Radiation Physics and Chemistry 89 (2013) 5156

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Radiation Physics and Chemistry

journal homepage: www.elsevier.com/locate/radphyschem

Synthesis of nickel nanoparticles on multi-walled carbon nanotubes

by gamma irradiation
Vivek M. Rao a, Carlos H. Castano b,n, Jessika Rojas b, Ahlam J. Abdulghani c
a

Department of Chemical and Biological Engineering, Missouri University of Science and Technology, 400 W. 11th St. Rolla, MO 65409, USA
Department of Mining and Nuclear Engineering, Missouri University of Science and Technology, 301 W. 14th St. Rolla, MO 65409, USA
c
Department of Chemistry, College of Science, University of Baghdad, Jaderiya, Baghdad, Iraq
b

H I G H L I G H T S

Nickel nanoparticles were deposited on multi-walled carbon nanotubes by gamma irradiation.

The effect of dose on size distribution of the nanoparticles was evaluated.

Between 30 and 60 kGy, as dose increases the average size of the nanoparticles decrease from 16 to 12 nm.

art ic l e i nf o

a b s t r a c t

Article history:
Received 7 September 2012
Accepted 2 April 2013
Available online 17 April 2013

Multi-walled carbon nanotubes (MWCNTs) were used as a substrate for nickel nanoparticles production.
Nickel nanoparticles of average sizes between 9 and 16 nm were synthesized by gamma irradiation of
aqueous solutions containing nickel sulfate or nickel chloride as precursors. MWCNTs were acid treated
and poly vinyl pyrrolidone (PVP, m44,000) or sodium dodecyl sulfate (SDS) were used as stabilizers.
Isopropanol was used as a scavenger of hydroxyl radicals, and deionized (DI) water as a solvent. Gamma
irradiation was carried out at room temperature and ambient pressure in a 60Co gamma source at doses
of 30, 40, 50, and 60 kGy. The nickel nanoparticles were characterized by transmission electron
microscopy (TEM), scanning transmission electron microscopy (STEM), and X-ray photoelectron spectroscopy (XPS). By controlling the dose and stabilizer's concentrations, nanoparticles with different sizes
were obtained. Poly vinyl pyrrolidone (PVP) was found to be more efcient at preventing coalescence of
Ni seeds than sodium dodecyl sulfate (SDS).
Published by Elsevier Ltd.

Keywords:
Nickel
Nanoparticles
Carbon nanotubes
Gamma-ray
Radiation induced chemistry

1. Introduction
Outstanding physical, chemical and electro-mechanical properties have brought carbon nanotubes (CNTs) to the forefront of
micro and nanotechnology ever since their discovery (Iijima, 1991).
Their high thermal conductivity in uid suspensions has uses in
enhancing industrial heat transfer efciency (Kamali and Binesh,
2010; Ding et al., 2006). CNTs have also been investigated for their
mechanical properties due to their low mass and high tensile
strength (tenfold that of stainless steel). The current energy crisis
and concerns with our environment have boosted our interest in
renewable and eco-friendly sources of energy. Hydrogen has been
considered a reliable and eco-friendly energy carrier for both
portable and stationary applications.
n

Corresponding author. Tel.: +1 573 341 6766; fax: +1 573 341 6309.
E-mail addresses: vmrgy5@mst.edu (V.M. Rao),
castanoc@mst.edu (C.H. Castano), jvr45d@mst.edu (J. Rojas),
ahlamjameel@scbaghdad.edu.iq (A.J. Abdulghani).
0969-806X/$ - see front matter Published by Elsevier Ltd.
http://dx.doi.org/10.1016/j.radphyschem.2013.04.006

Hydrogen, however, needs to be safely and reversibly stored to

be useful as an energy carrier. Carbon nanotubes are being studied
as hydrogen storage devices (Lipson et al., 2008). The DOE target
estimated for commercialization for hydrogen storage systems is
6.5 wt%. Adsorption of hydrogen by varying coverage on CNTs and
ip-in mechanisms for hydrogen atoms have been proposed to
increase hydrogen trapping capacities of CNTs (Park et al., 2005;
Lee et al., 2001). For pristine single walled CNTs, hydrogen storage
capacities have not exceeded 1 wt% due to weak CH bonding at
atmospheric pressure and 295 K. Hydrogen storage capacities have
been reported up to 6 wt% at cryogenic conditions (12 bar, 77 K),
but these conditions are not practical for commercialization
(Lawrence and Xu, 2004; Poirier et al., 2004; Pradhan et al.,
2002). Hydrogen uptake has been proven to be positively inuenced by the MWCNT diameter (Hao et al., 2003) and the presence
of metal catalysts (Lipson et al., 2008).
Hydrogen is known to form hydrides readily with many
transition and noble metals (Fukai and Sugimoto, 1985). Choosing
the right metal is expected to improve the hydrogen storage

