In our previous work, TaF5 and VCl3 were added to Mg, leading to the preparation of samples with good hydriding and dehydriding properties. In this work, Ni was added together with TaF5 and VCl3 to increase the reaction rates with hydrogen and the hydrogen-storage capacity of Mg. The addition of Ni together with TaF5 and VCl3 improved the hydriding and dehydriding properties of the TaF5 and VCl3-added Mg. MgH2 was also added with Ni, TaF5, and VCl3 and Mg-x wt% MgH2-1.25 wt% Ni-1.25 wt% TaF5-1.25 wt% VCl3 (x = 0, 1, 5, and 10) were prepared by reactive mechanical milling. The addition of MgH2 decreased the particle size, lowered the temperature at which hydrogen begins to release rapidly, and increased the hydriding and dehydriding rates for the first 5 min. Adding 1 and 5 wt% MgH2 increased the quantity of hydrogen absorbed for 60 min, Ha (60 min), and the quantity of hydrogen released for 60 min, Hd (60 min). The addition of MgH2 improved the hydriding–dehydriding cycling performance. Among the samples, the sample with x = 5 had the highest hydriding and dehydriding rates for the first 5 min and the best cycling performance, with an effective hydrogen-storage capacity of 6.65 wt%.
We developed a method to determine the activation energy for hydride decomposition using a Sieverts-type apparatus and the Kissinger equation, not using thermal analysis methods. The quantity of hydrogen released from the sample and the temperature of the reactor were first measured as a function of time at different heating rates (Φ) in a Sieverts-type apparatus. The dehydriding rates were calculated according to time and the temperature Tm (at which the dehydriding rate was the highest). Φ and Tm were then applied to the Kissinger equation. The dehydriding rate of Mg-5Ni samples obeyed a first-order law, and the Kissinger equation could thus be used to determine the activation energy. On a heating rate of 3 K/min, the decomposition rate of hydride was the highest at 590 K. From a plot of ln (Φ/Tm2) versus 1/Tm, the obtained activation energy for hydride decomposition was 174 kJ/mole.
Thermal analysis methods - such as TGA, DSC analysis, DTA, and TDS analysis - have been used in many reports to determine the activation energy for hydride decomposition. In our preceding work, we showed that the dehydriding rate of Mg-5Ni samples obeyed the first-order law and the Kissinger equation could thus be used to determine the activation energy. In the present work, we used the Mg-5Ni samples after activation. We obtained Tm at different heating rates by finding the temperature at which the ratio of the desorbed hydrogen quantity Hd change to T change, dHd/dT, was the highest from the desorbed hydrogen quantity Hd versus temperature T curves. Tm’s at different heating rates were also obtained from points of inflection (Φ = dT/dt = 0) in temperature T versus time t curves. The activation energy for hydride decomposition was then calculated by applying Tm’s at different heating rates to the Kissinger equation.
A new study for CH4 reforming to hydrogen and hydrogen storage was performed using magnesium-based alloy. MgH2-12Ni (with the composition of 88 wt% MgH2 + 12 wt% Ni) was prepared in a planetary ball mill by milling in hydrogen atmosphere (reaction-involved milling). X-ray diffraction (XRD) analyses were performed for the samples after reaction-involved milling and after reactions with CH4. The variation of adsorbed or desorbed gas with time was measured by a Sieverts’ type high-pressure apparatus at 773 K. The microstructures of the powders were observed using scanning transmission microscope (STEM) with energy-dispersive X-ray spectroscopy (EDS). The synthesized samples were also characterized using Fourier Transform Infrared (FT-IR) spectroscopy. XRD pattern of MgH2-12Ni after reaction with CH4 of 12 bar at 773 K and decomposition under 1.0 bar at 773 K exhibited phases of MgH2 and Mg2NiH4. This shows that reforming of CH4 was occurred, hydrogen produced after reforming of CH4 was then adsorbed on the particles, and hydrides were formed during cooling to room temperature. Ni and Mg2Ni formed during heating up to 773 K are believed to have brought about catalytic effects for reforming CH4. MgH2-12Ni adsorbed 0.8 wt% reformed CH4 within 1 min in a reaction with CH4 of 12 bar at 773 K and then desorbed 0.8 wt% reformed CH4 (hydrogen-containing mixture) within 1 min under 1 bar at 773 K. Attenuated total reflectance FT-IR spectroscopy (ATR-FTIR) spectra of MgH2-12Ni after reactions under 12 bar CH4 at 723 K and 773 K showed peaks of C-H bending, C=C stretching, O-H stretching, O-H bending, and C-O stretching.
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