Recent Advances on Mg–Li–Al Systems for Solid-State Hydrogen Storage: A Review

The problem of providing compact and safe storage solutions for hydrogen in solid-state materials is demanding and challenging. The storage solutions for hydrogen required high-capacity storage technologies, which preferably operate at low pressures and have good performances in the kinetics of absorption/desorption. Metal hydrides such as magnesium hydride (MgH₂) are promising candidates for such storage solutions, but several drawbacks including high onset desorption temperature (>400°C) and slow sorption kinetics need to be overcome. In this study, we reviewed the recent developments in the hydrogen storage performance development of MgH₂ and found that the destabilization concept has been extensively explored. Lithium alanate or LiAlH₄ has been used as a destabilizing agent in MgH₂–LiAlH₄ (Mg–Li–Al) due to its high capacity of hydrogen, which is 10.5 wt.%, and low onset desorption temperature (∼150°C). In this article, a review of the recent advances in the Mg–Li–Al system for the solid-state hydrogen storage material is studied. We discussed the effect of the ratio of MgH₂ and LiAlH₄, milling time, and additives in the Mg–Li–Al system. After the destabilization concept was introduced, the onset of the desorption temperature and activation energy of MgH₂ were reduced, and the sorption properties improved. Further study showed that the intermetallic alloys of Li_0.92Mg_4.08 and Mg₁₇Al₁₂ that were formed in situ during the dehydrogenation process provide synergetic thermodynamic and kinetic destabilization in the Mg-Li-Al composite system.

De/rehydrogenation measurements indicate that the intermetallic alloys of Li_0.92Mg_4.08 and Mg₁₇Al₁₂ were fully reversibly absorbed and desorbed hydrogen. Next, the remaining challenges and a possible development strategy of the Mg–Li–Al system are analyzed. This review is the first systematic study that focuses on the recent advances in the Mg–Li–Al system for storage solutions for hydrogen in solid-state materials.

Introduction

Due to global environmental issues and the search for new energy sources and carriers, hydrogen is viewed as the most promising alternative to replace fossil fuel-based energy (Yang et al., 2019; Yao L. et al., 2020; Zhang et al., 2019b). Hydrogen is an environment-friendly energy carrier since it has near-zero greenhouse gas emissions. In addition, hydrogen can also reduce the dependence on imported oil for countries without natural resources (Peláez Peláez et al., 2021; Sartbaeva et al., 2008). Hydrogen is not found naturally, but it can be produced from a variety of primary energy sources (e.g., fossil fuels and biomass) and secondary energy sources (e.g., renewable electricity from wind and hydropower) (Abdin et al., 2020; Thapa et al., 2021). As reported by Dunn (Dunn, 2002), since the mid-19^th century, the world has been shifting slowly from one form of energy to another, from solids to liquids and gases, as shown in Figure 1. Compared to fossil fuel, hydrogen holds high energy content and can be stored in large quantities over a long time (Satyapal et al., 2007; Sadhasivam et al., 2017). Hydrogen can offer a long-term solution as it can be continuously supplied and can contribute to a variety of automotive fuel sources. As a result, important research and developmental activities are being carried out to improve the efficiency of the hydrogen-based energy system to make it competitive with the existing fossil fuels.

FIGURE 1

FIGURE 1. Global transition of energy systems 1850–2150 (Dunn, 2002).

In addition to the lack of infrastructures for hydrogen (for example, production, distribution, and refueling), one of the main roadblocks to the spread of hydrogen is reliable hydrogen storage. Hydrogen-compressed gas tanks, hydrogen liquid tanks, and solid-state storage of hydrogen are possible current approaches to store hydrogen (Sazelee et al., 2018; Doğan et al., 2020). Liquid hydrogen storage systems present a promising opportunity to efficiently increase the capacity of hydrogen fueling stations and are also preferred for space missions (Jiang et al., 2021; Correa-Jullian & Groth, 2022). Although liquid hydrogen tanks are usually super-insulated tanks, at approximately 20 K, boil-off may occur due to the substantial temperature difference between the ambient and liquid hydrogen (Khurana et al., 2006; Zuo et al., 2020). On the other hand, although storage in a compressed gas tank is possible, technical simplicity and the fast filling-releasing rate requires very high pressure and has high costs (Zheng et al., 2012). Therefore, solid-state hydrogen storage draws more attention due to its security, high storage capacity, and hydrogen purification (Niaz et al., 2015; Sazelee et al., 2020b; Ye et al., 2020). However, a drawback of the solid-state hydrogen storage materials, especially for metal/complex hydrides, is their high decomposition temperature and sluggish sorption kinetics (absorb and desorb hydrogen) (Daulbayev et al., 2022).

An Overview of the Mg–Li–Al Systems

A wide variety of materials are currently being considered as the future reversible solid-state hydrogen storage materials (Zacharia & Rather, 2015). As claimed by David (David, 2005), the ability to separate hydrogen differs from each metal, and this ability depends on the metals’ purity, surface structure, and morphology. The list of the storage systems with their gravimetric capacities is shown in Table 1.

TABLE 1

TABLE 1. Hydride materials and theoretical gravimetric hydrogen density (Kojima, 2019).

Globally, among the solid-state hydrogen storage materials, research into the use of magnesium (Mg) in hydrogen storage applications is of considerable importance (Jain et al., 2010; Crivello et al., 2016; Zhang et al., 2019a; Ouyang et al., 2020). In recent years, much attention has been given to examining the specific material properties of Mg alloys for the development of new functional materials (Yang et al., 2021). Mg is also one of the most abundant and lightly packed solid materials (1.738 g/cm³) (Li et al., 2015). Increasing interest in MgH₂ has been shown due to its high hydrogen storage capacity (7.6 wt.%), low cost, and superior reversibility (Imamura et al., 2005; Sakintuna et al., 2007; Montone et al., 2010; El Khatabi et al., 2018).

