international journal of hydrogen energy 33 (2008) 71107115

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Accurately measuring the hydrogen generation rate for

hydrolysis of sodium borohydride on multiwalled carbon
nanotubes/CoB catalysts
Yueqiang Huanga, Yi Wanga, Ruixiong Zhaoa, Pei Kang Shena,*, Zidong Weib,*
a

State Key Laboratory of Optoelectronic Materials and Technologies, School of Physics and Engineering, Sun Yat-Sen University,
Guangzhou 510275, China
b
The State Key Laboratory of Power Transmission Equipment & System Security and New Technology, Chongqing University,
Chongqing 400044, China

article info

abstract

Article history:

Multiwalled carbon nanotubes supported cobaltboron catalysts (CoB/MWCNT) were

Received 20 August 2008

developed via the chemical reduction of aqueous sodium borohydride with cobalt chloride

Received in revised form

for catalytic hydrolysis of alkaline NaBH4 solution. The hydrogen generation (HG) rates

18 September 2008

were measured on an improved high-accuracy, low-cost and automatic HG rate

Accepted 19 September 2008

measurement system based on the use of an electronic balance with high accuracy. The HG

Available online 7 November 2008

of CoB/MWCNT catalyst was investigated as a function of heat treatment, solution

temperature, CoB loading and supporting materials. The catalyst was mesoporous

Keywords:

structured and showed lower activation energy of 40.40 kJ mol1 for the hydrolysis of

Catalytic hydrolysis

NaBH4. The CoB/MWCNT catalyst was not only highly active to achieve the average HG

Hydrogen generation

rate of 5.1 l min1 g1 compared to 3.1 l min1 g1 on CoB/C catalyst under the same

Sodium borohydride

conditions but also reasonably stable for the continuous hydrolysis of NaBH4 solution.

Multiwalled carbon nanotubes

2008 International Association for Hydrogen Energy. Published by Elsevier Ltd. All rights

CoB catalyst

1.

Introduction

The supply of hydrogen for portable fuel cells is crucial, but is

still a problem [1]. Among hydrogen storage methods, chemical hydrides have been demonstrated to be promising
hydrogen sources for portable applications [2,3]. Sodium
borohydride (NaBH4) has been intensively investigated due to
its advantages of high H2 storage efficiency (10.8 wt.%),
stability of its solution under high pH value in air, easily
controlled hydrogen generation (HG) and high purity of
hydrogen from the catalytic hydrolysis of NaBH4 solution,
nonflammability and side product recyclability [35]. Various
catalysts have been developed for catalytic hydrolysis of

reserved.

NaBH4 solution to generate pure hydrogen, such as Pt [2], Ru

[3,6], Pd [7], nickel boride [8] and cobalt boride [9]. The use of
highly active noble metal catalysts in practical applications is
restricted by their high cost. However, the reported catalysts
used for the decomposition of NaBH4 are readily poisoned by
the borate ion that is generated with hydrogen [10]. Our
motivation is to develop highly active and relative stable
catalysts for the hydrogen generation from NaBH4 [11].
High-surface-area supporting materials provide a potential
route to achieve the well dispersion of a catalyst to increase
the contact area with the reactants sufficiently. Actually,
carbon supported platinum [12] and carbon supported CoB
[13] catalysts show very good activities for the catalytic

* Corresponding author. Tel.: 86 20 84036736; fax: 86 20 84113369.

E-mail addresses: stsspk@mail.sysu.edu.cn (P.K. Shen), zdwei@cqu.edu.cn (Z. Wei).
0360-3199/$ see front matter 2008 International Association for Hydrogen Energy. Published by Elsevier Ltd. All rights reserved.
doi:10.1016/j.ijhydene.2008.09.046

