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Experimental study of metal hydride-basedhydrogen storage tank at constant supply pressure
A. Souahlia, H. Dhaou*, S. Mellouli, F. Askri, A. Jemni, S. Ben Nasrallah
Laboratoire d’Etudes des Systemes Thermiques et Energetique, Rue Ibn Eljazzar,
Ecole Nationale d’Ingenieurs de Monastir, University of Monastir, Monastir 5019, Tunisia
a r t i c l e i n f o
Article history:
Received 11 December 2013
Received in revised form
14 February 2014
Accepted 19 February 2014
Available online xxx
Keywords:
Hydrogen
Metal hydride
Supply pressure
Cooling temperature
* Corresponding author. Tel./fax: þ216 73501E-mail address: [email protected]
Please cite this article in press as: Souaconstant supply pressure, International J
http://dx.doi.org/10.1016/j.ijhydene.2014.02.10360-3199/Copyright ª 2014, Hydrogen Ener
a b s t r a c t
Metal hydride-based hydrogen storage tank is tested using 1 kg of AB5 alloy, namely LaNi5.
The hydrogen tank is of annular cylindrical with inner and outer heat exchangers. The
inner one is a finned spiral heat exchanger and the outer one is a conventional jacket.
Performance (storage capacity and storage time) studies are carried out by varying the
supply pressure and the cooling temperature of the hydride bed. At any given cooling
temperature, hydrogen storage rate is found to increase with supply pressure. Cooling
temperature is found to have a significant effect on hydrogen storage capacity at lower
supply pressures.
Copyright ª 2014, Hydrogen Energy Publications, LLC. Published by Elsevier Ltd. All rights
reserved.
Introduction
Since environmental pollution proceeds from the large
amount of fossil fuel energy consumption, new clean energy
sources have been developed as alternatives. In addition,
hydrogen is one of the most clean energy carriers. However,
hydrogen storage and transportation become problematic.
Among different hydrogen storage means (compressed gas,
liquid hydrogen) reversiblemetal hydrides are considered as a
safe and volume efficient hydrogen storage medium under
low pressure conditions. Metal hydrides are generally used as
packed beds. Themetal hydride formation is closely related to
the hydrogen pressure and bed temperature. Also, hydrogen
absorption/desorption is an exothermic/endothermic reac-
tion. Those phenomena and many others are complicatedly
coupled together, so it requires a lot of experimental and
597.(H. Dhaou).
hlia A, et al., Experimenournal of Hydrogen Ene
21gy Publications, LLC. Publ
theoretical works to optimize hydrogen metal hydride
reservoir.
Suda and Kobayashi [1] performed a series of experimental
studies on the hydriding and dehydriding kinetics for several
alloys and their binary mixtures under isothermal conditions.
They concluded that the mixing of hydriding materials offers
several technical advantages such as controlling the reaction
rate and the kinetic properties by varying the mixing ratio.
Miyamoto et al. [2] investigated the reaction kinetics for
LaNi5eH2 system under constant hydrogen pressure, and
proposed the chemical reaction rate models. Goodell and
Rudman [3] measured the intrinsic reaction rates for the
hydriding and dehydriding of LaNi5 over a wide range of
pressures in the temperature range 60e65 �C. Approximately
isothermal conditions were maintained by a thermal ballast
technique. Later numerical models were developed for
assessing the transient heat and mass transfer within metal
tal study of metal hydride-based hydrogen storage tank atrgy (2014), http://dx.doi.org/10.1016/j.ijhydene.2014.02.121
ished by Elsevier Ltd. All rights reserved.
Fig. 1 e Schematic of the hydride tank.
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 en e r g y x x x ( 2 0 1 4 ) 1e82
hydride beds [4e7]. It was found that the heat transfer plays a
determining factor in enhancing the performance of storage
tanks. For the sake of simplicity, these models neglected the
convective effects of hydrogen gas on the heat and mass
transfer, which however may be influential at high pressure
cases.