Thus, researchers suggested that hydrogen interaction with Mg is one of the most promising approaches (Eftekhari & Fang, 2017; Luo et al., 2019). While Mg satisfies many practical application requirements, the on-board applications can still not be used for many reasons, such as 1) the desorption/absorption kinetics process is very slow for pure Mg (Schlapbach et al., 1979) and 2) releasing hydrogen at high temperatures (>400°C), is correlated with the high stability of Mg–H bonds and is expressed in the high enthalpy of hydride formation (Zaluska et al., 1999; Dornheim et al., 2007; Jain et al., 2010). To boost MgH₂ hydrogen storage properties, numerous techniques have been developed including alloying (Li et al., 2019; Liang et al., 2020; Marques et al., 2020; Dematteis et al., 2021), nanosizing (Ranjbar et al., 2009; Zhang et al., 2015; Yu et al., 2017; Ma et al., 2021), and catalyzing (Polanski et al., 2011; Baricco et al., 2012; Ismail et al., 2016; Jangir et al., 2018; Yao P. et al., 2020; Ismail, 2021; Liu et al., 2021; Lu et al., 2021; Zhang et al., 2021). The remarkable improvements of these techniques have been demonstrated as the most successful methods but still do not fulfill the Department of Energy (DOE) target for solid-state hydrogen storage materials (Urgnani et al., 2008).

The ‘destabilization concept’ has been introduced as another method to enhance the sorption kinetics and alter the thermodynamics of MgH₂ (Vajo et al., 2004; Vajo et al., 2007; Vajo & Olson, 2007; Ali et al., 2021; Sulaiman et al., 2021b). The concept aims to modify the thermodynamics and kinetics of the hydrogen sorption reaction (Barkhordarian et al., 2007). Thermodynamic destabilization is achieved when the mixed hydrides react and form a new intermediate compound that alters the thermodynamic properties and facilitates hydrogen release and absorption (Reilly & Wiswall, 1968; Ismail & Mustafa, 2016; Ali & Ismail, 2021). Since several studies have been reported on this concept, researchers attempted to destabilize MgH₂ by using the reactive hydride composite approach, as in the systems such as MgH₂–AlH₃ (Liu et al., 2013; Liu et al., 2014; Ismail, 2016), MgH₂–Mg(AlH₄)₂ (Wang et al., 2014), MgH₂–NaAlH₄ (Ismail et al., 2013; Rafi-ud-din et al., 2014; Bendyna et al., 2015; Ali & Ismail, 2021), MgH₂–NaBH₄ (Mao et al., 2009; Kato et al., 2012; Mulas et al., 2012), and other promising destabilizing systems. Among all the destabilizing systems, the researchers tried the destabilizing concept with the most studied materials under the complex hydride, which is LiAlH₄, in order to enhance the performance for the practical use of MgH₂. Due to its high capacity for storage (10.5 wt.%), LiAlH₄ is interesting compared to the other complex hydrides such as NaAlH₄ (5.5 wt.%) (Sazelee & Ismail, 2021). LiAlH₄ decomposes in three steps (Liu C. et al., 2020). With 5.3 wt.% of H₂ at 150°C, the first decomposition occurs as in Eq. 1. Meanwhile, the second decomposition occurs at ∼180°C (2.6 wt.%), and the third decomposition occurs with a temperature above 350°C (2.6 wt.%), as in Eqs 2, 3, respectively.

$3\text{L}\text{i}\text{A}\text{l}{\text{H}}_4\to \text{L}{\text{i}}_3\text{A}\text{l}{\text{H}}_6+2\text{A}\text{l}+3{\text{H}}_2,(1)$

$\text{L}{\text{i}}_3\text{A}\text{l}{\text{H}}_6\to 3\text{L}\text{i}\text{H}+\text{A}\text{l}+3/2{\text{H}}_2,(2)$

$3\text{L}\text{i}\text{H}+3\text{A}\text{l}\to 3\text{L}\text{i}\text{A}\text{l}+3/2{\text{H}}_2.(3)$

Even though LiAlH₄ offers several benefits, it suffers from slow desorption kinetics (hard to release hydrogen at certain conditions), and the last reaction temperature is quite high (Hsu et al., 2014a; Ismail et al., 2021). The enthalpy change of Eq. 1 is calculated to be −27 kJmol⁻¹ (Ke & Chen, 2007), which indicates that the hydrogen evolution from the solid LiAlH₄ is thermodynamically allowed at low temperatures but is restricted by a relatively high kinetic barrier in transforming tetrahedron (AlH₄)⁻ to octahedron (AlH₆)³⁻ (Chen et al., 2010). All the theoretical and experimental works showed that the LiAlH₄ system could absorb hydrogen when a higher hydrogen pressure is applied (more than 8.0 MPa) (Sazelee & Ismail, 2021). This is because LiAlH₄ is restricted by weak reversibility and very high thermodynamic stability (Graetz et al., 2008). For instance, Jang et al. (Jang et al., 2006) stated that more than 10³ bar of hydrogen partial pressure is required for the absorption reaction of Li₃AlH₆ to LiAlH₄ above the room temperature.

To that end, this review concentrated on the destabilized MgH₂–LiAlH₄ composite (Mg–Li–Al system). This idea is based on the hypothesis that so-called mechano-chemical reactions could occur between MgH₂ and LiAlH₄, and the intermediate phases (Li_0.92Mg_4.08 and Mg₁₇Al₁₂) could be formed to modify the thermal stability of the Mg–Li–Al system. The primary goal of this article is to review the progress of the destabilized MgH₂–LiAlH₄ system in improving the performance of MgH₂ and LiAlH₄ hydrogen storage. Up to date, no researchers have been reviewing this Mg–Li–Al system. Therefore, we believed that the researchers and practitioners involved in research on hydrogen storage materials will benefit from this review article. Figure 2 illustrates the main topics discussed in this review.