international journal of hydrogen energy 33 (2008) 71107115

hydrolysis of NaBH4 solution. Pore structures of the supporting materials affect the performance of catalysts as well.
Mesoporous structures of the supporting materials are beneficial to the gas and water transport. The mesoporous SiCNcoated multiwalled carbon nanotubes (MWCNTs) paper
supported Pt and Pd showed excellent activities [14]. The
hydrophilicity of the supporting materials contributes to the
well-stable dispersion for a catalyst. MWCNTs have been used
in many areas due to the high specific BET area and unique
electronic properties. The walls of the MWCNTs can be made
hydrophilic by acid treatment [15]. In the 1950s, Schlesinger
et al. firstly found that cobalt chloride could catalyze the
hydrolysis of NaBH4 [4]. Since then, CoB catalysts were
intensively interested [13,1620] for on-demand HG due to its
good catalytic activity and low cost. In the present work, acid
treated MWCNTs were used to support CoB via the chemical
reduction of aqueous sodium borohydride with cobalt chloride. HG rate was investigated using the as-prepared CoB/
MWCNT catalysts as a function of heat treatment, CoB
loading, solution temperature and supporting materials.
As we know, the in situ measurement of the HG rate is
important for hydrolysis of NaBH4. Many useful HG rate
testing methods have been developed, such as water
displacement method [3,5], water trap method [2,21], flow
meter method [22], and fuel cell test method [23]. The accuracy is limited by using either water displacement method or
water trap method. The electronic gas flow meter gives
accuracy at 1 FS% and is relatively expensive. Besides, the
temperature, pressure and the water vapour in the hydrogen
affect the data accuracy measured by the gas flow meter [23].
The development of a high-accuracy, low-cost and easymanipulative method is necessary and important. In this
work, we report an improved testing system for automatically
and accurately measuring the HG rate.

2.

Experimental

2.1.

Catalyst preparation

All the reagents were of analytical grade and used as received.

In a typical experiment, CoB/MWCNT catalysts were prepared
by the impregnation-chemical reduction method [18].
MWCNTs (3.0 g, Shenzhen Nanotech. Co., Ltd., China) with
nanotube diameters of 1020 nm and purity of >95% were
mixed with 100 ml of the solution of 98% H2SO4 and 65% HNO3
(1:1 by volume) under constant stirring for 15 min and then
refluxed at 100  C for 4 h. The acid treated MWCNTs were

7111

filtered, rinsed thoroughly using distilleddeionized water until

neutral and dried in vacuum at 80  C for 12 h. After the treatment, acid treated MWCNTs (1.0 g) were added into 136 ml
CoCl2 solution (0.025 mol l1) in a beaker. Then, the solution
was stirred for 24 h. Subsequently, the alkaline NaBH4 solution
(5.1 ml, 1 mol l1 NaBH4 1 mol l1 NaOH) as a reducing agent
was added to CoCl2 solution drop wise with magnetic stirring.
During the reduction reaction, the reactor was placed in ice
water that was maintained at 0  C in order to prevent
a vigorous reaction. The produced black precipitates were
filtered and washed repeatedly using distilleddeionized water.
Five catalyst samples with different CoB loadings (3.26 wt.%,
7.71 wt.%, 17.33 wt.%, 29.36 wt.% and 100 wt.%, respectively)
were prepared by changing the reactants ratios. The CoB/
MWCNT catalysts were then dried in vacuum at 80  C and
treated in Ar (99.99% purity) atmosphere at 300, 500 and 700  C,
respectively. CoB on carbon (Vulcan XC-72 C, Carbot, USA)
(CoB/C) catalysts were also prepared for the comparison.

2.2.

Catalyst characterization

Phase structures of the as-prepared CoB/MWCNT catalysts

were characterized by powder X-ray diffraction (XRD, Rigaku
D/MAX-III A, Cu Ka1 radiation). The morphologies of the
prepared catalysts were characterized on a scanning electron
microscope (SEM, Quanta 400 FEG). Co and B contents in the
catalysts were determined by inductively coupled plasmaatomic emission spectrometry (ICP-AES, TJA Iris). Nitrogen
adsorptiondesorption of the catalysts was measured at
196  C on a Nova-1000 surface area analyzer (Quantachrome
Instruments).

2.3.

