Controlled hydrogen generation by reaction of aluminum/sodium ...

international journal of hydrogen energy 37 (2012) 5811e5816
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Controlled hydrogen generation by reaction of aluminum/
sodium hydroxide/sodium stannate solid mixture with water
Guang-Lu Ma, Hong-Bin Dai*, Da-Wei Zhuang, Hai-Jie Xia, Ping Wang*
Shenyang National Laboratory for Materials Science, Institute of Metal Research, Chinese Academy of Sciences, 72 Wenhua Road,
Shenyang 110016, PR China
article info
Article history:
Received 1 November 2011
Received in revised form
22 December 2011
Accepted 29 December 2011
Available online 23 January 2012
Keywords:
Hydrogen storage
Hydrogen generation
Aluminum
Kinetics
abstract
Aluminum/water reaction system has gained considerable attention for potential
hydrogen storage applications. In this paper, we report a new aluminum-based hydrogen
generation system that is composed of aluminum/sodium hydroxide/sodium stannate
solid mixture and water. This new system is characterized by the features as follows: the
combined usage of sodium hydroxide and sodium stannate promoters, the use of solid fuel
in a tablet form and the direct use of water as a reaction controlling agent. The factors that
influence the hydrogen generation performance of the system were investigated. The
optimized system exhibits a favorable combination of high hydrogen generation rate, high
fuel conversion, rapid dynamic response, which makes it promising for portable hydrogen
source applications.
Copyright ª 2012, Hydrogen Energy Publications, LLC. Published by Elsevier Ltd. All rights
reserved.
1. Introduction
Hydrogen storage is widely recognized as the most technically
challenging barrier to the implementation of hydrogen fuel cell
technology. The last few decades have witnessed the discovery
of many novel solid materials that can reversibly store
hydrogen [1]. But unfortunately, the research efforts on these
materials have led to no viable systems that can reversibly
store over 6 wt% hydrogen under relevant conditions to the
practical operation of proton exchange membrane fuel cell.
Recently, the hydrogen-rich chemical hydrides received everincreasing
attention as potential hydrogen storage media.
Extensive studies of the representative chemical hydrides (e.g.
sodium borohydride and ammonia borane) have given rise to
a number of material systems that exhibit rapid and controlled
H 2 release at moderate temperatures [2e6]. But the viability of
any chemical hydrogen storage system depends not only on its
dehydrogenation performance, but also on the recyclability of
the hydride materials. Currently, owing to the lack of energyefficient
and cost-effective routes for spent fuel regeneration,
the boron-containing chemical hydrides are greatly limited in
the practical hydrogen storage applications [2]. This situation
has motivated the development of affordable hydrogen
generation (HG) system using cheap and/or renewable materials.
Here, aluminum (Al) is clearly a preferred choice [7,8].
Al þ 3H 2 O/AlðOHÞ 3
Y þ 1:5H 2 [ þ 426:5kJ (1)
Al reacts with H 2 O following Eq. (1), yielding 3.7 wt% H 2 .
Although the gravimetric hydrogen density is moderately low,
the Al/H 2 O system has many favorable attributes that make it
an attractive candidate for portable applications. Al is an
abundant, inexpensive and readily available material. HG
from the Al/H 2 O reaction occurs in a self-sustaining way
without external providing energy at ambient temperature.
Furthermore, the environmentally benign by-products
generated in the Al/H 2 O reaction can be recycled back to
* Corresponding authors. Tel.: þ86 24 2397 1622; fax: þ86 24 2389 1320.
E-mail addresses: hbdai@imr.ac.cn (H.-B. Dai), pingwang@imr.ac.cn (P. Wang).
0360-3199/$ e see front matter Copyright ª 2012, Hydrogen Energy Publications, LLC. Published by Elsevier Ltd. All rights reserved.
doi:10.1016/j.ijhydene.2011.12.157

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international journal of hydrogen energy 37 (2012) 5811e5816
metallic Al using well-established technologies [8,9]. But the
development of Al/H 2 O system as practical hydrogen source
requires a solution to the long-standing problem of surface
passivation of Al. Currently, there are a number of approaches
under investigation, which can be divided into two categories:
one is addition of hydroxides [10,11], metal oxides [12,13] or
selected salts [14,15] to disrupt the passivation layer; the other
is alloying Al with low melting point metals to inhibit the
formation of a coherent passivation layer [16e19]. In our study
of the Al/H 2 O reaction system, we mainly focused on the alkali
approach because the alkali-promoted system always
outperforms other systems in terms of HG kinetics. But
meanwhile, the use of alkali promoter causes corrosion of the
system apparatus. From a practical point of view, novel
technologies that enable minimization of alkali concentration
without compromising of HG performance are highly
desirable.