From previous literature, the chemical reactions in metal
beds may be simplified as a two-dimensional problem. Jemni
and Ben Nasrallah developed two-dimensional heat and
mass transfer models for hydrogen adsorption and desorp-
tion respectively [8,9]. The hydrogen flow motion within the
hydride beds was described by Darcy’s law. Their results
show that the difference between the solid and hydrogen
temperatures is negligible, except for some limited areas
close to the gas outlet and tank wall. So the local thermal
equilibrium hypothesis can be used. In a subsequent study,
Ben Nasrallah and Jemni [10] further tested the hypotheses
that were usually adopted in the analysis of heat and mass
transfer in a metal hydride tank. They reached the conclu-
sion that for an LaNi5eH2 reactor, (i) solid and gas tempera-
tures can be treated as the same, (ii) the convection term is
negligible, and (iii) the effect of hydrogen concentration on
the equilibrium pressure variation is negligible in the ab-
sorption case, But in the desorption case this effect cannot be
neglected in the determination of the temperature distribu-
tion in the reactor. The simplified numerical simulations
were later compared with experiments and a good agreement
is obtained [11,12].
Recently, Tange et al. [13] examined the feasibility of an on-
site energy storage system using a tank packed with 50 kg of
hydride metal, and discuss the energy efficiency of the sys-
tem. This tank stores hydrogen at night and supply a fuel cells
to generate power during the day. The system also utilizes the
endothermic hydrogen desorption process for air
Please cite this article in press as: Souahlia A, et al., Experimenconstant supply pressure, International Journal of Hydrogen Ene
conditioning. D’Orazio et al. [14] analyzed and reported the
dynamic behavior of a metal hydride tank to propose a
method to design a multi-tank storage system. The hydride
tanks design and the heat flow are the key parameters for the
optimization of the system working condition. Nyamsi et al.
[15] conducted an analytical and numerical study to optimize
a finned tube heat exchanger considering both enhanced heat
transfer and metal hydride tank volume efficiency. It was
shown that the fin dimensions, the cooling tube diameter and
the fin length are the key parameters to reduce the thermal
resistance of the heat exchanger. The results showed that the
decreasing of the thermal resistance of 13% leads to a
decreasing in charging time of 42%. Corgnale et al. [16]
developed a scoping tool, referred to as the Acceptability En-
velope, to identify the range of chemical, physical and
geometrical parameters that allow a coupled media and
hydrogen storage system to meet technical targets. Nam et al.
[17] developed a three-dimensional model to study the
hydrogen absorption reaction, heat and mass transport phe-
nomena in metal hydride hydrogen storage tank. The simu-
lation results demonstrate that the use of higher hydrogen
supply pressure leads to not only rapid hydrogen charging
performance but also a reduction in the cooling burden of the
tank.
We studied, in previous work [18,19], the dynamic behavior
of several metal hydride-based hydrogen storage tanks using
a Sievert-type apparatus. We noticed that the reference vol-
ume variation influences the stored amount of hydrogen and
the storage time. In order to have consistentmeasurements of
a tank performances (storage time and storage capacity), the
reference volume influence should be excluded. The solution
would be to supply the tank with a constant hydrogen pres-
sure. In this paper, a test bench was built to implement this
solution. Also, a modified version of the metal hydride tank
tal study of metal hydride-based hydrogen storage tank atrgy (2014), http://dx.doi.org/10.1016/j.ijhydene.2014.02.121
i n t e rn a t i o n a l j o u rn a l o f h y d r o g e n en e r g y x x x ( 2 0 1 4 ) 1e8 3
studied by H. Dhaou et al. [18] was designed and its perfor-
mances were evaluated for various dynamic operating con-
ditions (hydrogen supply pressures, cooling temperature).