FIGURE 2

FIGURE 2. Schematic representation of the main topics discussed in this review.

The Effect of the MgH₂ and LiAlH₄ Ratios

The first systematic study on the mutual destabilization between MgH₂ and LiAlH₄ was reported by Zhang et al. (Zhang et al., 2008). They studied the different molar ratios (1:1, 2:1, and 4:1) of MgH₂–LiAlH₄. The result showed that the initial desorption temperature for the MgH₂–relevant decomposition in all the different molar ratios of the MgH₂–LiAlH₄ composite was decreased to ∼250°C, which is 50°C lower than the milled MgH₂, as shown in Figure 3. By using the Kissinger method, the activation energy value of MgH₂–relevant decomposition in the composite was reduced dramatically compared to the undoped MgH₂. The dehydrogenation enthalpies of the MgH₂–LiAlH₄ composites with different molar ratios 4:1, 2:1, and 1:1 are 61, 48.66, and 45 kJ/mol, respectively. These enthalpy values were smaller than the undoped MgH₂ (76 kJ/mol), which indicates that MgH₂ was destabilized by LiAlH₄. Further study revealed that the dehydrogenation process in the MgH₂–LiAlH₄ system can be divided into two steps: the first step is due to the two-step decomposition of LiAlH₄ (The first step is the decomposition of LiAlH₄ to Li₃AlH₆ and Al (as in Eq. 1), and the second step is the decomposition of Li₃AlH₆ to LiH and Al (as in Eq. 2) and the second step is due to the reaction between LiH and Al phases to form Li_0.92Mg_4.08 and Mg₁₇Al₁₂ phases, as indicated in Eqs 4, 5.

$4.08\text{M}\text{g}{\text{H}}_2+0.92\text{L}\text{i}\text{H}\to \text{L}{\text{i}}_{0.92}\text{M}{\text{g}}_{.08}+4.54{\text{H}}_2,(4)$

$17\text{M}\text{g}{\text{H}}_2+12\text{A}\text{l}\to \text{A}{\text{l}}_{12}\text{M}{\text{g}}_{17}+17{\text{H}}_2.(5)$

FIGURE 3

FIGURE 3. Initial desorption temperature for the as-milled LiAlH₄, as-milled MgH₂, and MgH₂–LiAlH₄ composites with different molar ratios (1:1, 2:1, and 4:1) (Zhang et al., 2008).

Moreover, rehydrogenation measurement shows that Li_0.92Mg_4.08 and Mg₁₇Al₁₂ are the fully absorbed hydrogen, as shown in Eqs 6, 7.

$\text{L}{\text{i}}_{0.92}\text{M}{\text{g}}_{4.08}+4.5{\text{H}}_2\to 4.08\text{M}\text{g}{\text{H}}_2+0.92\text{L}\text{i}\text{H},(6)$

$\text{A}{\text{l}}_{12}\text{M}{\text{g}}_{17}+\left(17-2y\right){\text{H}}_2\to \text{y}\text{M}{\text{g}}_2\text{A}{\text{l}}_3+\left(17-2y\right)\text{M}\text{g}{\text{H}}_2+\left(12-3y\right)\text{A}\text{l}.(7)$

Lin and Tsai (Lin & Tsai, 2017) in their study exposed that the diffraction peak intensity of LiAlH₄ decreased with an increasing amount of MgH₂ addition, as in Figure 4. No other compounds were found after milling, indicating that no reaction occurred between LiAlH₄ and MgH₂ during the milling process. This result is in agreement with a previous study by Hsu et al. (Hsu et al., 2014b), in which the diffraction peak intensity of MgH₂ increased with a decreasing amount of LiAlH₄ in the MgH₂–LiAlH₄ mixture.

FIGURE 4

FIGURE 4. XRD patterns of different ratios of MgH₂ and LiAlH₄ in the Mg–Li–Al system after the milling process (Lin & Tsai, 2017).

Next, the temperatures of desorption and the amount of hydrogen released from the composites of MgH₂–LiAlH₄ were quantitively evaluated by the thermogravimetric analysis (TGA), as shown in Table 2. It was evident that with the increasing MgH₂ content in the composites, the first desorption temperature was lowered. These findings showed that MgH₂ played an effective role in reducing the initial desorption temperature of these composites. As soon as the desorption of these composites was completed, absorption kinetics was initiated with a temperature maintained at 400°C, while charging hydrogen to the target pressure. As displayed in Table 2, the total amount of hydrogen absorbed (wt.%) increased from 0.3 to 3, and the onset desorption temperature also decreased to 85°C compared to 100°C with an increase in the MgH₂ content in the composites. The results proved that MgH₂ was the main compound that exhibited reversibility concerning the hydrogen absorption/desorption reaction. As shown in Table 2, the ability of the MgH₂–LiAlH₄ composite to absorb hydrogen increased as the MgH₂ ratio increased.

TABLE 2

TABLE 2. TGA results show the temperature of desorption and the amount of hydrogen absorption/desorption from MgH₂–LiAlH₄ with different amounts of composites (Lin & Tsai, 2017).