HG rate measurement method

We developed a HG rate measurement method based on the

use of an electronic balance. Instead of the measurement of the
gas volume, we measure the weight of the water replaced by
the gas generated during the hydrolysis of NaBH4. High accuracy and sensitivity can be achieved using an electronic balance
(0.002 FS% compared to 1 FS% for a gas flow meter) since the
mass density of water is very close to 1.0 g cm3 from 0  C
(0.99984 g cm3) to 50  C (0.98804 g cm3). An automatic HG rate
testing system is schematically shown in Fig. 1. An electronic
balance (G&G JJ5000, 0.002 FS% accuracy) was connected to
a computer. The weight data were automatically recorded by
a data acquisition software modified by ourselves (one datum
every two seconds generally). The systematic error and
personal error can be substantially reduced in such a way.

Fig. 1 Schematic diagram of HG rate measurement system.

international journal of hydrogen energy 33 (2008) 71107115

The catalytic activities of the synthesized catalysts for the

hydrolysis of alkaline NaBH4 solution were studied in a batch
reactor. In a typical experiment, 50.0 g of the alkaline NaBH4
solution and 10.0 mg catalyst were introduced into a round
bottom flask which was water-bathed in a thermostatic
apparatus. The NaBH4 solution was maintained at a temperature of 30  C. In order to reduce the pressure variation, the
generated gas was cooled down to 25  C by a thermostatic
apparatus. After the test, the corresponding hydrogen volume
was calculated according to the weight of water displaced by
hydrogen. The specific HG rate (l min1 g1 CoB) was used to
compare the activities of the catalysts.

3.

Results and discussion

3.1.

Effect of heat-treatment temperature

Fig. 2 is a SEM micrograph which shows the surface

morphology of the CoB/MWCNT catalyst treated at 300  C.
The tube diameter of the original MWCNT is 2040 nm. After
loaded catalyst, each MWCNT was uniformly coated with
a layer of CoB and the tube diameter was expanded to 90
120 nm.
It was reported that the freshly prepared CoB catalysts
were amorphous in structure, while crystallization and
decomposition of the CoB amorphous occurred at temperature above 300  C [9,24]. The dependence of the product
composition on the temperature is shown in Fig. 3. It is clear
that the products were amorphous until the heat treatment
over 300  C. In fact, it is a mixture of different CoB
compounds. The diffraction peak around 44 is overlapped by
the peaks of CoB compounds and metallic Co when the
product was treated over 500  C. Scherrer equation was
adopted to calculate the average crystalline size of the CoB
catalysts, as described by Eq. (1):

MWCNT
Metallic Co
CoB
Co2B

Intensity / a.u.

7112

(d)
(c)
(b)
(a)

20

30

40

50

60

70

80

2 Theta / deg.
Fig. 3 XRD patterns of CoB/MWCNT catalysts heattreated at (a) 80 8C, (b) 300 8C, (c) 500 8C and (d) 700 8C,
respectively.

0:9lKa1
B2q cos qmax

(1)

where lKa1 is the wavelength of Cu Ka1 radiation (1.54056 nm),

B2q is the half-width of the diffraction peak. Another parameter qmax is the 2q degree of the diffraction peak. The value of
the average crystalline size L can be calculated through Eq. (1).
The peak at 44.2 was used to calculate the average crystalline
sizes of the catalysts and the values are 15 nm, 23 nm and
52 nm at the heat temperature of 300  C, 500  C and 700  C,
respectively. The effect of the heat temperature of CoB/
MWCNT catalysts on their catalytic activities is described in
the following sections.
It is known that the activity of catalyst is proportional to its
active surface area or inversely proportional to its particle size.
The XRD results showed that the crystalline size of CoB is
related to the heat-treatment temperature. Fig. 4 shows the
real-time HG rate of CoB/MWCNT catalysts treated at different

HG rate / l min-1 g-1 Co-B

80 oC
300 oC

500 oC

700 oC

4
3
2
1
0
0

10

15

20

25

30

Time / min

Fig. 2 SEM micrograph of a 17.33 wt.% CoB/MWCNT

catalyst treated at 300 8C.

Fig. 4 Effect of the heat temperature on the HG rate

measured in 20 wt.% NaBH4 D 3 wt.% NaOH solution
containing 10 mg of 17.33 wt.% CoB/MWCNT at 30 8C.