Experimental setup
The metal hydride tank considered in this paper is of annular
cylindrical configuration (Fig. 1). One kilogram (1 kg) of LaNi5alloy is packed in the inner volume of the tank. The purities of
the lanthanum and nickel were 99.80% and 99.97%, respec-
tively. The average particle size of the alloy was approxi-
mately 50 mm. Heat transfer fluid (water) flows through two
heat exchangers. The first is a finned spiral heat exchanger
immersed in the packed alloy. It consists of a stainless steel
tube (5 mm inner diameters and 1 mm thickness) bent into a
circular helix of 50 mm diameter and 11 turns with a pitch of
7 mm. A copper fin was inserted between each pair of turns
(Fig. 2). The second heat exchanger is implemented by
mounting a sealed stainless steel cylindrical jacket over the
tank, creating an annular space within which the heat trans-
fer fluid flows. The tank is made of a seamless stainless steel
(316-L). The upper end of the tank is flanged with the brazed
assembly of three-grounded metal-sheathed “K” type ther-
mocouples (sensitivity 0.1 �C) at different positions
((r ¼ 10 mm, z ¼ 25 mm), (r ¼ 30 mm, z ¼ 10 mm) and
(r ¼ 30 mm, z ¼ 20 mm)). Other instrumentation and sensors
are shown in Fig. 3. Piezoresistive-type pressure transducers
of range 0e100 bar (sensitivity 0.01 bar) are used formeasuring
the pressure inside the tank (P1) and the supply pressure (P2). A
hydrogen-calibrated rotameter (sensitivity 0.1 L/min) is used
for measuring the hydrogen flow rate and temperature of the
hydrogen gas. High-pressure ball valves are used in the gas
lines for controlling/diverting the gas flow. A vacuum pump is
used to evacuate the tank before hydrogen storage experi-
ments. A thermostatic water bath is used for supplying hot
and cold water (0e80 �C, accuracy � 0.1 �C) at flow rates
ranging from 3 to 13 g/s. A data logger is used to record
Fig. 2 e Schematic of the finned spiral heat exchanger.
Please cite this article in press as: Souahlia A, et al., Experimenconstant supply pressure, International Journal of Hydrogen Ene
temperature and pressure readings for further processing and
interpretation. Additional efforts were made to guarantee
accurate and precise measurement of various parameters
involved in the process of hydrogen storage. For example,
mechanical devices that generate vibrations (pump, cooling
device, devices equipped with fans.) are isolated from the
rest of the experimental setup, thermocouples, pressure
transducers and rotameter are calibrated before performing
the series of measurements presented in this paper.
To be able to reversibly store hydrogen, the LaNi5 alloy
must be activated. Activation consists in executing repeated
absorption/desorption cycles (25 cycles) until the maximum
hydrogen storage capacity is reached (1.4 w%). Absorption is
performed at 10 bar and 25 �C till the hydrogen flow is no
longer detected. Desorption reaction is performed at low
pressure and 70 �C till the pressure inside the tank becomes
constant and equal to 0.01 bar.
For each experiment, efforts are made to have the same
initial condition of the tank. First, the tank is evacuated down
to 0.01 bar. Then, the hydride bed is cooled by circulating the
cold fluid from bath B1. Meanwhile, the hydrogen supply
pressure and the fluid temperature of bath B2 are set. Later,
valve V1 is opened. The hydrogen storage is continued till the
hydrogen flow is no longer detected. During the storage pro-
cess, pressures, temperatures and hydrogen flow rate, are
recorded for every 1 s.
Results and discussion
In practice, a metal hydride tank would not be packed full of
metal hydrides but contain some void space called expansion
volume because metal lattices expand during absorption [20].
Consequently, the inner volume of a tank may be split into
two: a reactional volume corresponding to the volume occu-
pied by the totality of the hydride particles and a free volume
including the expansion volume and the hydride pores vol-
ume. In case of the studied tank, 85% of the inner volume is a
reactional volume, 12% is a free volume and not forgetting the
volume occupied by the internal heat exchanger (3%).
The terminology used in this paper distinguishes between
hydrogen absorption and hydrogen storage. The term “ab-
sorption” limits the discussion to the phenomenon occurring
in the reactional volume.
Figs. 4e6 show time history of hydrogen storage rate, hy-
dride bed temperature and hydrogen pressure inside the
reservoir, respectively. The hydrogen supply pressure is equal
to 6 bar and the cooling fluid temperature is equal to 20 �C.Overall, the hydrogen storage rate instantaneously reaches
a peak initially and then decreases gradually toward zero at
the end of the storage process (Fig. 4). Similarly, the bed
temperature increases sharply and then decreases gradually
tending toward the preset value of the cooling fluid temper-
ature (Fig. 5). Thus, the time history of the storage process can
be split into two stages A and B [19,21].
Over the A stage, at the experiment beginning, the
hydrogen storage rate increases rapidly toward a peak (Fig. 4).