The LiAlH₄–MgH₂ hydrogen storage system was studied by Chen et al. (Chen et al., 2010). The commercial LiAlH₄ was decomposed at 163°C; meanwhile, the commercial MgH₂ decomposed at 405°C. However, LiAlH₄ and MgH₂ mixtures start to release hydrogen at ∼107°C, indicating that the combination of LiAlH₄ and MgH₂ may improve their thermodynamic properties. Measurement of the XRD was performed after desorption, and the results showed that in all the LiAlH₄–xMgH₂ composites (LiAlH₄–MgH₂, LiAlH₄–2.5MgH₂, and LiAlH₄–4MgH₂), the Mg₁₇Al₁₂ phase was formed. In addition, the LiAlH₄–4MgH₂ composite contained major Li_0.92Mg_4.08 phases, whereas LiAlH₄–2.5MgH₂ contained minor Li_0.92Mg_4.08 phases, as shown in Figure 5. This indicates that Li_0.92Mg_4.08 can be formed while the ratio of MgH₂/LiAH₄ is relatively high. These composites also undergo an absorption process at 350°C under a pressure of 10 MPa hydrogen. In 60 min, the LiAlH₄–4MgH₂ composites reach 90% of their maximum absorption capacity. In brief, these reported studies indicated that the combination of LiAlH₄ and MgH₂ may have been shown to affect the thermal stability of both LiAlH₄ and MgH₂ by the formation of intermetallic Mg₁₇Al₁₂ and Li_0.92Mg_4.08.

FIGURE 5

FIGURE 5. XRD patterns of LiAlH₄ + xMgH₂ (x = 1, 2.5, and 4) after dehydrogenation at 350°C (Chen et al., 2010).

Based on the abovementioned discussions, the different molar ratios of the MgH₂–LiAlH₄ composites also affected the performance of the Mg–Li–Al system. This review article outlined that 4MgH₂–LiAlH₄ shows the best performance compared to the other ratios (e.g., 1:1, 2:1, and 2.5:1). The 4MgH₂–LiAlH₄ composite created an intermediate compound of Li_0.92Mg_4.08 and Mg₁₇Al₁₂ that helps to enhance the hydrogen storage performance of the Mg–Li–Al system.

The Effect of Different Milling Times

Vittetoe et al. (Vittetoe et al., 2009) explored the destabilization effects of the combination of LiAlH₄ with a nanocrystalline MgH₂ by mechanical–chemical milling concerning reversibility and kinetics problems. Interestingly, they investigated the LiAlH₄–MgH₂ composite with different durations of milling (1, 2, 3, and 5 h). They discovered that the LiAlH₄–MgH₂ samples that have been milled for 1, 2, and 3 h started to decompose at ∼100°C. Researchers verified that for an optimal ball milling period of 2 h, a three-step hydrogen desorption response with an early-onset temperature and greater amount of hydrogen release is required. In addition, further study elucidates LiAlH₄–MgH₂ and LiAlH₄–nanoMgH₂ of TGA and differential scanning calorimetry (DSC) profiles milled for 2 h, as seen in Figure 6. The LiAlH₄–nanoMgH₂ systems show a greater weight loss of approximately 5.2 wt.% (∼200°C), at least 1.0 wt.% higher capacity than the commercial-grade sample (LiAlH₄–MgH₂).

FIGURE 6

FIGURE 6. Comparison of TGA/DSC mechano-chemically milled for 2 h for LiAlH₄-MgH₂ and LiAlH₄–nanoMgH₂ (Vittetoe et al., 2009).

As LiAlH₄–nanoMgH₂ showed better performance than LiAlH₄–MgH₂, this material underwent repeated absorption of hydrogen (80 bars) and desorption at two different temperatures (300 and 350°C). After numerous attempts of hydrogen absorption–desorption experiments, these samples were carefully examined under a scanning electron microscope (SEM), as shown in Figure 7. SEM images of LiAlH₄–nanoMgH₂ after cycling indicated that the sample had a relatively smaller grain with a highly porous matrix and uniform (as in Figure 7B) as compared to LiAlH₄–nanoMgH₂ (as in Figure 7A). This is due to the host structure’s effective uptake and release of hydrogen.

FIGURE 7

FIGURE 7. SEM images of LiAlH₄–nanoMgH₂ (A) after milling for 2 h and (B) after absorption–desorption cycling (Vittetoe et al., 2009).

Milanovic et al. (Milanović et al., 2013) investigated the catalytic influence on the desorption of hydrogen from MgH₂. Indeed, when mixing MgH₂ with a 5 wt.% of LiAlH₄ for 15 min, the peak of the hydrogen desorption shifts to a lower temperature than as received MgH₂ and as milled MgH₂. In this study, milling up to 30 and 60 min of the MgH₂–LiAlH₄ composites may reduce the catalytic activity of the LiAlH₄ additive, as revealed by the shift to a higher peak of desorption temperatures. According to Leon et al. (Léon et al., 2009), experiments conducted under various conditions revealed that the milling parameters, in particular the milling speed and milling time, can be of great importance through reactive ball milling for the formation of the new hydride phase. Next, Ding et al. (Ding et al., 2013) studied the MgH₂–LiAlH₄ composites milled at different milling times (2, 5, and 9 h). The result revealed that MgH₂–LiAlH₄ composites milled for 2 h decompose in the temperature ranges of ∼130–183°C; meanwhile, after the MgH₂–LiAlH₄ composites were milled for 5 h, the composites start to release hydrogen at 102°C. However, the capacity of hydrogen released decreased compared with 2 h milled composites. In addition to that, the initial desorption temperature decreases to 86°C when the milling time increases to 9 h, but the amount of hydrogen released also decreases. The XRD pattern showed that the peaks of Li₃AlH₆ and Al appeared after milling the MgH₂–LiAlH₄ composites up to 5 h. Interestingly, milling up to 9 h proved that the intensity peaks of Li₃AlH₆ and Al become stronger. This indicated that more LiAlH₄ has been decomposed into Li₃AlH₆ and Al, accounting for the lowest onset desorption temperature. Based on the results obtained, the lower decomposition temperature was attributed to the decomposition of LiAlH₄ that had occurred, and more LiAlH₄ decomposed as the milling time increased. In addition, the peaks of the Mg₁₇Al₁₂ phase can also be detected when the MgH₂–LiAlH₄ composites were heated to 250°C. Furthermore, Ding et al. (Ding et al., 2013) also studied the reversibility of the destabilized MgH₂–LiAlH₄ composite under a hydrogen pressure of 3 MPa and at 300°C, and the results show that the MgH₂–LiAlH₄ composite exhibits fast ab/desorption kinetics in the first two cycles, but the ab/desorption kinetics worsened during the third cycle, as shown in Figure 8. Moreover, SEM images indicated that the morphology of MgH₂–LiAlH₄ composites was smaller. A reduction in the particle size and crystallite size results in the introduction of high surface defect density and the creation of more grain boundaries. In addition to that, a high density of the nanosized catalyst particles forms a large number of nucleation sites at the surface of the LiAlH₄ matrix, leading to the larger surface area of LiAlH₄ particles, as indicated by Zhai et al. (Zhai et al., 2012). Xia et al. (Xia et al., 2020) also stated that the morphological change should be beneficial for the enhancement of the desorption properties of LiAlH₄, owing to the reduction of the particle size and the process of creating small crystallite sizes. Halim Yap et al. (Halim Yap et al., 2019), in their study, revealed that the decrement of the grain sizes led to the increment of the contact surface area. As a result, the desorption reaction of hydrogen has been improved due to the reduction of the hydrogen diffusion length. A study conducted by Czujko et al. (Czujko et al., 2011) revealed that the average particle size of MgH₂+50 wt% LiAlH₄ composites was reduced to ∼3.5 ± 2.7 µm. It demonstrated that during MgH₂ ball milling, lithium alanate could act as a lubricant, and the reduction of particle size is much less efficient when the LiAlH₄ additive level reaches 50 wt.%. Based on this subsection, appropriate milling time is beneficial to the Mg–Li–Al systems. This indicates that the milling time at a suitable time is helpful to improve the hydrogen storage performance of the Mg–Li–Al system. The variation of the milling duration has obvious effects on the onset desorption temperature, activation energy, and morphology of the samples.