7113

international journal of hydrogen energy 33 (2008) 71107115

15

10

25

30

35

40

45

50

55

120

0.8
0.6
0.4
0.2
0

5 10 15 20 25 30
Pore Diameter/nm

40

Co-B/MWCNT
Co-B/C

60

0.0

0.2

0.4

0.6

0.8

Relative Pressure/P

1.0

Po-1

Fig. 7 Nitrogen adsorption/desorption isotherm curves for

CoB/MWCNT and CoB/C. The inset is the pore size
distribution of the CoB/MWCNT.

b
E=40.40 kJ mol-1
lnr=lnk0+(-E/R)*T-1

-0.5

lnrreact

Co-B/MWCNT

1.0

0.0

80

Temperature / oC
0.0

1.2
3 -1

20

160

dV(logd)/cm g

Adsorbed Nitrogen Volume/cm3 g-1

Average HG rate / l min-1 g-1 Co-B

25

-1.0

-1.5

-2.0
3.0

3.1

3.2

3.3

3.4

temperatures. It can be clearly seen from Fig. 4 that the catalyst

treated at 300  C exhibited the best catalytic activity for the
hydrolysis of NaBH4 and achieved an average HG rate of
4.78 l min1 g1, which is much higher than those treated at
500  C (1.25 l min1 g1) and 700  C (0.246 l min1 g1). This
could be contributed to the size effect that the catalyst treated at
300  C gave the smallest particle size.

T-1 / [1000*K-1]
Fig. 5 (a) Effect of solution temperature on the average HG
rate measured after 20 min in 20 wt.% NaBH4 D 3 wt.%
NaOH solution containing 10.0 mg of 17.33 wt.% CoB/
MWCNT and (b) Plot of ln r versus 1/T according to the
original data as shown in Fig. 5a.

3.2.

Effect of solution temperature

The dependence of the HG rate on the temperature (2560  C)

was measured in 20 wt.% NaBH4 3 wt.% NaOH solution
containing 10.0 mg of the as-prepared CoB/MWCNT catalyst
and the results are presented in Fig. 5a. It is clear that the
average HG rate increases from 3.35 to 22.18 l min1 g1 with

Real-time HG rate / l min-1g-1Co-B

Average HG rate / l min-1 g-1 Co-B

6
5
4
3
2
1
0

20

40

60

80

100

Co-B loading / wt.%

Fig. 6 Relationship between CoB loading and the average
HG rate measured after 1 h running in 20 wt.%
NaBH4 D 3 wt.% NaOH solution containing 10 mg of CoB/
MWCNT.

Co-B/MWCNT
Co-B/C

Co-B

5
4
3
2
1
0
0

10

20

30

40

50

60

Time / min
Fig. 8 Steady-state performance of CoB supported on
different materials for hydrolysis of NaBH4 in 20 wt.%
NaBH4 D 3 wt.% NaOH solution containing 10 mg of
catalysts.

7114

international journal of hydrogen energy 33 (2008) 71107115

Table 1 Comparison of HG rates on various catalysts

Catalyst
Ru/IRA-400
Pt/XC-72 C
Pt/Al2O3
PtRuLiCoO2
Co/gAl2O3
CoB/C
CoB/C
CoB/MWCNTs

Initial solution
temperature for HG ( C)

NaBH4
concentration (wt.%)

NaOH
concentration (wt.%)

Average HG
rate (l min1 g1)

Reference

32.5
30
30
25
30
30
30
30

7.5
5
5
5
5
w0.8
20
20

1
5
5
5
5
w0.08
3
3

0.6
3.7
3.0
2.4
0.15
3.9
3.1
5.1

[3]
[25]
[25]
[26]
[27]
[18]
This paper
This paper

the solution temperature increasing from 25 to 60  C. The

following equation can be used to calculate the reaction rate:
 
E
(2)
r k0 exp
RT
where r is the reaction rate (mol min1 g1), k0 is the reaction
constant (mol min1 g1), E is the activation energy for the
reaction, R is the gas constant and T is the solution temperature. By plotting ln r versus 1/T based on the data in Fig. 5a,
a linear relationship is observed as shown in Fig. 5b. The
activation energy for the HG reaction was calculated from the
slope of the linear curve in Fig. 5b to be 40.40 kJ mol1, which is
lower than the reported value of 64.87 kJ mol1 on other
catalyst [16].

3.3.