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V.M. Rao et al. / Radiation Physics and Chemistry 89 (2013) 5156

capacity of a nanomaterial. Reported electrochemical loadings of

hydrogen on CNTs encapsulated in a Pd matrix, resulted in 812 wt%
hydrogen absorption. The mass of the substrate used (Pd), however,
countered the increased hydrogen storage capacity (Lipson et al.,
2008). Decoration of CNTs with titanium was predicted to store 8 wt
% hydrogen (Yildirim and Ciraci 2005) but experimental work has
reported much lower values (Brieno-Enriquez et al., 2009; Rather
et al., 2009). Platinum nanoparticles dispersed on CNTs are predicted to cross the DOE requirements at extremely high pressures
(Park and Lee, 2010). Nickel has long been known for its hydrogen
catalytic properties. Nickel nanoparticles have been coated on CNTs
by thermal evaporation (Bittencourt et al., 2007), and electroless
deposition (use of a redox reaction to deposit metal on a substrate
without the passage of an electric current) (Chen et al., 2010).
Impregnating CNTs with varying amounts of nickel have shown up
to 2.8 wt% hydrogen storage capacity (Kim et al., 2005). Nickel has
also been studied for surface or subsurface hydride formations by
electrochemical methods, which differs from conventional threedimensional bulk hydride formations (Baranowski, 1999).
Our objective is to produce a nanocomposite structure
(MWCNT- Ni matrix) that can enhance the hydrogen storage
capacities of pristine nanotubes by utilizing the nickel hydride
formation to form a link between the CNT walls and hydrogen
atoms (similar to Lipson et al., 2008). This work presents the
synthesis of nickel nanoparticles adsorbed on MWCNTS using a
60
Co gamma source in aqueous solutions containing MWCNT, a
nickel precursor salt, a stabilizer, and isopropanol as a hydroxyl
scavenger. The resulting nanostructures were characterized with
STEM, TEM, and XPS.

and were then purged with a stream of argon for 1 h to evacuate

the oxygen. Each vial with a designated concentration of SDS and
PVP was then irradiated by a 60Co gamma source at doses of 30,
40, 50, and 60 kGy, respectively. Blank samples were also prepared
in parallel to test the formation Ni nanoparticles in identical
conditions but in absence of gamma irradiation.
2.3. Apparatus
FTIR spectra of MWCNTs before and after treatment with nitric
acid were recorded on a Nicolet NE X US470 FTIR spectrophotometer in the region 4004000 cm1 using KBr pellets. The
morphology of Ni nanoparticles deposited on MWCNTs was
characterized and their sizes and distribution were studied by
using a Helios Nanolab 600 FIB scanning transmission electron
microscope (STEM) and transmission electron microscope (TEMTechnai F20). Scanning transmission electron microscope (STEM)
mode was also used to obtain the energy dispersion X-ray spectra of
Ni nanoparticles. Binding energies and detection of nanostructures
Ni/MWCNTs were studied by X-ray photoelectron spectroscopy
(XPS) using a KRATOS AXIS 1 65-X-ray photoelectron spectrometer.
Degassed samples were irradiated in a Gamma Cell 220 Excell 60Co
irradiator (MSD NORDION 447 Ontario Canada), dose rate 10 KGy/h
with a cylindrical irradiation chamber of 152 mm diameter and
203 mm height.

3. Results and discussion

3.1. FTIR spectra

2. Experimental
2.1. Chemicals
The chemical nickel precursors used in this work were nickel
chloride hexahydrate (NiCl2.6H2O) or nickel sulfate hexahydrate
(NiSO4  6H2O). MWCNTs with 320 nm outside diameter, 13 nm
inside diameter, 0.110 m long were used as substrate for
deposition of Ni nanoparticles. PVP with m44,000 and SDS were
used as stabilizers, and isopropanol (99%) as a scavenger of
hydroxyl radicals. All chemicals were purchased from Alfa-Aesar.
Purication and functionalization of MWCNTs were done by
surface oxidation reaction using concentrated nitric acid (15.6 M,
65% v/v) from Acros Organics. In a typical experiment, a suspension of MWCNTs in HNO3 (1 mg/ml) was ultrasonicated for 30 min
to eliminate agglomeration of CNTs. The mixture was then heated
in a round bottom ask tted with a reux condenser at 80 1C for
2 h in a water bath with continuous stirring. The resulting solution
was cooled to room temperature, and the removal of acid layer
was done by successive dilution with DI water followed by
centrifugation until the pH of washing water was approximately
5. After decantation of the supernatant solution, the MWCNTs
were dried overnight at 80 1C.

