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Effect of Sc substitution on hydrogen storage

properties of TieVeCreMn alloys

Jingbo Zhu a,b, Liqun Ma a,*, Fei Liang b, Limin Wang b,**
a
College of Material Science and Engineering, Nanjing Tech University, Nanjing 210009, China
b
State Key Laboratory of Rare Earth Resource Utilization, Changchun Institute of Applied Chemistry, CAS,
Changchun 13002, China

article info abstract

Article history: The microstructure and hydrogen absorption/desorption properties of (40-x)Tie40Ve10Cr

Received 4 December 2014 e10Mn-xSc (x ¼ 0, 5, 10, 15) were investigated. The result shows that the Sc-free sample has
Received in revised form a V-based solid solution phase with body-center cubic structure (BCC phase), while the Sc-
1 February 2015 contained samples consist of a BCC phase, a C14-type Laves phase, a Sc-based hydride
Accepted 29 March 2015 phase with face-center cubic (FCC) structure (derived from hydrogen decrepitation pro-
Available online 17 April 2015 cess). The hydrogen absorption kinetic process can be described by chemical reaction
mechanism when x ¼ 0, 10, 15 and 3-D diffusion mechanism when x ¼ 5. As the Sc content
Keywords: increases, the hydrogen absorption capacity at 298 K first decreases and then increases,
Hydrogen storage alloy getting the minimum when x ¼ 5. However, the hydrogen desorption capacity and hys-
Sc substitution teresis at 298 K are gradually improved with Sc content increasing.
TieV-Based alloy Copyright © 2015, Hydrogen Energy Publications, LLC. Published by Elsevier Ltd. All rights
Kinetic mechanism reserved.

hydride. To solve the above issues, researchers have been

Introduction making significant efforts for modification work, of which
element substitution has proved to be a simple and effective
As a clean energy source, hydrogen has drawn extensive at- way. Maeland [3] and Akiba, etc [4e7] are respectively the
tentions, expected to be applied in fuel-cell vehicle field. Thus, earliest and most representative reporters on the hydrogen
a safe and effective hydrogen storage method comes to be a properties of TieV-M (M ¼ transition metal) and found that Fe,
key technical issue. Owing to its privilege in compactness and Mn, Co, Cr, Ni are helpful to enhance the reaction rate. Since
lightweight, metal hydrides have become one of the most then, the ternary and quaternary TieV-based samples came to
attractive and potential hydrogen storage materials. Among be reported extensively, of which TieV-M (M ¼ Cr, Mo) [8e11]
them, TieV-based hydrogen storage alloys have a larger and TieVeCr-M (M ¼ Mn, Fe, Zr) [12e16] samples exhibit a
hydrogen storage capacity than the conventional AB5 and AB2 most favorable hydrogen storage properties.
alloys [1] and show high reactivity with hydrogen at low However, the Sc element, which is adjacent to the Ti
temperature [2]. However, there also exist shortcomings with element in the periodic table, has seldom been reported to
TieV-based alloys, such as: limited gravimetric storage den- substitute other elements in TieV-based samples. As we
sity and high temperature to dehydrogenate the mono- know, the Sc element has a smaller relative atomic mass,

* Corresponding author. Tel.: þ86 025 83587243; fax: þ86 025 83240205.
** Corresponding author. Tel./fax: þ86 0431 85262447.
E-mail addresses: [email protected] (L. Ma), [email protected] (L. Wang).
http://dx.doi.org/10.1016/j.ijhydene.2015.03.149
0360-3199/Copyright © 2015, Hydrogen Energy Publications, LLC. Published by Elsevier Ltd. All rights reserved.
 i n t e r n a t i o n a l j o u r n a l o f h y d r o g e n e n e r g y 4 0 ( 2 0 1 5 ) 6 8 6 0 e6 8 6 5 6861

larger affinity with H and larger atomic radius than Ti, which
indicates that Sc substitution for Ti in TieV-based samples
may favor increasing the theoretical and effective hydrogen
storage capacity. Thus, we conducted a systematic research
on the microstructure, hydrogen storage properties of the Sc-
substituted TieVeCreMn samples. Besides, the Sc-
substituted TieVeCreMn system was reported for the first
time.