Effect of catalyst loading

Fig. 6 shows the relationship between the CoB loading and

the HG rate. It is obvious that the HG rate increases with the
increase in the CoB loading up to 10 wt.%. However, the HG
rate tends to decrease with the further increase in the CoB
loading. The highest activity achieved is 5.12 l min1 g1 CoB.
The unsupported CoB exhibits the lowest activity due to
lowest dispersion degree.

3.4.

Effect of supporting material

MWCNTs and carbon as supporting materials were compared.

The acid treated MWCNTs or carbon supported CoB catalysts
were developed via chemical reduction of aqueous sodium
borohydride with cobalt chloride. Fig. 7 shows nitrogen
adsorption/desorption isotherm curves for CoB/MWCNT and
CoB/C. The pore size distribution of the CoB/MWCNT is
shown in the inset of the figure. The specific surface areas of
the CoB/MWCNT and CoB/C catalysts, calculated by the
BrunauerEmmettTeller (BET) equation, were 118 and
176 cm2 g1, respectively. The hysteresis on isotherm curve of
CoB/MWCNT is the evidence of the mesoporous structure
even the BET area is lower. The mesopore distribution peak is
located at 4.8 nm. In fact, the support with mesopores is more
useful than that of micropores used in liquid media due to the
liquid-sealing effect.
Fig. 8 compares the steady-state catalytic activities for the
NaBH4 hydrolysis on CoB/MWCNT, CoB/C and pure CoB
without support. The supported catalysts showed higher
activity than that of unsupported one due to the better
dispersion and higher surface area. It is further demonstrated
that the catalytic activity of mesoporous CoB/MWCNT is

higher than that of CoB/C since the mesoporous structure of

MWCNT allows to increase the active surface area. The
comparison of HG rate of CoB/MWCNT catalyst with other
catalysts is given in Table 1. Amendola et al. [3] reported that
IRA-400 supported Ru catalysts produced an average HG rate
of 0.6 min1 g1 catalyst. Ye et al. [25] found that the carbon
supported Pt and Al2O3 supported Pt gave HG rates of 3.7 and
3.0 l min1 g1 catalyst in 5 wt.% NaBH4 5 wt.% NaOH solution. It is also reported that the HG rates of 2.4 and
0.15 l min1 g1 on PtRuLiCoO2 and Co/gAl2O3 catalysts
[26,27]. Carbon supported CoB catalyst gave a HG rate of
3.9 l min1 g1 at very low concentration of 0.8 wt.% NaBH4
containing 0.08 wt.% NaOH [20]. In the present work, CoB/
MWCNT catalyst exhibits a higher average HG rate of
5.1 l min1 g1.

4.

Conclusions

CoB/MWCNT catalysts were prepared via the chemical

reduction of aqueous sodium borohydride with cobalt chloride for catalytic hydrolysis of NaBH4 solution. It is proved that
the use of MWCNTs as support is beneficial to the dispersion
of the CoB to increase the active surface area, resulting in
enhanced catalytic activity. The catalyst was mesoporous
structured and showed lower activation energy of
40.40 kJ mol1 for the hydrolysis of NaBH4. A high-accuracy,
low-cost and automatic HG rate measurement system was
developed based on the use of an electronic balance, which
has high accuracy of 0.002 FS%. The CoB/MWCNT catalyst
treated at 300  C exhibited the highest catalytic activity and
achieved the average HG rate of 5.1 l min1 g1 compared to
3.1 l min1 g1 on CoB/C catalyst in 20 wt.% NaBH4 3 wt.%
NaOH solution containing 10 mg catalyst at 30  C.

Acknowledgements
The work was financially supported by the Guangdong Sci. &
Tech. Key Projects (2007A010700001, 2007B090400032),
Guangzhou Sci. & Tech. Key Projects (2007Z1-D0051,
SKT[2007]17-11), Dongguan Sci. & Tech. Project (2005d029), the
NNSF of China (20676156), China National 863 Program
(2006AA11A141, 2007AA05Z124), the Chinese Ministry of
Education (307021) and the Chongqing Sci. & Tech. Key Project
(CSTC2007AB6012).

international journal of hydrogen energy 33 (2008) 71107115

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