Remarkable catalysis of spinel ferrite XFe2O4 (X = Ni, Co, Mn, Cu, Zn) nanoparticles on the dehydrogenation properties of LiAlH4: An experimental and theoretical study

doi:10.1016/j.jmst.2021.08.088

Abstract

Abstract:

Safe, compact, lightweight and cost-effective hydrogen storage is one of the main challenges that need to be addressed to effectively deploy the hydrogen economy. LiAlH₄, as a solid-state hydrogen storage material, presents several advantages such as high hydrogen storage capacity, low price and abundant sources. Unfortunately, neither thermodynamic nor kinetic properties of dehydrogenation for LiAlH₄ can fulfill the requirements of practical application. Thus, a series of spinel ferrite nanoparticles such as XFe₂O₄ (X = Ni, Co, Mn, Cu, Zn, Fe) were prepared by using the modified thermal decomposition method, and then doped into LiAlH₄ by using ball milling. Our results show that LiAlH₄ doped with 7 wt% NiFe₂O₄ starts to release hydrogen at 69.1 °C, and the total amount of hydrogen released is 7.29 wt% before 300 °C. The activation energies of the two-step hydrogen release reactions of LiAlH₄ doped with 7 wt% NiFe₂O₄ are 42.32 kJ mol^-1 and 71.42 kJ mol^-1, which are 59.0% and 63.6% lower than those of as-received LiAlH₄, respectively. Combining the density functional theory (DFT) calculations, we reveal that both the presence of NiFe₂O₄ and in-situ formed Al₄Ni₃ in ball-milling decrease the desorption energy barrier of Al-H bonding in LiAlH₄ and accelerate the breakdown of Al-H bonding through the interfacial charge transfer and the dehybridization of the Al-H cluster. Thus, the experimental and theoretical results open a new avenue toward designing high effective catalysts applied to LiAlH₄ as a candidate for hydrogen storage.

Key words: Hydrogen storage, Lithium aluminum, Spinel ferrite nanoparticles

Sheng Wei, Jiaxi Liu, Yongpeng Xia, Huanzhi Zhang, Riguang Cheng, Lixian Sun, Fen Xu, Pengru Huang, Federico Rosei, Aleskey A. Pimerzin, Hans Jüergen Seifert, Hongge Pan. Remarkable catalysis of spinel ferrite XFe₂O₄ (X = Ni, Co, Mn, Cu, Zn) nanoparticles on the dehydrogenation properties of LiAlH₄: An experimental and theoretical study[J]. J. Mater. Sci. Technol., 2022, 111: 189-203.

Figures/Tables 14

Fig. 1. Schematic illustration of XFe2O4 (X = Ni, Co, Mn, Cu, Zn, Fe).

Fig. 2. XRD patterns (a), Raman spectra (b) and FT-IR spectra (c) of XFe2O4 (X = Ni, Co, Mn, Cu, Zn, Fe).

Table 1. Raman study of XFe2O4 (X = Ni, Co, Mn, Cu, Zn, Fe) nanoparticles.

Sample	Peak positions (cm^-1)
Sample	T_2g (1) (F_2g (1))	E_g	T_2g (2) (F_2g (2))	T_2g (3) (F_2g (3))	A_1g
NiFe₂O₄	206	280	463	542	674
CoFe₂O₄	188	284	456	597	672
MnFe₂O₄	213	268	376	487	583
CuFe₂O₄	220	285	400	493	604
ZnFe₂O₄	215	278	389	484	590
Fe₃O₄	215	277	391	491	592

Fig. 3. XPS spectra (a-f) of XFe2O4 (X = Ni, Co, Mn, Cu, Zn, Fe).

Table 2. XPS study of XFe2O4 (X = Ni, Co, Mn, Cu, Zn, Fe) nanoparticles.

Sample	ions	Binding Energy (eV)
Sample	ions	2p_1/2 (tetrahedral sites)	2p_1/2 (octahedral sites)	2p_3/2 (tetrahedral sites)	2p_3/2 (octahedral sites)	Satellite peak
NiFe₂O₄	Ni²⁺	877.1	872.3	855.1	853.4	881.2 860.9
NiFe₂O₄	Fe³⁺	726.6	723.7	713.2	710.4	732.5 718.5
CoFe₂O₄	Co²⁺	795.8	792.9	781.3	778.0	801.3 786.6
CoFe₂O₄	Fe³⁺	726.2	722.3	711.2	708.6	732.3 717.1
MnFe₂O₄	Mn²⁺	653.4	652.1	642.2	640.6	659.4 645.9
MnFe₂O₄	Fe³⁺	727.1	724.0	712.8	710.3	732.1 719.1
CuFe₂O₄	Cu²⁺	955.3	953.6	935.1	933.3	963.1 959.6 943.8 940.5
CuFe₂O₄	Fe³⁺	727.4	724.0	713.4	710.5	733.5 719.0
ZnFe₂O₄	Zn²⁺	1044.8		1021.6
ZnFe₂O₄	Fe³⁺	727.1	724.0	712.8	710.3	732.1 719.1
Fe₃O₄	Fe²⁺		723.4		709.5	732.3 716.4
Fe₃O₄	Fe³⁺	728.1	725.1	712.8	710.9	735.4 719.3

Fig. 4. SEM images (a-f) of XFe2O4 (X = Ni, Co, Mn, Cu, Zn, Fe).