Two major events contribute in the amplitude of the peak: A
rapid spread of hydrogen into the initially nearly empty free
volume and an impulsive absorption reaction induced by the
tal study of metal hydride-based hydrogen storage tank atrgy (2014), http://dx.doi.org/10.1016/j.ijhydene.2014.02.121
Fig. 3 e Synoptic scheme of the experimental setup.
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 en e r g y x x x ( 2 0 1 4 ) 1e84
high-pressure difference between the hydrogen pressure in-
side the tank and the hydride equilibrium pressureðPH2 � PeqÞ,known as driving potential for mass transfer. It should be
pointed that in our case the effect of the first event is negli-
gible due to the small free volume, also because of the rapid
absorption reaction which takes over.
Fig. 4 e Time history of hydrogen storage rate. Accuracy
±0.7 g/min.
Please cite this article in press as: Souahlia A, et al., Experimenconstant supply pressure, International Journal of Hydrogen Ene
As time progresses, a fast and significant drop in hydrogen
storage rate and a rapid rise of both hydride bed temperature
and hydrogen pressure within the reservoir are recorded (Figs.
4 and 5). Due to the poor thermal conductivity of the hydride
bed, the generated heat of absorption is unable to be trans-
ferred from the bed to the cooling fluid at the initial period of
rapid absorption and hence the excess heat is stored in the
hydride bed itself, resulting in a sudden rise in bed tempera-
ture. Thus, the hydride equilibriumpressure increases and the
hydrogen storage rate decreases. The hydrogen pressure
within the tank increases to compensate for the drop of the
driving potential for mass transfer (Fig. 6).
The observations above prove that, along the A stage, the
evacuation of the hydrogen absorption heat via the heat ex-
changers of the reservoir has no influence on the storage rate
because of the rapidity of the reaction. In sum, at the begin-
ning, the hydrogen storage process is driven mainly by the
difference between the hydrogen pressure within the reser-
voir and the hydride equilibrium pressureðPH2 � PeqÞ.Over the B stage, the absorption rate slows down and de-
creases gradually toward zero (Fig. 4). The hydrogen pressure
inside the reservoir has an almost constant value close to the
supply pressure (Fig. 6). The bed temperature decreases
gradually tending toward the preset value of the cooling fluid
temperature (Fig. 5). This is due to an improvement of the heat
tal study of metal hydride-based hydrogen storage tank atrgy (2014), http://dx.doi.org/10.1016/j.ijhydene.2014.02.121
Fig. 5 e Time history of hydride arithmetic average of bed
temperature. Accuracy ±2 �C.
05101520253035404550
3 4 5 6 7 9 11
Volu
me
of st
ored
hyd
roge
n (L
)
Hydrogen supply pressure (bar)
Fig. 7 e Effect of supply pressure on the volume of
hydrogen stored in the tank. Accuracy ±3 L.
i n t e rn a t i o n a l j o u rn a l o f h y d r o g e n en e r g y x x x ( 2 0 1 4 ) 1e8 5
evacuation rate owing to a higher temperature gradient be-
tween hydride bed and coolant and a fall of heat generation.
The observations above prove that, along the B stage,
hydrogen storage is driven mainly by heat transfer rate
through reduction of hydride equilibrium pressure Peq.
Effect of supply pressure
The reservoir is allowed to store hydrogen at different supply
pressures maintaining constant temperature and flow rate of
cooling fluid, respectively, at 20 �C and 10 g/s.
Increasing supply pressure leads to a decrease in the vol-
ume of hydrogen stored in the tank (Fig. 7) and an increase in
the mass of hydrogen stored (Fig. 8). In fact, according to the
perfect gas law, the hydrogen density increases with pressure.
According to Fig. 9, hydrogen storage duration diminishes
with increasing supply pressure. For example, it takes 23 min
to store 10 g of hydrogen at 4 bar supply pressure, while it only
takes one and a half minutes at 11 bar supply pressure.
In Fig. 10, hydrogen storage rate increases with the supply
pressure. At higher supply pressures, the difference between
Fig. 6 e Time history of hydrogen pressure inside the tank.
Accuracy ±0.3 bar.