FIGURE 8

FIGURE 8. Reversibility study for the initial three cycles of the destabilized MgH₂–LiAlH₄ composite under a hydrogen pressure of 3 MPa and at 300°C (Ding et al., 2013).

The Effect of Different Additives

A study conducted by Halim Yap and Ismail (Halim Yap & Ismail, 2017) indicated that the hydrogen sorption properties of the MgH₂–LiAlH₄ system can be enhanced by the addition of K₂ZrF₆. The onset desorption temperature for 4MgH₂–LiAlH₄ exhibited two significant stages. For the 4MgH₂–LiAlH₄ systems, the onset desorption temperature was 135 and 275°C for the first and second desorption stages, with the total amount of hydrogen desorption being 7.5 wt.%. After the addition of 10 wt.% K₂ZrF₆, the desorption temperature for the first and second stages was decreased by 40 and 25°C, respectively. In addition, 4MgH₂–LiAlH₄ + 10 wt.% K₂ZrF₆ demonstrates better kinetics of desorption, and the value of activation energy was decreased to 102.9 kJ/mol compared to the undoped composites (129.8 kJ/mol). However, the absorption kinetics under 33.0 atm at 320°C exposed that adding 10 wt.% of K₂ZrF₆ to 4MgH₂–LiAlH₄ showed no improvement in the absorption of hydrogen. Meanwhile, the SEM images for comparing the morphology of undoped and doped samples are shown in Figure 9. The doped samples show that the particles size is less agglomerated and smaller as in Figure 9D than the undoped samples (Figure 9C). This result was also supported by Ranjbar et al. (Ranjbar et al., 2010) who suggested that the smaller particle size improves hydrogen ab/desorption as it makes the particle larger surface area and reduces the diffusion length of hydrogen.

FIGURE 9

FIGURE 9. SEM images for the (A) as-received MgH₂, (B) as-milled MgH₂, (C) 4MgH₂-LiAlH₄, and (D) 4MgH₂-LiAlH₄ + 10 wt.% K₂ZrF₆ (Halim Yap & Ismail, 2017).

Further research indicated that the new peaks of Al₃Zr and KH (indicating LiAlH₄ react with K₂ZrF₆) were formed after 4MgH₂–LiAlH₄ + 10 wt.% K₂ZrF₆ were heated at 200°C. In addition, the peaks of MgH₂ were also present as well as LiH and Al (illustrated the decomposition as in Eq. 2). Heating up to 450°C, the peaks of Mg, Li_0.92Mg_4.08, and Mg₁₇Al₁₂ were detected, whereas the Al₃Zr and KH peaks remained unchanged. Furthermore, the XRD pattern of absorption for K₂ZrF₆-doped 4MgH₂–LiAlH₄ sample at 300°C also exposed the peaks of Al₃Zr, KH, LiH, and Al remain unchanged. However, the peaks of the Mg₁₇Al₁₂ and Li_0.92Mg_4.08 disappeared, and it is suggested that a reaction occurred during the absorption process, as indicated in Eqs 6, 7. The amount of K₂ZrF₆ was increased to 20 wt.% to obtain a better insight into the F-containing, Zr-containing, and K-containing phase structures. New minor peaks attributed to LiF were detected along with the KH and Al₃Zr phases. Therefore, it is recognized that the new LiF, KH, and Al₃Zr products created during the heating process worked together as active components to work on improving the 4MgH₂–LiAlH₄ system of the hydrogen storage performance. The hydrogen storage properties of MgH₂/LiAlH₄ were improved by the addition of SrFe₁₂O₁₉, as suggested by Sulaiman and Ismail (Sulaiman & Ismail, 2017). The result disclosed that the addition of 5 wt.% of SrFe₁₂O₁₉ resulted in a decrease of 40 and 10°C in the first and second stages of desorption, respectively, compared to the MgH₂/LiAlH₄ system. The doped samples begin to release hydrogen at ∼80°C for the first stages and ∼260°C for the second stages. Interestingly, the hydrogen released by the doped samples was 7.1 wt.%, which is the amount of hydrogen released equivalent to milled MgH₂. The energy barriers for the release of hydrogen affected the kinetic desorption performance of the samples. From the calculation of as-received MgH₂, the activation energy was 175 kJ/mol. However, the activation energy was decreased to 133 kJ/mol after MgH₂ was milled for 1 h. This proves that the value of the activation energy is also affected by the milling process (Sabitu & Goudy, 2012; Ismail, 2015; Lin et al., 2015; Zhang et al., 2017). Furthermore, after destabilizing MgH₂ with LiAlH₄, the activation energy was reduced to 121 kJ/mol, which showed a reduction of 12 kJ/mol compared to the milled MgH₂ (133 kJ/mol). The improvement of desorption kinetics is related to the energy barrier for the hydrogen release from the composite. Lower activation energy means faster kinetics. In this context, the activation energy is the least energy required to instigate the decomposition process of the system (Ismail et al., 2020). The activation energy decreased to 104 kJ/mol, after the addition of 5 wt.% SrFe₁₂O₁₉ to 4MgH₂–LiAlH₄. Furthermore, these findings appear to be comparable to the previous studies reporting on the role of catalysts in reducing the activation energy, leading to improved dehydriding kinetics (Sazelee et al., 2019). Conversely, the newly developed products formed during the heating process of in situ Li₂Fe₃O₄ and Al₂Sr exhibit a synergistically catalytic effect on the improvement of the 4MgH₂–LiAlH₄ composites.