The FTIR spectra of as-prepared and oxidized MWCNTs are

compared in Fig. 1. The immediate distinction between these two
spectra is the difference in the peak intensities. It is recognized that
treatment with nitric acid increased intensities of the main absorption
peaks exhibited by the two samples at 1062, 1406, 1656, 2938 and
3468 cm1 corresponding to stretching vibrations of COH, CO (and
OH in-plane deformation of sorbed water), CO, CH and OH groups
(Stobinski et al., 2010). This indicates the removal of catalytic metallic
impurities from the binding sites of MWCNTs by surface oxidation. The
spectrum of the acid treated MWCNTS exhibited additional absorption
peaks appeared at 1250, 1530, 1765, 2355, and 2531 cm1 which refers
to further functionalization of MWCNTS by chemical oxidation with
nitric acid (Stobinski et al., 2010). The peak observed at 1250 cm1 may
be assigned to OH deformation and CO stretching combination in
surface phenols and aromatic carboxylic acid (Stobinski et al., 2010),
while that at 1530 cm1 is assigned to stretching modes of aromatic
CC bonds associated with the backbone of treated nanotubes

2.2. Preparation of Ni/MWCNT nanomaterial

Small scale batches for the synthesis of Ni nanoparticles/
MWCNTs by gamma irradiation were prepared as follows: Solvent
mixture of DI water and isopropanol in a volume ratio of (2:1)
respectively containing a nickel salt (5  103 M), and three different concentrations of each surfactant (SDS: 0.05 M, 0.07 M, 0.1 M
and PVP: 0.1 mM, 0.3 mM, 0.5 mM were distributed in into small
(1 ml) glass vials. To each 1 ml was added 1 mg MWCNTs. The
resulting mixtures were ultrasonicated for 60 min to enhance
complete dispersion of reactants within the aqueous solution

Fig. 1. FTIR spectra of as obtained MWCNTs before (a) and after (b) reux with
nitric acid for 2 h at 80 1C.

V.M. Rao et al. / Radiation Physics and Chemistry 89 (2013) 5156

(Stobinski et al., 2010; Rojas and Castano, 2012). The bands observed at
1765 and 2530 cm1 were attributed to stretching modes of additional
carboxylic groups while the peak at 2355 cm1 can be associated with
the OH stretching vibration of strongly hydrogen-bonded COOH
groups (Stobinski et al., 2010).
3.2. Preliminary synthesis and characterization of Ni/MWCNTs
nanocomposites
Radiolysis of water with gamma radiation leads to the formation of reactive species such as hydrated electron (e aq.), hydroxyl
radical (OH), and hydrogen radical(H) H3O+, H2O2, and H2. The

53

normally accepted values of product yields are well known

(Parajon et al., 2008; Appleby and Schwarz, 1969). These species
play an important role in the reduction of metal atoms in this case,
from Ni+2 to Ni0. The hydrated electrons (e aq.) and hydrogen
radicals (H) are strong reducing agents and can reduce Ni2+ ions
into neutral Ni0 atoms in a two step process similar to other
divalent metal atoms (Belloni et al., 1998). On the ipside, hydroxyl radicals (OH) tend to strongly oxidize Ni0 back to Ni+2 ions.
To prevent this oxidation, isopropanol is introduced into the
reaction medium as a scavenger for hydroxyl radicals (Belloni
et al., 1998; Michealis and Henglein, 1992). The OH radicals can
react with isopropanol molecules during and after irradiation to

Fig. 2. STEM and TEM micrographs of nickel nanoparticles adsorbed on MWCNTs with (a) 0.07 mM SDS and (b) 0.5 mM PVP samples irradiated with a dose of 40 kGy from a
60
Co gamma source.

Fig. 3. STEM micrographs of the same nickel samples of (a) SDS (0.07 mM) and (b) PVP (0.5 mM ) surfactants 30 days after 40 kGy gamma irradiation showing no nickel
nanoparticles on MWCNTs in the former, while the Ni nanoparticles still remaining on the MWCNTs in the latter.