Quite recently, our study found that a combined usage of
NaOH and Na 2 SnO 3 can dramatically improve the HG
kinetics of the Al/H 2 Osystem[20]. Furthermore, the addition
of a small amount of Na 2 SnO 3 causes a remarkable decrease
of NaOH concentration that is required for achieving favorable
HG performance. This finding provides a simple but
effective method for simultaneously addressing the reaction
kinetics and alkali corrosion problems of the Al/H 2 O system.
Stimulated by this finding, we further investigated a new
system, which is composed of Al/NaOH/Na 2 SnO 3 solid
mixture and H 2 O. In comparison with the traditional Al/H 2 O
system using aqueous NaOH solution, the new system
exhibits a series of advantages on HG performance, manipuility
and adaptability, which makes it promising for
portable hydrogen source applications. We herein show the
study results.
2. Experimental
2.1. Preparation of solid fuel and sample
characterization
Al powder (99% purity), NaOH (98% purity) and sodium stannate
trihydrate (Na 2 SnO 3 $3H 2 O, 99% purity) were purchased
from Sinopharm Chemical Reagent Corporation. In the
present study, a series of Al powder samples with different
particle sizes were employed and characterized by a Mastersizer
2000 particle size analyzer. Anhydrous sodium stannate
(Na 2 SnO 3 ) was prepared by calcining Na 2 SnO 3 $3H 2 O at 350 C
for 1 h.
The Al/NaOH/Na 2 SnO 3 powder mixtures in varied mass
ratios were hand-milled using a glass mortar and pestle or
mechanically milled by a Fritsch 7 planetary mill at 400 rpm
for 1 h. After the ball-milling, the solid fuel mixture was
pressed into a tablet by a pellet machine at 10 MPa for 10 min.
The diameter and height of the resulting tablet were 15 and
3 mm, respectively.
The solid residue of the Al/H 2 O reaction was analyzed by
powder X-ray diffraction (XRD, Rigaku D/max-2500, Cu Ka
radiation). In preparation of the XRD samples, the solid
residue was dried at 80 C under a dynamic vacuum condition
for 48 h.
2.2. Hydrogen generation performance testing
The experimental setup used for measurement of HG properties
has been described in a previous paper [21]. The reaction
was carried out in a 250 ml three-neck flask, wherein the solid
fuel was preloaded. The water was fed into contact with the
solid fuel using a pressure-equalizing dropping funnel. Typically,
the feeding rate of water was controlled at around
10 g min 1 . The generated hydrogen gas passed through
a trap/heat exchanger to cool to room temperature followed
by contacting with a silica drier to remove the moisture in the
gas stream. The HG rate was measured using an online mass
flow meter (Sevenstar Huachang, MFM D07e7BM, accuracy
within 2%) that was equipped with a computer. The HG
volume was calculated by integrating the measured HG rate
over time. In the whole testing process, no attempt was made
to control the temperature of the reaction system. The reaction
temperature was monitored using a thermocouple
embedded in the solid fuel and recorded using an online
recorder. Each experiment was repeated twice. The determined
relative error was no more than 5%.
3. Results and discussion
3.1. Development of a new Al-based hydrogen
generation system
The newly developed HG system is composed of Al/NaOH/
Na 2 SnO 3 solid mixture and water. In comparison with the
previous systems that use aqueous solution of promoting
additives, the present system using water as a reaction
controlling agent is clearly of increased practicability. As
shown in Fig. 1, feeding water into contact with the Al/NaOH/
Na 2 SnO 3 solid fuel rapidly initiates vigorous H 2 release. The
system can complete a 100% fuel conversion within 3 min
with a maximum HG rate of 1740 ml min 1 . In contrast, the
systems containing the same mass of individual NaOH or
Fig. 1 e A comparison of the HG rate (top) and yield
(bottom) among the systems: (a) 1 g of Al powder/0.2 g of
NaOH/0.1 g of Na 2 SnO 3 /5 g of H 2 O; (b) 1 g of Al powder/0.3 g
of NaOH/5 g of H 2 O; (c) 1 g of Al powder/0.3 g of Na 2 SnO 3 /5 g
of H 2 O.