According to Mao et al. (Mao et al., 2011), dehydrogenation has been improved after LiAlH₄ was combined with MgH₂, in which the first-stage desorption temperature is close to LiAlH₄ (∼150°C), while the second-stage desorption was completed at 233°C. This suggested that in the binary LiAlH₄–MgH₂ system, a mutual destabilization occurred. However, after being doped with TiF_3, hydrogen starts to release at ∼60°C (100°C lower than the undoped LiAlH₄–MgH₂ system). The desorption and absorption kinetics were also improved after the addition of TiF₃. For the LiAlH₄–MgH₂–TiF₃ system, the amount of hydrogen desorbed was 2.48 wt.% after 10 min, compared to the LiAlH₄–MgH₂ system (1.59 wt.%) at 300°C. Furthermore, the reversibility of this system was performed at 300°C under ∼2 MPa for both samples. LiAlH₄–MgH₂–TiF₃ systems demonstrate the ability to absorb 2.68 wt.% hydrogen after 5 min, which is greater than the LiAlH₄–MgH₂ system (1.75 wt.%). Further study showed that the intermediate phase of Mg₁₇Al₁₂ and Li₃Mg₇ produced during the heating process is mainly due to the Al/LiH reaction with MgH₂, as shown in Eqs 5, 8:

$3\text{L}\text{i}\text{H}+7\text{M}\text{g}{\text{H}}_2\to \text{L}{\text{i}}_3\text{M}{\text{g}}_7+8.5{\text{H}}_2.(8)$

The hydrogen sorption properties of 4MgH₂–LiAlH₄ were greatly improved after the addition of 5 wt.% Fe₂O₃, as eloquently stated by Mustafa et al. (Mustafa & Ismail, 2014). As-milled MgH₂ can release hydrogen at 350°C; meanwhile, the as-milled LiAlH₄ can release at 135–160°C. For the destabilized system of 4MgH₂–LiAlH₄, the onset desorption temperature was reduced similar to the as-milled LiAlH₄. However, after the addition of Fe₂O₃, the onset of desorption was decreased to 95°C. The desorption and absorption kinetics were also improved after the addition of Fe₂O₃. The apparent activation energy of 4MgH₂–LiAlH₄ + Fe₂O₃ was reduced to 117 kJ/mol compared to the undoped 4MgH₂–LiAlH₄ systems. Further research exposed that the Li₂Fe₃O₄ was developed by heating 4MgH₂–LiAlH₄ + Fe₂O₃ up to 400°C and revealed that the Li₂Fe₃O₄ also plays a crucial role in reducing the value of desorption temperature and activation energy in the 4MgH₂–LiAlH₄ systems.

According to Wan et al. (Wan et al., 2013), the hydrogen storage performance of MgH₂–LiAlH₄ was effectively improved after the addition of MnFe₂O₄ nanoparticles. As indicated in Table 3, the onset desorption temperature for MgH₂–LiAlH₄ + 5 mol% of MnFe₂O₄ and MgH₂–LiAlH₄ + 7 mol% of MnFe₂O₄ revealed the lowest onset desorption temperature. However, the total amount of hydrogen released for MgH₂–LiAlH₄ + 5 mol% of MnFe₂O₄ is higher than the addition of 7 mol% of MnFe₂O₄. Nonetheless, the addition of MnFe₂O₄ can reduce the onset desorption temperature of the MgH₂–LiAlH₄ systems.

TABLE 3

TABLE 3. Onset desorption temperature and the total amount of hydrogen released for MgH₂–LiAlH₄ and MgH₂–LiAlH₄ + xMnFe₂O₄ composites (x = 1, 2, 5, and 7 mol% of MnFe₂O₄ nanoparticles) (Wan et al., 2013).

For the desorption kinetics at 200°C, under 0.1 MPa, the MgH₂–LiAlH₄ systems release 0.94 wt.% hydrogen, whereas the MgH₂–LiAlH₄ + 5 mol% of MnFe₂O₄ can release 2.91 wt.%. Furthermore, the reversibility for those samples was investigated at 300°C under 3 MPa, and the doped samples show better absorption kinetics than the undoped samples. For MgH₂–LiAlH₄ + 5 mol% of MnFe₂O₄, a hydrogen absorption capacity of 3.64 wt.% was achieved within 300 s. In the meantime, the MgH₂–LiAlH₄ systems only absorbed 2.81 wt.% of hydrogen under the same conditions. Moreover, after heating up to 400°C, the XRD pattern shows the peaks of Li_0.92Mg_4.08 and Mg₁₇Al₁₂. Furthermore, the new peak of Fe_0.872O observed also indicated that the interaction between LiAlH₄ and MnFe₂O₄ had occurred. However, no Mn-containing peak has been seen due to the low amount of MnFe₂O₄ that has been used. Also, the XRD pattern observed after the absorption kinetics at 300°C stated that no peaks of Li_0.92Mg_4.08 and Mg₁₇Al₁₂ have been detected. The peaks of Fe_0.872O can still be seen in the XRD pattern of the absorption results. Therefore, they concluded that the in situ formed Fe oxide and the Mn-containing peak enhanced hydrogen storage performances of the MgH₂–LiAlH₄ system.

