reduction
reaction. The cyclic voltammetry measurements were carried out in 6M KOH and scanning rate of
1mV/s.
The alloy Mg0.8Ti0.1V0.1 shows high peak current which means the current at the working electrode in a
volt
metric measurement. This ensures that Mg0.8Ti0.1V0.1 has high absorption and desorption rate.
Impedance studies helped to find the resistance, capacitance and diffusion co-efficient values .Nb
react with KOH and forms passive layer which reduces the Kinetics. The alloy Mg0.8Ti0.1V0.1 has low
charge
transfer resistance and high double layer capacitance. So it shown low impedance value. From the
above
discussion it is confirmed that Mg0.8Ti0.1V0.1 has the higher kinetics compared to remaining alloys.