Fig. 4. STEM micrographs of nickel chloride samples irradiated with (a) 40 kGy (b) 50 kGy and (c) 60 kGy absorbed dose using PVP (0.5 mM) as a stabilizer. At higher doses a
higher population of Ni nanoparticles was adsorbed on MWCNTs. (c) also shows a layer of PVP well dispersed over the nanoparticles and MWCNTs.

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V.M. Rao et al. / Radiation Physics and Chemistry 89 (2013) 5156

Fig. 5. Particle size distribution and nickel nanoparticles populations in nickel chloride and PVP (0.5 mM) samples irradiated with (a) 30 kGy (b) 40 kGy (c) 50 kGy
(d) 60 kGy gamma radiation doses.

Table 1
Average particle sizes and variation with intensity of radiation.
Intensity of radiation
(kGy)

Average particle size

(nm)

Standard deviation
(nm)

30
40
50
60

16.61
16.04
13.65
11.97

7 3.5
7 1.7
7 2.1
7 2.4

form reducing isopropanol radicals which react with metal ions to

form long lived clusters zero-valent metal atoms M0 (Belloni,
2006; Rojas and Castano, 2012). Nickel is an example of nonnoble metals whose monomers and oligomers are quite fragile to
corrosion by the solvent. Thus the presence of OH scavengers is
crucial for the formation of long-lived clusters (Belloni et al., 1998).
Once formed, nano-sized nickel colloids tend to agglomerate easily
into large particles and settle out of solution. In addition to van der
Waals attractive forces, nickel colloids possess additional magnetic
attraction (Chou and Huang, 2001). The magnetic Ni nanocrystals
have very large surface areas, and also have very high surface
energy. As a result, they will be very reactive with oxygen and
water, forming nickel oxides (Yan et al., 2009). In order to prevent
agglomeration, surfactants or dispersants such as anionic surfactant sodium dodecyl sulfate (SDS) or a polymerpoly vinyl
pyrrolidone (PVP) were used as stabilizers. Fig. 2(a) and (b) show
the electron micrographs of Ni/MWCNTs nanocomposites

synthesized by gamma irradiation at 40 kGy using SDS and PVP,

respectively. Repeated STEM analysis after 30 days for SDS treated
samples showed no presence of Ni nanoparticles on MWCNTs in
contrast to what was observed with the samples stabilized by PVP.
This indicates that SDS had weak interactions with the Ni
nanoparticles leading to their oxidation and agglomeration while
PVP had stronger interaction with both the metal nanoparticles
and functionalized MWCNTs compared to SDS. Fig. 3(a) shows a
settlement of SDS on the outer walls of the MWCNTs, conrmed by
EDS spectra of the outer wall. PVP has N and O atoms in its
heterocyclic ve membered ring moiety which can associate with
the nickel atom on the surface of the crystal while the long chains
of PVP stretch out around, causing a steric hindrance effect that
depresses the collision between nickel crystals and thus prevent
the growing of particles effectively and decreased their surface
energy (Hussain and Haque 2010). By their high dispersion power,
the strongly adsorbed PVP molecules were capable of protecting Ni
nanoparticles from agglomeration and from oxidation for 30 days,
as is shown in Fig. 3(b). According to these preliminary results, PVP
was selected for further experiments.
Attempts to deposit nickel nanoparticles on MWCNTs by
adsorption using nickel sulfate as a metal precursor was less
successful compared with nickel chloride. This may be attributed
to the lower solubility of nickel sulfate in aqueous solution (44.4 g/
100 ml) which makes the synthesized reactive Ni nanoparticles
become more susceptible to oxidation forming nickel ions and
nickel oxide, or to agglomeration before being adsorbed on CNTs.
Furthermore it was reported that reducing agents such as hydrogen required for synthesis of nickel nanoparticles from nickel