international journal of hydrogen energy 37 (2012) 5811e5816 5813
Na 2 SnO 3 additive can only fulfill a 60e70% fuel conversion
within 8 min, and the maximum HG rates of the two systems
are 860 and 280 ml min 1 , respectively. These results are
consistent with the previous finding [20], showing the
advantage of the combined usage of NaOH and Na 2 SnO 3
additives in promoting Al/H 2 O reaction.
Examination of the HG kinetics curves in Fig. 1 found that
the system containing NaOHþNa 2 SnO 3 additives shows one
major HG event, whereas the system containing 0.3 g NaOH
additive exhibits two separated HG steps. This finding clearly
indicates that addition of Na 2 SnO 3 causes a significant change
of Al/H 2 O reaction behavior. In our effort to understand these
phenomena, we first conducted a series of control experiments
to gain insight into the reaction behavior of Al/NaOH/
H 2 O system. Fig. 2 presents a comparison of the HG kinetics of
the Al/H 2 O system containing different quantities of NaOH
additive. It was found that the systems containing 0.3e0.8 g of
NaOH, corresponding to 1.5e4 M with respect to water, show
two HG steps and the time interval between the two steps is in
inverse proportion to the NaOH quantity. When the addition
quantity of NaOH is beyond this critical range, the system
exhibits only one HG step. These results clearly show that the
quantity of NaOH or OH concentration plays a decisive role in
the two step HG phenomenon. For a given system containing
moderate quantity of NaOH, the termination and restart of the
HG reaction should originate from the variation of local OH
concentration. Presumably, it is the mass transfer factor that
causes variation of OH concentration, as discussed below.
Al þ 4OH /AlðOHÞ 4
þ 3e E 0 ¼ 2:310V (2)
3H 2 O þ 3e /1:5H 2 [ þ 3OH E 0 ¼ 0:828V (3)
AlðOHÞ 4
4AlðOHÞ 3
Y þ OH (4)
The Al/H 2 O reaction in the presence of hydroxide involves
formation of aluminate, water reduction and the reversible
decomposition of Al(OH) 4 [22], as described by Eqs. (2)e(4).
Although the overall HG reaction consumes no OH (as
expressed by Eq. (1)), considerable amount of OH is trapped
in the form of Al(OH) 4 owing to its relatively slow regeneration
rate following Eq. (4). More importantly, the local accumulation
of Al(OH) 4 ions may block the diffusion of OH to the
reaction region. A combination of these two factors may cause
gradual decrease of OH concentration in the vicinity of Al
surface. As a consequence, both the HG rate and dissolution
rate of Al(OH) 3 will be reduced. This may ultimately result in
the formation of coherent Al(OH) 3 passivation layer on the
surface of Al and the termination of HG reaction. Once the
Al(OH) 4 “barrier layer” is diminished due to dilution, OH may
gain access again to the Al surface. If the OH concentration is
high enough for disrupting the Al(OH) 3 passivation layer, the
Al/H 2 O reaction can be restarted. This hypothesis can well
explain the observed effect of OH concentration on the HG
behavior of the Al/H 2 O system. For example, increasing the
quantity of NaOH additive will result in an increase of the
mass transfer rate of OH ion, and thereby shortening the
time interval for restarting the HG reaction. When the quantity
of NaOH is higher than the critical range, a 100% fuel
conversion can be completed before the cohesive Al(OH) 3
passivation layer is formed. In another extreme case, the low
OH concentration is insufficient for disrupting the formed
Al(OH) 3 passivation layer, thereby prohibiting the occurrence
of the second HG event.
4Al þ 3SnðOHÞ 2 6 /4AlðOHÞ 4 þ 3Sn þ 2OH E0 ¼ 1:41V (5)
The stepwise HG is undesirable for practical hydrogen
storage applications as it may cause problematic HG controllability
of Al/H 2 O reaction system. Our study showed that the
combined usage of NaOH and Na 2 SnO 3 additives provides
a simple approach for addressing this problem. The rationale
behind this approach is to inhibit the formation of cohesive
Al(OH) 3 passivation layer on the surface of Al. As seen in Fig. 3,
XRD analysis of the post-reacted Al/NaOH/Na 2 SnO 3 /H 2 O
system clearly identified Al(OH) 3 and AlO(OH) by-products, as
well as metallic Sn. The formation of metallic Sn from
Na 2 SnO 3 , which exists in form of Na þ and [Sn(OH) 6 ] 2 in the
alkaline solution, can be described by Eq. (5). The in situ
formed Sn particles may combine with Al to construct
numerous microgalvanic cells to accelerate the Al/H 2 O reaction.
