Characterization and Hydrogen Storage Capacity Analysis of Dip Coated Lithium Aluminium Hydride Thin Films

Complex metal hydrides are one of the most effective hydrogen storage materials due to their unique property to absorb and desorb hydrogen with the hydrogen storage capacity of about 5-7 wt%. In this study, lithium aluminium hydride (LiAlH4) was coated on glass substrate using dip coating method. The coating conditions investigated were LiAlH4 concentrations of 6 g/l, 10 g/l and 20 g/l and post-annealing time from 0 to 60 min. Phase and grain size of the deposited LiAlH4 were analyzed using X-ray powder diffraction (XRD). Scanning electron microscope (SEM) was used for surface morphology analysis. The hydrogen storage capacity of the deposited thin films was analyzed using thermogravimetric analysis (TGA). The experimental results revealed that the phase of the deposited LiAlH4 thin films on glass substrate were mixed with lithium aluminium hydroxide hydrate (LiAl2(OH)7·2H2O) and lithium hexahydroaluminate (Li3AlH6). The intensity of the LiAl2(OH)7·2H2O and LiAlH4 peaks tends to decrease with increasing LiAlH4 concentration and post-annealing time while the intensity of the Li3AlH6 peaks increased with increasing LiAlH4 concentration and post-annealing time. The grain size was decreased with increasing LiAlH4 concentration and post-annealing time. The smaller grain size the better the hydrogen storage capacity. The hydrogen storage capacity of the deposited LiAlH4 thin film was increased from 0.124 wt % using LiAlH4 concentration of 6 g/l without post-annealing to 1.675 wt % using LiAlH4 concentration of 20 g/l with 60 min post-annealing time.

Improvement in the Hydrogenation and Dehydrogenation Features of Mg by Milling in Hydrogen with Vanadium Chloride

VCl3 (vanadium (III) chloride) was selected as an additive to Mg to increase the hydrogenation and dehydrogenation rates and the hydrogen storage capacity of Mg. Instead of MgH2, Mg was used as a starting material since Mg is cheaper than MgH2. Samples with a composition of 95 wt% Mg + 5 wt% VCl3 (named Mg-5VCl3) were prepared by milling in hydrogen atmosphere (reactive milling). In the first cycle (n=1), Mg-5VCl3 absorbed 5.38 wt% H for 5 min and 5.95 wt% H for 60 min at 573 K in 12 bar hydrogen. The activation of Mg-5VCl3 was completed after three hydrogenation-dehydrogenation cycles. During milling in hydrogen, β-MgH2 and γ-MgH2 were produced. The formed β-MgH2 and γ-MgH2 are considered to have made the effects of reactive milling stronger as β-MgH2 and γ-MgH2 themselves were being pulverized. The introduced defects and the interfaces between the Mg and the phases formed during the reactive milling and during hydrogenation-dehydrogenation cycling are believed to serve as heterogeneous active nucleation sites for MgH2 and Mg-H solid solution. The phases generated during hydrogenation-dehydrognation cycling are also believed to prevent the particles from coalescing during hydrogenation-dehydrognation cycling.

Improvement in the Hydrogenation and Dehydrogenation Features of Mg by Milling in Hydrogen with Vanadium Chloride

VCl3 (vanadium (III) chloride) was selected as an additive to Mg to increase the hydrogenation and dehydrogenation rates and the hydrogen storage capacity of Mg. Instead of MgH2, Mg was used as a starting material since Mg is cheaper than MgH2. Samples with a composition of 95 wt% Mg + 5 wt% VCl3 (named Mg-5VCl3) were prepared by milling in hydrogen atmosphere (reactive milling). In the first cycle (n=1), Mg-5VCl3 absorbed 5.38 wt% H for 5 min and 5.95 wt% H for 60 min at 573 K in 12 bar hydrogen. The activation of Mg-5VCl3 was completed after three hydrogenation-dehydrogenation cycles. During milling in hydrogen, β-MgH2 and γ-MgH2 were produced. The formed β-MgH2 and γ-MgH2 are considered to have made the effects of reactive milling stronger as β-MgH2 and γ-MgH2 themselves were being pulverized. The introduced defects and the interfaces between the Mg and the phases formed during the reactive milling and during hydrogenation-dehydrogenation cycling are believed to serve as heterogeneous active nucleation sites for MgH2 and Mg-H solid solution. The phases generated during hydrogenation-dehydrognation cycling are also believed to prevent the particles from coalescing during hydrogenation-dehydrognation cycling.