V.M. Rao et al. / Radiation Physics and Chemistry 89 (2013) 5156

55

sulfate were twice that required for nickel chloride (Joseph et al.,
2011) as is shown in the following equations
NiCl2+H2 (g)-Ni+2HCl (g)
NiSO4+2H2 (g)-Ni+SO2 (g)+2H2O
Nickel chloride was accordingly chosen for further experimentation and analysis.
3.3. Synthesis of Ni/MWCNTs by gamma irradiation at different
doses using nickel chloride as a precursor and PVP as a stabilizer
Based on the preliminary characterization, the experiments
were repeated with doses of ionizing radiation at 30, 40, 50, and
60 kGy using nickel chloride hexahydrate as the source of nickel
ions and PVP as a stabilizer. The samples were prepared and
irradiated as before, and the results of STEM analysis are shown in
Fig. 4.
All three irradiated nickel chloride samples showed high
population of nickel nanoparticles with average sizes of 913 nm
adsorbed on MWCNTs which indicates that the functionalized
MWCNTs provided active sites for adsorption of nickel atoms/
clusters. At higher doses, higher yields and more attachment of
nanoparticles to the MWCNTs took place. Fig. 5 shows the particle
size distributions of Ni nanoparticles supported by MWCNTs at
each dose of gamma radiation. No marked reduction in the
average particle size was observed for samples irradiated at
30 kGy compared with those irradiated at 40 kGy, while there
was a 50% reduction in standard deviation, followed by a more
signicant reduction in average particle sizes for samples irradiated at doses of 50 and 60 kGy, respectively. Table 1 lists the
average particle sizes and their corresponding standard deviations
obtained at each dose. The variation of average particle size with
absorbed dose is shown in Fig. 6 evidencing a decrease in the size
of nickel nanoparticles on MWCNTs with increasing dose.
Varying the PVP concentration (o1 mM) showed insignicant
effects. Since nickel nanoparticles were adsorbed on MWCNTs
even at 30 kGy of gamma irradiation, the concentrations of PVP
employed proved sufcient to retain the nanoparticles in their Ni0
state. These results indicate that PVP serves as a good linker

Fig. 7. XPS analysis of Ni/MWCNT nanocomposite (a) Ni peak (b) C peak.

between the Ni nanoparticles and functional groups present on

the oxidized CNT surface. This linking may take place through
interaction of N and O atoms of PVP ring with the formers and
through weak intermolecular interactions (such as stacking,
hydrophobic or electrostatic attractions) with latters (Georgakilas
et al., 2007). The absence of Ni nanoparticles on some MWCNTs in
the STEM images is attributed to a lack of active sites on their
surfaces.
Fig. 7(a) and (b) show the XPS analysis of the Ni-CNT nanocomposite. Fig. 7(a) shows a relatively low intensity Ni 2p3/2 peak
at 852.6 eV compared to the NiO peak at 853.8 eV. Since the NiO
peak is sharper, it is suggested that the reduction of Ni+2 to Ni0 is
accompanied by the possible bonding between nickel and oxygen.
Fig. 7(b) shows that carbon has peaks at 284.6 V (1s) and 285.3 eV
(carbonyl CO). The carbonyl CO peak arises from the functionalized
sites of MWCNTs. In the absence of data for NiC peak, we believe
the adsorption of nickel on MWCNTs is through a NiOMWCNT
bond. The NiO bond is weaker as compared to the CO bond,
indicated by the higher free energy of the former.

4. Conclusions

Fig. 6. The variation of average particle size (nm) with absorbed gamma
doses (kGy).

Nickel nanoparticles with average sizes of 913 nm were

successfully synthesized and deposited on carbon nanotubes
induced by gamma radiation at doses 30, 40, 50, and 60 KGy using
nickel chloride as a metal precursor, PVP as a stabilizer and
isopropanol as hydroxyl radical scavenger and DI water as a
solvent. Increasing the dose of gamma radiation caused a reduction in average particle size. Lower concentrations of nickel salt are

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V.M. Rao et al. / Radiation Physics and Chemistry 89 (2013) 5156

desirable in order to prevent agglomeration and to ensure

complete adsorption of nickel atoms on MWCNTs. Preliminary
characterization proved PVP as a more suitable stabilizer for nickel
nanoparticles than SDS. Varying the PVP concentration (o1 mM)
yields insignicant effects. The physical obstruction provided by
PVP restricts both: oxidation of nickel nanoparticles before being
adsorbed on MWCNTs and desorption of nickel atoms from
MWCNTs and subsequent agglomeration of nickel nanoparticles.
Functionalization of MWCNTs by nitric acid provided active sites
for adsorption of Ni0 nanoparticles. The reaction conditions such
as the type of stabilizer used (surfactant, polymer) functionalization of carbon nanotubes, metal precursor salt, secondary alcohol
and their concentrations as well as absorbed dosage are all
important factors in dictating the stability of synthesized nanocomposites (Rojas and Castano, 2012). Optimum conditions for
producing higher yields of smaller Ni nanoparticles (o10 nm),
will require to take all these factors into consideration.
Acknowledgements
This work was partially supported by NRC Grant NRC-38-10966512. The authors would like to specially thank Dr. Stoyan
Toshkov for providing the irradiation services at the University
of Illinois at Urbana Champaign and Dr. Kai Song, Sr. Research
Scientist, Missouri University of Science & Technology for technical
assistance with electron microscopy.
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