The impact of various additives on the hydrogen storage properties of the MgH₂-LiAlH₄ system was studied by Ismail et al. (Ismail et al., 2011). Milled MgH₂ starts to decompose at 330°C and desorb about 7.1 wt.% of hydrogen at 420°C. Meanwhile, the as-milled LiAlH₄ decomposes at ∼142°C for the first and ∼173°C for the second stage. After the two hydrides (MgH₂–LiAlH₄) with ratio 4:1 have been mixed, the samples began to decompose at 130°C for the first stage (attributed to the decomposition of LiAlH₄), while at 270°C for the second stages (corresponding to the decomposition of Li₃AlH₆). The 4MgH₂–LiAlH₄ was completed at ∼360°C with 7.5 wt.% of hydrogen released (attributed to the decomposition of MgH₂). After the addition of metal halides, the temperature-programmed desorption (TPD) curves of 4MgH₂–LiAlH₄ systems were significantly improved. TiF₃ followed by NiF₂, CrF₂, NbF₅, and YF₃ showed a strong catalytic influence on the decomposition of MgH₂–LiAlH₄, as shown in Figure 10. The MgH₂–LiAlH₄ composite doped with TiF₃ begins to decompose at 70°C. However, the desorption kinetics of the MgH₂–LiAlH₄ composite were significantly enhanced after the addition of 5 wt.% of metal halides. Furthermore, the addition of metal halide additives could reduce the activation energy of the MgH₂–LiAlH₄ composite. The apparent activation energy for the MgH₂–LiAlH₄ composite with the selected different metal halides is shown in Table 4.

FIGURE 10

FIGURE 10. Decomposition temperature results of the MgH₂-LiAlH₄ composite with different selected metal halides (Ismail et al., 2011).

TABLE 4

TABLE 4. Apparent activation energy for the MgH₂-LiAlH₄ composite with different selected metal halides (Ismail et al., 2011).

In order to study the phase structure of these samples, the 4MgH₂–LiAlH₄ samples were characterized by using XRD. After the samples were heated up to 400°C, apart from Mg, the intermediate phases of Li_0.92Mg_4.08 and Al₁₂Mg₁₇ were eventually created in the composite system. The XRD measurements were also carried out on the absorption kinetics. The results showed that the peaks of Li_0.92Mg_4.08 and Al₁₂Mg₁₇ disappeared; meanwhile, the appearance of peaks of Al₃Mg₂ indicated that the reaction, as in Eqs 6, 7, occurred during the absorption process. For the doped samples, further research showed that LiF and Al₃Ti are believed to act as the actual catalyst that can enhance the interaction of the MgH₂–LiAlH₄ system, while speeding up the hydrogen desorption process of the MgH₂–LiAlH₄ system. According to Mustafa et al. (Mustafa et al., 2015), the addition of K₂TiF₆ improves the 4MgH₂–LiAlH₄ system of hydrogen storage performance. The desorption temperature of the 4MgH₂–LiAlH₄ system was reduced to 80 and 250°C for the first and second stages, respectively, after the addition of K₂TiF₆. Meanwhile, the 4MgH₂–LiAlH₄ composite decomposed at 130 and 270°C for the first and second stages, respectively. In addition, after the addition of K₂TiF₆, desorption and absorption kinetics were also enhanced. The activation energy for 4MgH₂–LiAlH₄ systems has also been reduced from 126 to 107 kJ/mol. The XRD analysis was conducted on 4MgH₂–LiAlH₄ + K₂TiF₆ for the possible reaction of catalytic additives on the 4MgH₂–LiAlH₄ systems. The intermediate phases of Li_0.92Mg_4.08, Al₁₂Mg_17, and Mg were eventually formed after desorption at 400°C. The complete recovery of LiH and MgH₂ from the Li–Mg and Al–Mg alloys was accomplished in the absorption samples due to the reaction of Al₁₂Mg₁₇ and Li_0.92Mg_4.08 with hydrogen. Further verification stated that the peaks of TiH₂, LiF, and Al₃Ti act as the real catalyst, thus proving that the addition of K₂TiF₆ enhanced the sorption properties of the 4MgH₂–LiAlH₄ systems.

Recently, Sulaiman et al. (Sulaiman et al., 2021a) observed an improvement in the onset desorption temperature and the morphology of the 4MgH₂–LiAlH₄ systems when 5 wt.% of Al₂TiO₅ was added. The hydrogen started to release at 85°C which is decreased by 35°C for the undoped systems. It is important to note that the inclusion of Al₂TiO₅ to the 4MgH₂–LiAlH₄ systems resulted in significantly smaller particle sizes which help to shorten the diffusion length and larger nucleation sites. Moreover, based on the XRD result, the new in situ active species of LiTi₂O₄, TiH_2, and AlTi₂ were detected after the de/rehydrogenation process which is believed to act as a true catalyzer in improving the hydrogen storage performance of the Al₂TiO₅-doped Mg–Li–Al systems. From the results, it is noted that the addition of additives ameliorates the performance of the MgH₂–LiAlH₄ composite by reducing the onset decomposition temperature and fastening the sorption kinetics performance than the unary MgH₂ and LiAlH₄, as demonstrated in Table 5. Table 5 presents the onset desorption temperature, total desorption, absorption capacity, and activation energy for the MgH₂–LiAlH₄ system doped with several additives. The undoped MgH₂, LiAlH₄, and MgH₂–LiAlH₄ systems are also included in Table 5 for comparison purposes.