More importantly, the deposited metallic Sn on the
Fig. 2 e Effects of NaOH concentration on the HG rate (top)
and yield (bottom) of the system containing 1 g of Al
powder and x g of NaOH (x [ 0.2, 0.3, 0.5, 0.8 and 1.2) and
5gofH 2 O.
Fig. 3 e XRD pattern of the solid residue that was collected
after HG reaction of the system.

5814
international journal of hydrogen energy 37 (2012) 5811e5816
surface of Al may prevent the formation of cohesive Al(OH) 3
passivation layer. As a consequence, the Al/H 2 O reaction can
proceed in a continuous way, even in the presence of low OH
concentration.
3.2. Study of hydrogen generation properties of the Al/
NaOH/Na 2 SnO 3 /H 2 O system
As demonstrated, the newly developed Al/NaOH/Na 2 SnO 3 /
H 2 O system possesses a series of advantages over the traditional
NaOH-promoted system in terms of HG performance.
To evaluate its potential for practical hydrogen storage
applications, we further conducted a systematic study of the
factors that influence the HG performance of the system. The
first factor we examined is the NaOH:Na 2 SnO 3 mass ratio. For
comparison purpose, the quantities of Al, H 2 O and promoting
additives were fixed at 1, 5 and 0.3 g, respectively. As seen in
Fig. 4, changing the NaOH:Na 2 SnO 3 mass ratio from 2:1 to 1:2
results in a decrease of the HG rate and yield, showing that the
system containing 0.2 g of NaOH and 0.1 g of Na 2 SnO 3 shows
the best HG performance.
Next, we examined the effect of the particle size of Al
powder on the HG performance of the system. As seen in
Table 1, both the HG rate and yield increase with reducing the
particle size of Al powder. This should be ascribed to the
variation of the surface area of Al. When using Al powder with
an average particle size smaller than 68 mm, the system
exhibited high HG rate and achieved 100% fuel conversion. In
an overall consideration of the HG performance, material cost
and availability, we selected the Al powder with an average
particle size of 68 mm for further investigation.
The newly developed HG system uses Al/NaOH/Na 2 SnO 3
mixture as solid fuel. Our study found that the mixing state
and form of the solid fuel exert important effect on the HG
performance of the system. As shown in Fig. 5, pretreatment
of the solid fuel by ball-milling instead of hand-milling results
in an increase of HG rate and a reduction of induction period.
This should be mainly attributed to the improved dispersion
Table 1 e Effect of the particle size of Al powder on the HG
performance of the Al-based system. Note: the Al-based
system is composed of 1 g of Al powder, 0.2 g of NaOH,
0.1 g of Na 2 SnO 3 and 5 g of H 2 O.
Average particle
size of Al (mm)
Max. HG rate
(ml min 1 g 1 Al)
Yield (%)
278 410 83.4
198 515 85.2
152 740 88.3
125 1025 94.3
68 1740 100
16 2100 100
of promoting additives in the solid fuel. In addition, the
extensive mechanical milling may create increased opportunity
for the close contact between the additive particles and
the fresh surface of Al, which should also contribute to the
improvements of HG performance. In spite of the clear benefits
on HG performance, the solid fuel in powder form is
undesirable for the practical hydrogen storage application due
to the poor operationality, safety concern, as well as the
complicated system design. For this reason, we pressed the
ball-milled fuel powder into the tablets. As seen in Fig. 5, the
system using the solid fuel tablets shows a similar HG rate, but
a much longer induction period than those of the systems
using solid powder fuel. Our preliminary study found that this
problem can be alleviated by adding small amount of Al
powder. For example, extra addition of 0.2 g of Al powder into
the system containing 1.3 g of solid fuel tablet leads to
a reduction of induction period from 1 to 0.5 min, as shown in
Fig. 5(d).
Finally, we examined the effect of water type on the HG
performance of the system. As seen in Fig. 6, changing the
water type from deionized water to tap water exerts no
appreciable influence on the HG performance of the system.
Among the three types of water we examined, the sea water
containing 3.5 wt% of NaCl is the best choice. In comparison
Fig. 4 e Effects of the NaOH:Na 2 SnO 3 mass ratio on the HG
rate (top) and yield (bottom) of the system. The quantities
of Al, H 2 O and promoting additives were fixed at 1, 5 and
0.3 g, respectively.