Please cite this article in press as: Souahlia A, et al., Experimenconstant supply pressure, International Journal of Hydrogen Ene
supply pressure and hydride equilibrium pressure is impor-
tant, which results in higher absorption rate and shorter
storage time.
Fig. 11 shows the time history of hydride bed temperature
for each hydrogen supply pressure. It’s observed that the rise
in bed temperature is higher at higher supply pressures. This
reflects not only an increase in absorption rate at higher
supply pressures but also an improvement in the distribution
of absorption rate inside the reactional volume (Larger num-
ber of hydride particles absorb hydrogen simultaneously). It’s
also observed from Fig. 11 that hydride bed cooling is even
faster than supply pressure increases. This is explained by the
fact that the heat transfer rate enhances with the increase of
temperature difference between the hydride bed and the
coolant. In addition, a higher hydrogen supply pressure leads
to a greater driving potential all along the storage process even
during impulsive stage of absorption (see Fig. 12), it follows
that hydride bed tends rapidly toward its maximum hydrogen
capacity, causing a faster fall in the rate of heat generation
and hence a rapid cooling of hydride bed.
To summarize, at low supply pressures, the pressure dif-
ference ðPH2 � PeqÞ drives the process of hydrogen storage for a
short span of time, hence most of the storage process is gov-
erned and controlled by the heat transfer rate. However, at
0
2
4
6
8
10
12
14
3 4 5 6 7 9 11
Mas
s of s
tore
d hy
drog
en (g
)
Hydrogen supply pressure (bar)
Fig. 8 e Effect of supply pressure on the mass of hydrogen
stored in the tank. Accuracy ±0.7 g.
tal study of metal hydride-based hydrogen storage tank atrgy (2014), http://dx.doi.org/10.1016/j.ijhydene.2014.02.121
0
2
4
6
8
10
12
14
0 500 1000 1500 2000 2500 3000
Mas
s of s
tore
d hy
drog
en (g
)
Time (s)
3 bar4 bar5 bar6 bar7 bar9 bar11 bar
Fig. 9 e Effect of the supply pressure on mass of hydrogen
stored in the tank. Accuracy ±0.5 g.
20
25
30
35
40
45
50
55
60
65
0 500 1000 1500 2000 2500 3000
Aver
age
bed
tem
pera
ture
(°C
)
Time (s)
3 bar4 bar5 bar6 bar7 bar9 bar11 bar
Fig. 11 e Effect of the supply pressure on the arithmetic
average of bed temperature. Accuracy ±2 �C.
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 en e r g y x x x ( 2 0 1 4 ) 1e86
high supply pressures, pressure difference ðPH2 � PeqÞ and heat
transfer rate combine together leading to a faster hydrogen
storage process. In the case of studied tank, a pressure above
5 bar can be considered as a high pressure, because beyond
this pressure, the decrease in the time of hydrogen storage
becomes slower.
Effect of cooling fluid temperature
The effect of cooling fluid temperature on the hydrogen stored
mass illustrated on Fig. 13 show the expected trend that the
hydrogen storage capacity increases at lower cooling fluid
temperature ranges. At lower cooling fluid temperatures, hy-
dride equilibrium pressure is low which results in a larger
pressure difference between supply pressure and hydride
equilibrium pressure. This results in an increase in the
hydrogen storage capacity.
It’s also observed in Fig. 13 that, at high supply pressure,
the effect of cooling fluid temperature on hydrogen storage
capacity is less pronounced because the difference between
supply and equilibrium pressures is large.
0
5
10
15
20
25
0 500 1000 1500 2000 2500 3000
Stor
age
rate
(g/m
in)
Time (s)
3 bar4 bar5 bar6 bar7 bar9 bar11 bar
0
5
10
15
20
25
0 5 10 15 20
Fig. 10 e Effect of the supply pressure on hydrogen storage
rate. Accuracy ±0.7 g/min.
Please cite this article in press as: Souahlia A, et al., Experimenconstant supply pressure, International Journal of Hydrogen Ene
Identification
The main aim of system identification is to determine a
mathematical model of a physical/dynamic system from
experimental data. The identification procedure is summa-
rized in the following steps:
� Record the response of the system to a known excitation
(usually a step signal).
� According to the shape of the response, select a known
mathematical model (the simplest possible with minimal
parameters).