Experimental methods

The alloys of (40-x)Tie40Ve10Mne10Cr-xSc (weight percent-

age, x ¼ 0, 5, 10, 15) were prepared by arc melting method and
re-melted for several times to obtain a higher homogeneity,
with respectively denoted as S0, S5, S10, S15. The purity of the
starting element metals is: V > 99.9%, Ti > 99.7%, Cr > 99.9%,
Fig. 1 e XRD patterns of (40¡x)Tie40Ve10Cre10Mn-xSc
Mn > 99.95%, Sc > 99.9%. The obtained as-cast alloys in button
(x ¼ 0, 5, 10, 15) samples.
shape were mechanically crushed to small pieces and further
pulverized by hydrogen decrepitation process (TieV-based
alloys is too hard to be crushed by mechanical force). And all
the hydride powders were further dehydrogenated at 673 K for
5 h. the following hydriding/dehydriding tests is based on the
The kinetic and pressure-composition-isotherm (PCI) tests dehydrogenated powders but not the original alloys.
were conducted in a Sieverts-type apparatus. The purity of the As we can see, the diffraction peaks of BCC phase broaden
hydrogen used is 99.999%. In the kinetic tests, the hydrogen severely, which should be attributed to the internal stress and
absorption process was conducted under the initial pressure peak overlap of two BCC phases, with the latter confirmed by
of 7 MPa. Then, the reactor was evacuated for 5 h at 673 K for the following section. When x increases from 5 to 15, the
the next hydrogen absorption process. In the PCI tests, the abundance of the BCC phase and Laves phase decreases, but
hydrogen absorption/desorption capacity is defined as the the abundance of the ScH2 phase increases. The detail relative
amount of hydrogen absorbed/desorbed when the hydrogen phase abundance is listed in Table 1, which is manually
equilibrium pressure is 4 MPa/from 4 MPa to 0.01 MPa (cut-off calculated by means of reference intensity ratios (i.e., RIR, also
pressure). called I/Ic in the PDF database) assisted by software Jade 6.
The phase composition and crystal structure of the pow- Although Jade 6 provide automatic calculation on phase
ders before and after absorbing hydrogen were determined by abundance, we find it deviates a lot when it calculates the area
X-ray diffraction analysis (XRD) in a thermo ARL X’TRA of the overlapped peak (all of the peaks of BCC phase is
diffractometer with Cu Ka radiation. The microstructures overlapped). Thus, the area of the strongest peaks of each
were observed under a JSM-5610LV scanning electron micro- phase was calculated manually with embedded tools in Jade 6,
scopy (SEM) with the acceleration voltage of 20 KV and the so the range of deviation was not given.
chemical compositions were determined by energy dispersive Moreover, as the Sc content increases, all the peaks of BCC
spectroscopy (EDS). phase first shift to the right and then to the left, with the one of
S5 reaching the rightmost and the one of S0 in the left of S15. It
indicates the lattice parameter of BCC phase in Sc-free sample
Results and discussion is larger than in Sc-contained samples and it increases grad-
ually when x increases from 5 to 15 (getting the minimum
Phases and microstructures when x ¼ 5).
To study the structure transformation after hydrogen ab-
The XRD patterns of (40-x)Tie40Ve10Mne10Cr-xSc (x ¼ 0, 5, sorption at 273 K, we conducted an XRD analysis on the hy-
10, 15) samples (dehydrogenated powders) are shown in Fig. 1. drides. As we can see in Fig. 2, the BCC phase transforms to
The Sc-free sample has a V-based solid solution phase with two different FCC phases respectively denoted as FCC-1 and
BCC structure (BCC phase), while Sc-contained samples
consist of a BCC phase, a C14-type Laves phase and a Sc-based
hydride phase with FCC structure (ScH2 phase). The formation
of ScH2 phase is derived from hydrogen decrepitation process Table 1 e Relative phase abundance in (40¡x)
Tie40Ve10Cre10Mn-xSc (x ¼ 0, 5, 10, 15) samples.
for pulverization and the temperature (673 K) of the following
dehydriding process is not enough to dehydrogenate ScH2, so BCC (wt. %) ScH2 (wt. %) Laves (wt. %)
it remains. That is to say, this XRD patterns does not represent x ¼ 0 100 0 0
the original alloys but the dehydrogenated powders. However, x ¼ 5 90.1 4.5 5.4
this XRD patterns are more meaningful and instructive for the x ¼ 10 88.5 7.2 4.3
x ¼ 15 88.0 9.8 2.2
study of hydrogen storage properties, as every initial state of
6862 i n t e r n a t i o n a l j o u r n a l o f h y d r o g e n e n e r g y 4 0 ( 2 0 1 5 ) 6 8 6 0 e6 8 6 5