TABLE 5

TABLE 5. Hydrogen storage performance of the Mg–Li–Al doped system with several additives compared with the undoped Mg–Li–Al system and unary MgH₂ and LiAlH₄.

Based on the abovementioned discussion and Table 5, it can be stated that the addition of the additives significantly enhanced the hydrogen storage performance of the MgH₂–LiAlH₄ systems. It is reported that the active species that are in situ formed during the heating process are believed to play a catalytic role in enhancing the hydrogen sorption performance of the MgH₂–LiAlH₄ additive system. Up to this date, the addition of MnFe₂O₄ to Mg–Li–Al composites has presented the best performance which can release hydrogen approximately at 55°C (Wan et al., 2013). In addition, the MgH₂–LiAlH₄–MnFe₂O₄ system can absorb 3.64 wt.% of hydrogen in only 300 s and desorb more hydrogen (approximately 4 wt.% in 200 s), which shows a better performance in the sorption kinetics of MgH₂–LiAlH₄ systems.

Challenges and Possible Development Strategies

Continuous plans to improve solid-state hydrogen storage materials will undoubtedly demonstrate a further positive effect on the development of hydrogen storage technologies and the widespread use of hydrogen in global energy transitions. Continuous research to identify new hydrogen storage materials indicates that the Mg–Li–Al system is a promising material for the future storage of hydrogen. Although the destabilized system of the Mg–Li–Al system has attracted a lot of attention and many types of research and development were carried out in this field, some problems and challenges still exist in achieving a suitable hydrogen storage material for practical applications. A few possible developmental strategies are listed as follows:

1) The addition of additives has shown considerable promise in improving the Mg–Li–Al system’s performance. It is interesting to investigate the effect of other catalysts/additives to boost the performance of the Mg–Li–Al system and to understand the way catalysts/additives have an effect on improving the hydrogen storage properties of the Mg–Li–Al system.

2) The investigation on the reversible absorbs and desorbs hydrogen of the Mg–Li–Al system under moderate temperature and pressure must be the main target, and significant work is required to find the solution for the release and hydrogen uptake kinetics deteriorated during the cycling process.

3) It is reported that the formation of the Mg₂Al₃ during the rehydrogenation process has a negative effect on the hydrogen capacity and kinetic performance of the Mg–Li–Al system. The formation of Mg₂Al₃ could be avoided by applying a high pressure of hydrogen (> 10 MPa) during the rehydrogenation process. It is necessary to explore the ways of preventing the formation of Mg₂Al₃ without applying a high pressure of hydrogen, such as by using an appropriate additive or catalyst.

4) The hydrogen storage performance of the Mg–Li–Al system has been discovered to be influenced by the molar ratio and milling time. Furthermore, it is critical to investigate the other approaches, such as embedding materials in nanoconfinement, which could improve the hydrogen storage properties of the Mg–Li–Al system.

Therefore, we believe that with continuous effort, the limitations on the development of the Mg–Li–Al system as an ideal hydrogen storage material might be overcome and that the Mg–Li–Al system with favorable kinetics and thermodynamics should be one of the near-term goals.

Conclusion

In this review, it was clear that the transition from the current energy economy to cleaner energy like hydrogen was motivated by environmental and economic factors. Possible current approaches to store hydrogen are in the liquid state, compressed gas state, and solid state. However, due to the large amount of hydrogen that can be stored in a small amount and safety considerations, solid-state hydrogen storage systems are attractive to research. This comprehensive review highlighted the higher desorption temperature and sluggish sorption kinetics in MgH₂, which can be overcome through the destabilization concept (addition of LiAlH₄). Many researchers explored the reaction between the Mg–Li–Al system, including the ratio, the milling time, and the addition of an additive/catalyst to this composite. Interestingly, the doping Mg–Li–Al system with the catalyst can reduce the onset desorption temperature to below 60°C. The intermediate forms of Li_0.92Mg_4.08 and Mg₁₇Al₁₂ were eventually formed in the Mg–Li–Al composites. Cycling measurements show that Li_0.92Mg_4.08 and Mg₁₇Al₁₂ are fully reversible absorbs and desorbs of hydrogen. However, the Mg–Li–Al composites are still in their early development and need more time to prove themselves as viable long-term solutions for solid-state hydrogen storage. Further study, such as on doping with other additives/catalysts, could investigate the different milling times and ratios that should be focused on for the further design of advanced solid-state hydrogen storage materials.

Author Contributions

All authors listed have made a substantial, direct, and intellectual contribution to the work and approved it for publication.

Funding

This work was financially supported by the Golden Goose Research Grant (GGRG) VOT 55190, University Malaysia Terengganu and Casa Armada Sdn. Bhd. VOT 53468.

Conflict of Interest

MG was employed by the company Casa Armada Sdn. Bhd.

The remaining authors declare that the research was conducted in the absence of any commercial or financial relationships that could be construed as a potential conflict of interest.

Publisher’s Note

All claims expressed in this article are solely those of the authors and do not necessarily represent those of their affiliated organizations, or those of the publisher, the editors, and the reviewers. Any product that may be evaluated in this article, or claim that may be made by its manufacturer, is not guaranteed or endorsed by the publisher.

Acknowledgments

The authors would like to acknowledge Universiti Malaysia Terengganu for providing complete facilities to perform this research. SS and MI thank the World Class Professor Program 2021 managed by the Indonesian Ministry of Education, Culture, Research and Technology. N. A. Sazelee and N. A. Ali are grateful for the BUMT and SIPP scholarship provided by UMT.

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