Fig. 5 e Effect of pretreatment of the solid fuel on the HG
kinetics of the system composed of 1 g of Al powder/0.2 g of
NaOH/0.1 g of Na 2 SnO 3 and 5 g of water: (a) hand-milled; (b)
ball-milled; (c) ball-milled and pressed; (d) the system (c)
with extra addition of 0.2 g of Al powder. The inset shows
a photo of the solid fuel tablet with a density of 2.45 g cm L3 .

international journal of hydrogen energy 37 (2012) 5811e5816 5815
with the system using deionized water, the system using sea
water exhibits an around 10% increase on HG rate and
a slightly shortened induction period. Presumably, the
advantage of sea water over the other two types of water
originates from the enriched chlorine ions, which may accelerate
the dissolution reaction of the passivation layer on the
Al surface [18]. Evidently, using water as a reaction controlling
agent implies the wide applicability of the newly developed
HG system.
3.3. “Start/stop” hydrogen generation dynamics
Rapid dynamic response to the highly varying hydrogen
demands is another prerequisite for a practical HG system. In
the present study, we tested the dynamic response property of
the Al/NaOH/Na 2 SnO 3 /H 2 O system in a discontinuous HG
process, which involves cyclic start/stop of water supply to
the reactor containing solid fuel. To avoid the influence of fuel
temperature on the HG performance, the reactor was cooled
down to ambient temperature between each stop/start cycle.
As shown in Fig. 7, feeding water into contact with the solid
fuel immediately initiates vigorous H 2 release. In the first two
cycles, the HG reaction reaches its maximum rate within
around 1.3 min, and after switching off the water supply, the
HG reaction can be terminated within around 1 min. But in the
third cycle, the system exhibits a multi-step HG behavior and
requires a relatively long duration for terminating the HG
reaction. Most likely, this should be ascribed to the deteriorated
mass transfer environment, wherein the accumulated
by-products block the water from contacting the unreacted Al.
But despite of the property degradation, the HG reaction in the
third cycle exhibits a maximum rate of 450 ml min 1 , which is
75% of the level in the first cycle. After three start/stop cycles,
the total HG yield of the system reaches up to 93%. In a general
view, the newly developed system shows satisfactory
dynamic response property. This is of clear significance for
the design of practical hydrogen generator.
Using the data obtained from “start/stop” HG dynamics
measurement, we can estimate the power level of the newly
developed system. If the new system is combined with
Fig. 7 e “Start/stop” HG dynamics and temperature profiles
of the system composed of three pieces of solid fuel tablets
(as shown in the inset) and 15 g of water. The feeding rate
of water was fixed at 2 g min L1 .
a standard proton exchange membrane fuel cell operating at
0.7 V, a HG rate of 500 ml min 1 is equivalent to a power level
of 40 W. This can meet the power demands of some portable
or mobile apparatus. Using the current price of primary Al, 2.4
US$ per kg, as a calculation benchmark, the H 2 -production
cost of the present system is estimated to be around 21 US$
per kg H 2 [9]. This H 2 -production cost is much lower than
those of the chemical hydrogen storage systems using boroncontaining
chemicals [2,5].
4. Conclusions
Our study demonstrated a new Al-based hydrogen generation
system, which is composed of Al/NaOH/Na 2 SnO 3 solid mixture
and water. As a consequence of the pronounced promoting
effects of NaOH and Na 2 SnO 3 additives, the on-demand
hydrogen generation can be readily achieved by regulating
the water supply to the solid fuel. The new system possesses
a favorable combination of high hydrogen generation rate,
high fuel conversion, rapid dynamic response and low material
cost, which makes it promising for portable hydrogen source
applications. In addition, the use of solid fuel in a tablet form
and the adaptability to different types of water greatly increase
the applicability of the new system. Our study shows the
feasibility of achieving high-performance hydrogen generation
using cheap and readily available materials, thereby laying
a foundation for developing practical hydrogen generators.
Acknowledgments
Fig. 6 e Effects of the type of water on the HG rate (top) and
yield (bottom) of the system composed of a piece of solid
fuel tablet (1 g of Al powder/0.2 g of NaOH/0.1 g of Na 2 SnO 3 )
and 5 g of H 2 O.
The financial supports for this research from the National
Basic Research Program of China (973 program, Grant No.
2010CB631305), the National Outstanding Youth Science
Foundation of China (Grant No. 51125003), the National
Natural Science Foundation of China (Grant No. 51071155), the
Natural Science Foundation of Liaoning Province (Grant No.
20102231), and the Main Direction Program of Knowledge
Innovation of CAS are gratefully acknowledged.

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international journal of hydrogen energy 37 (2012) 5811e5816
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