Table 2 e The chemical composition of BCC phases in

(40¡x)Tie40Ve10Cre10Mn-xSc (x ¼ 0, 5, 10, 15).
x ¼ 0 (wt.%) x ¼ 5 (wt.%) x ¼ 10 (wt.%) x ¼ 15 (wt.%)
Ti 39.97 34.43 31.02 27.26
V 39.95 42.35 42.44 43.15
Cr 9.92 10.02 10.18 10.34
Mn 10.16 10.03 9.71 8.73
Sc e 3.17 6.65 10.52

controlled BCC phase, considering the phase abundance of

Laves phase is far less than the BCC phase.
Fig. 3 shows the SEM micrographs of (40-x)
Tie40Ve10Cre10Mn-xSc (x ¼ 0, 5, 10, 15) samples (original
alloys). It can be seen that there is no obvious second phase
appearing in the Sc-free sample, while there exists a visible
Fig. 2 e XRD patterns of (40¡x)Tie40Ve10Cre10Mn-xSc but minor second phase in Sc-contained samples (hereby, the
(x ¼ 0, 5, 10, 15) after hydrogen absorption at 273 K. second phase represents all the phases except BCC phase).
The EDS analysis on the chemical composition of the BCC
phase shows: as the Sc content increases, the percentage of
Sc, V and Cr element increases, while the percentage of Ti and
FCC-2 (deformed FCC-2 for S5) after saturated hydrogen ab- Mn element decreases. The detail chemical composition of
sorption at 273 K, which confirms that the BCC phase is BCC phase is listed in Table 2. In addition to it, the changing
actually composed by two BCC phases with similar peaks regulation of lattice parameter can be explained from the view
(namely pseudo-single BCC phase). Moreover, the peaks of of chemical composition: for the Sc-contained samples, the
ScH2 phase keep unchanged after the hydrogen absorption amount of the Sc element into BCC phase is much less than
process, which indicates it does not absorb hydrogen in this the amount of the Ti element out of BCC phase when
hydriding process; the peaks of the Laves phase changes a lot, compared with the Sc-free sample, thus the lattice parameter
which means it absorbs hydrogen in this process, but we of BCC phase in Sc-free sample is larger than in Sc-contained
cannot figure it out clearly owing to the peaks’ complicacy and samples; When x increases from 5 to 15, the amount of the Sc
low mass fraction. In the following sections, we assume that element into BCC phase is more than the amount of the Ti
the hydrogen absorption/desorption capacity is mainly element out of BCC phase when compared with the former Sc-

Fig. 3 e SEM images of (40¡x)Tie40Ve10Cre10Mn-xSc: (a) x ¼ 0; (b) x ¼ 5; (c) x ¼ 10; (d) x ¼ 15.
 i n t e r n a t i o n a l j o u r n a l o f h y d r o g e n e n e r g y 4 0 ( 2 0 1 5 ) 6 8 6 0 e6 8 6 5 6863

Fig. 4 e Initial absorption kinetic curves of (40¡x) Fig. 5 e Optimal linear fitting of reaction mechanism
Tie40Ve10Cre10Mn-xSc (x ¼ 0, 5, 10, 15) at 273 K. equation with t: (a) x ¼ 0, 15; (b) x ¼ 5, 10.