� Optimize the parameters of the mathematical model to fit
with the response.
The hydrogen tank studied in this paper is assimilated to a
system with a single input and a single output. The input is
the hydrogen pressure and the output is the stored mass of
hydrogen as mentioned in Fig. 14, where PH2 Pref, mstr and mss
are respectively inlet hydrogen pressure, reference pressure,
mass of stored hydrogen and maximum storage capacity of
hydrogen.
-1
0
1
2
3
4
5
6
7
8
9
10
0 200 400 600 800 1000Time (s)
3 bar4 bar5 bar6 bar7 bar9 bar11 bar
(bar
)
Fig. 12 e Effect of the supply pressure on driving potential
for mass transfer ðPH2LPeqÞ. Accuracy ±0.6 bar.
tal study of metal hydride-based hydrogen storage tank atrgy (2014), http://dx.doi.org/10.1016/j.ijhydene.2014.02.121
0
2
4
6
8
10
12
14
0 500 1000 1500 2000 2500
Mas
s of s
tore
d hy
drog
en (g
)
Time (s)
Fig. 13 e Effect of the thermostatic water temperature on
mass of stored hydrogen. Accuracy ±0.5 g.
Fig. 14 e Systemwith single input and output modeling the
tank.
00,10,20,30,40,50,60,70,80,91
0 500 1000 1500 2000 2500Time (s)
Response at 20°C
Model at 20 °C
Response at 40°C
Model at 40 °C
Fig. 16 e Time history of the response of the tank to a step
of hydrogen pressure at two different cooling temperatures
(20 �C and 40 �C).
i n t e rn a t i o n a l j o u rn a l o f h y d r o g e n en e r g y x x x ( 2 0 1 4 ) 1e8 7
For LaNi5 mss, ¼ 14 (g of H2/kg of LaNi5) and assuming that
the hydrogen working pressure of the tank is equal to 5 bar,
then Pref¼ 5 bar. Fig. 15 shows the time history of the response
of the tank to a step of hydrogen pressure PH2 ¼ 5 bar at cooling
temperature of 20 �C.According to the shape of the response, the tank can be
considered as a first order system and the corresponding
mathematical model is the following:
mstrðtÞmss
¼ K
�1� exp
��ts
��
where K is the asymptotic limit of the response and s (s) is the
time constant of the system. In our case, K and s are estimated
by trial and error. Other mathematic models and parameters
estimation methods exist and will be further discussed in
0
0,1
0,2
0,3
0,4
0,5
0,6
0,7
0,8
0,9
1
0 500 1000 1500Time (s)
Response
Model
Fig. 15 e Time history of the response of the tank to a step
of hydrogen pressure.
Please cite this article in press as: Souahlia A, et al., Experimenconstant supply pressure, International Journal of Hydrogen Ene
future work. The mathematical model fit well with the
experimental response for K ¼ 0.91 and s ¼ 460 s (Fig. 15).
Fig. 16 shows that an increasing cooling water tempera-
ture results in different values of the model parameters:
K ¼ 0.83 and s ¼ 1150 s. We can conclude that s estimates the
speed of the hydrogen storage and K evaluates the mass of
stored hydrogen in relation to a referential value (mss). The
step response described above and the derived parameters
allow a quantitative comparison between the performances
of tanks.
Conclusion
A prototype of a metal hydride cylindrical tank is tested. This
tank is fitted with two heat exchangers for a better hydride
temperature regulation: an inner finned spiral heat exchanger
and a lateral heat exchanger. The important characteristics of
the metal hydride tank were analyzed by means of constant
hydrogen supply pressure tests. At any given cold fluid tem-
perature, the hydrogen storage time was found to be lesser at
higher supply pressure. Also it was found that the volume of
stored hydrogen decreases with increase of supply pressure.
Furthermore, at higher supply pressure, the heat transfer rate
is enhanced and the effect of the driving force for mass
transfer is stronger and lasts longer. Cooling fluid temperature
has a strong influence on hydrogen storage capacity and time,
however this influence is less pronounced for high supply
pressures. We discussed the response of the tank to a
hydrogen pressure step and tow parameters were derived K
and s to characterize quantitatively the performances of the
metal hydride hydrogen storage tank.
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