Fig. 5. TEM images (a) and EDS mapping (b-e) of NiFe2O4.

Fig. 6. TG patterns (a, b) of the LiAlH4 (As-received), LiAlH4 (Ball milling), LiAlH4+7 wt% XFe2O4 (X = Ni, Co, Mn, Cu, Zn, Fe), LiAlH4+x wt% NiFe2O4 (x = 1, 3, 7, 10), DSC thermograms (c, d) of the LiAlH4 and LiAlH4+7 wt% NiFe2O4, and the corresponding Kissinger's plots (e, f), Isothermal dehydrogenation curves (g) of the LiAlH4 (As-received) and LiAlH4+7 wt% NiFe2O4, Isothermal rehydrogenation curves (h) of the LiAlH4 (As-received) and LiAlH4+7 wt% NiFe2O4.

Table 3. A comparison of onset desorption temperatures, activation energies and H2 desorption capacity of some metal oxides doped-LiAlH4 systems.

System	Onset desorption temperature ( °C)		Activation energy (kJ mol^-1)		H₂ desorption capacity (wt%)	Refs.
System	Step 1	Step 2	Step 1	Step 2	H₂ desorption capacity (wt%)	Refs.
LiAlH₄-Fe₂O₃	80.0	145.0	84.00	96.00	7.60	[44]
LiAlH₄-LaFeO₃	109.0	153.0	73.00	89.00	6.40	[45]
LiAlH₄-Li₂TiO₃	75.0	137.0	72.60	71.40	∼5.10	[46]
LiAlH₄-BaFe₁₂O₁₉	95.0	∼160.0	71.00	90.00	∼6.00	[47]
LiAlH_4-MgFe₂O₄	95.0	145.0	73.00	97.00	6.50	[19]
LiAlH₄-NiCo₂O₄@Rgo	62.7	∼150.0	77.56	91.45	6.28	[48]
LiAlH₄-NiFe₂O₄	69.1	129.4	42.32	71.42	7.29	This work

Fig. 7. XRD patterns (a-d) and FT-IR (e-h) of the LiAlH4 (As-received), LiAlH4 (Ball milling), LiAlH4+x wt% NiFe2O4 (x = 1, 3, 7, 10), LiAlH4+7 wt% NiFe2O4 after isothermal dehydrogenation (90 °C, 120 °C, 150 °C, 180 °C), LiAlH4+7 wt% XFe2O4 (X = Ni, Co, Mn, Cu, Zn, Fe), LiAlH4+7 wt% NiFe2O4 before and after isothermal rehydrogenation.

Fig. 8. SEM images of the (a) as-received LiAlH4, (b) ball milled LiAlH4, LiAlH4+7 wt% NiFe2O4 before (c, d) and after (i-l) dehydrogenation (90 °C, 120 °C, 150 °C, 180 °C), EDS mapping of the LiAlH4+7 wt% NiFe2O4 at different states: (e-h) after ball-milling.

Fig. 9. TEM images (a) and EDS mapping (b-f) of LiAlH4+7 wt% NiFe2O4.

Table 4. Atomic charge, bond length, and adsorption energy for LiAlH4, LiAlH4@NiFe2O4 and LiAlH4@Al4Ni3.

Empty Cell	LiAlH₄	LiAlH₄@NiFe₂O₄	LiAlH₄@Al₄Ni₃
Atom	Atomic charge (e^-)
Al	-2.11	-2.22	-2.06
H₁	0.53	0.72	0.76
H₂	0.53	0.31	0.85
H₃	0.53	0.31	0.42
H₄	0.53	0.57	0.67
Bond	Bond length(Å)
Al-H₁	1.65	1.63	1.66
Al-H₂	1.65	1.87	1.76
Al-H₃	1.65	1.88	1.86
Al-H₄	1.65	1.61	1.59
Adsorption energy (eV)		-4.15	-3.93

Fig. 10. Adsorption structures and charge density difference with an isovalue of 0.004 e Å-3 for LiAlH4 clusters on NiFe2O4 (a) and Al4Ni3 (b). Density of states (DOS) for LiAlH4, LiAlH4@NiFe2O4, and LiAlH4@Al4Ni3. The dashed line indicates the Fermi level.

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Remarkable catalysis of spinel ferrite XFe₂O₄ (X = Ni, Co, Mn, Cu, Zn) nanoparticles on the dehydrogenation properties of LiAlH₄: An experimental and theoretical study

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