contained sample, thus the lattice parameter of BCC phase in between P and t, we conducted the linear fitting of reaction
Sc-contained samples increases gradually. mechanism equations with t and held the equation with
maximum coefficient of determination (R2) as the kinetic
mechanism equation. The linear fitting results are shown in
Kinetic properties
Fig. 5.
R2 gets the maximum when gðaÞ ¼ ð1  aÞ1=2 for S0 and
Fig. 4 shows the initial hydrogen absorption kinetic curves of
S15, respectively 0.9992 and 0.9993. This equation belongs to
(40-x)Tie40Ve10Cre10Mn-xSc (x ¼ 0, 5, 10, 15) at 273 K. It was
chemical reaction mechanism. Moreover, the value of k is
found that the initial hydrogen absorption process could reach
respectively 2.377 and 2.113, indicating the reaction rate of the
the maximum hydrogen absorption capacity, indicating the
former is a little faster than the latter (only when kinetic
samples exhibit favorable activation properties. As it is shown
mechanism equations are the same, the value of k is
in Fig. 4, the hydrogen absorption capacity of Sc-free sample is
comparable).
larger than the Sc-contained samples and it increases gradu-
R2 gets the maximum when gðaÞ ¼ ½ð1  aÞ1=3  12 for S5
ally when x increases from 5 to 15, namely 3.587wt.%,
and gðaÞ ¼ ð1  aÞ2 for S10, respectively 0.9989 and 0.9985.
2.398wt.%, 2.903wt.%, 3.208wt.%. Moreover, it only takes 3.8,
These equations respectively belong to 3-D diffusion mecha-
4.3 min for S0 and S15, but 31.5, 42.1 min for S5 and S10 to
nism (S5) and chemical reaction mechanism (S10). Moreover,
reach the saturation of hydrogen absorption. The obvious re-
the value of k is respectively 0.220 and 15.605.
action rate's difference between S0, S15 and S5, S10 could be
In terms of S5, the lattice parameter of BCC phase is the
attributed to their different kinetic mechanisms which were
minimum (unfavorable for H atom's diffusion) and the
further studied as follows.
The gasesolid kinetic reaction function is [17]:

da
¼ kfðaÞ (1)
dt
Thus, we get the integration form of Eq. (1)
Z Z
da
¼ k$dt ¼ k$t (2)
fðaÞ

wherein a ¼ (PsP)/(PsPe), k is a reaction rate constant. f(a)

represents a reaction mechanism. Ps and Pe are the initial and
the equilibrium hydrogen pressure, respectively. P is the
R da
hydrogen pressure at time t. fðaÞ is defined as g(a), so Eq. (2)
becomes:

gðaÞ ¼ k$t (3)

According to the above description, if the reaction mech-

anism represented by g(a) can describe the kinetic process,
g(a) has a linear relationship with time t. Based on the reaction Fig. 6 e Absorption/desorption PCI curves of (40¡x)
mechanism equations [18] and the known relationship Tie40Ve10Cre10Mn-xSc (x ¼ 0, 5, 10, 15) at 298 K.
6864 i n t e r n a t i o n a l j o u r n a l o f h y d r o g e n e n e r g y 4 0 ( 2 0 1 5 ) 6 8 6 0 e6 8 6 5

abundance of Laves phase is the maximum (Laves phase is capacity at 298 K showing consistent changing regulation
benefit for chemical reaction), which explains the kinetic when x increases from 5 to 15.
mechanism of S5 transforms to 3-D diffusion mechanism. As we can see in Fig. 6, the plateaus at 298 K cannot be
figured out obviously, which should be attributed to the
inhomogeneous chemical composition [19] and the low
PCI properties plateau pressure. Moreover, the hysteresis of absorption/
desorption PCI curves is improved with the Sc content
Fig. 6 shows the hydrogen absorption/desorption PCI curves of increasing. T. Kabutomori [20] had ever reported: because of
(40-x)Tie40Ve10Cre10Mn-xSc (x ¼ 0, 5, 10, 15) at 298 K. The good symmetry of the BCC structure, dislocations can be
hydrogen absorption capacity of Sc-free sample is larger than easily produced by deformation of the crystal during hydrogen
the Sc-contained samples and it increases gradually when x absorption/desorption process, which contributes to the
increases from 5 to 15, which is in accord with the changing hysteresis of absorption/desorption PCI curves. That is to say,
regulation of hydrogen absorption capacity at 273 K. However, Sc element may contribute to suppressing the production of
the hydrogen desorption capacity gradually increases when dislocations during hydrogen absorption/desorption process,
the Sc content increases. The detail hydrogen absorption/ thus improving the hysteresis of absorption/desorption PCI
desorption capacity at 298 K is listed in Table 3. curves.
According to Cho S W's report [7], hydrogen absorption/ As we can get from the van't Hoff equation, the variation of
desorption plateau pressure generally shows a converse temperature will not affect the changing regulation of plateau
changing regularity with lattice parameter. As we mentioned pressure (hereby, DSq is assumed as a constant, generally
before, the lattice parameter of BCC phase in Sc-free sample 130 J/(mol k)). Thus, to verify the changing regulation of
is larger than in Sc-contained samples and it increases plateau pressure at 298 K and to study the desorption prop-
gradually when x increases from 5 to 15. Thus, we can erties at higher temperature, we conducted the hydrogen
deduce: the hydrogen absorption/desorption plateau pres- desorption PCI testing at 373 K (after saturated hydrogen ab-
sure of Sc-free sample is smaller than Sc-contained samples sorption at 298 K).
and it decreases gradually when x increases from 5 to 15. As it is shown in Fig. 7, the hydrogen desorption plateau
This changing regulation of plateau pressure is also pressure of Sc-free sample is smaller than Sc-contained
confirmed by the next section of hydrogen desorption at samples and it decreases gradually when x increases from 5
373 K. Further, hydrogen absorption capacity generally shows to 15. Thereby, it confirms the changing regulation of plateau
a converse changing regulation with hydrogen absorption pressure we deduced at 298 K. As it is shown in Table 3, as the
plateau pressure, thus the hydrogen absorption capacity of Sc content increases, the changing regulation of hydrogen
Sc-free sample is larger than Sc-contained samples and it desorption capacity at 373 K is consistent with the changing
increases gradually when x increases from 5 to 15, showing regulation of hydrogen absorption capacity at 298 K. This
the consistent changing regulation with lattice parameter of phenomenon can be explained as follows: the cut-off pressure
BCC phase. is lower than the hydrogen desorption plateau pressure of all
Hydrogen desorption capacity is generally related to the samples at 373 K, thus hydrogen desorption capacity is
hydrogen desorption plateau pressure, cut-off pressure and mainly controlled by hydrogen absorption capacity, resulting
hydrogen absorption capacity. And the reason why S0 get the in hydrogen desorption capacity at 373 K and hydrogen ab-
minimum hydrogen desorption capacity should be explained sorption capacity at 298 K showing consistent changing
as follows: the cut-off pressure is higher than the hydrogen regulation.
desorption plateau pressure of S0 (whose plateau pressure is
the minimum), suppressing the hydrogen desorption reac-
tion, thus getting the minimum hydrogen desorption capac-
ity. Moreover, the reason why the hydrogen desorption
capacity increases when x increases from 5 to 15 should be
explained as follows: the cut-off pressure is lower than the
hydrogen desorption plateau pressure of Sc-contained sam-
ples, thus hydrogen desorption capacity is mainly controlled
by hydrogen absorption capacity, resulting in hydrogen
desorption capacity at 298 K and hydrogen absorption

Table 3 e Hydrogen absorption/desorption capacity (HAC/

HDC) of (40¡x)Tie40Ve10Cre10Mn-xSc (x ¼ 0, 5, 10, 15)
at 298 K, 373 K.
HAC (298 K) HDC (298 K) HDC (373 K)
x ¼ 0 3.577 wt.% 0.111 wt.% 1.698 wt.%
x ¼ 5 2.341 wt.% 0.294 wt.% 0.701 wt.%
x ¼ 10 2.883 wt.% 0.425 wt.% 1.215 wt.% Fig. 7 e Desorption PCI curves of (40¡x)
x ¼ 15 3.143 wt.% 0.442 wt.% 1.381 wt.%
Tie40Ve10Cre10Mn-xSc (x ¼ 0, 5, 10, 15) at 373 K.
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