Journal of Alloys and Compounds 419 (2006) 32–39

Synthesis and magnetic characterization of Ni nanoparticles and Ni

nanoparticles in multiwalled carbon nanotubes
Daniele Gozzi a,∗ , Alessandro Latini a , Gustavo Capannelli b , Fabio Canepa c ,
Myrta Napoletano c , Maria Roberta Cimberle d , Matteo Tropeano e
aDipartimento di Chimica, Università di Roma La Sapienza, Piazzale Aldo Moro 5, 00185 Roma, Italy
b INSTM and Dipartimento di Chimica e Chimica Industriale, Via Dodecaneso 31, 16146 Genova, Italy
c INFM-LAMIA and Dipartimento di Chimica e Chimica Industriale, Via Dodecaneso 31, 16146 Genova, Italy
d CNR-IMEM Dipartimento di Fisica, Via Dodecaneso 33, 16146 Genova, Italy
e INFM-LAMIA, C. so Perrone, Genova, Italy

Received 15 September 2005; received in revised form 10 October 2005; accepted 14 October 2005
Available online 21 November 2005

Abstract
Nickel nanoparticles were synthesized by reduction of nickel acetylacetonate in a monosurfactant system. These nanoparticles, mostly amorphous,
were used as catalyst for the growth of multiwalled carbon nanotubes by the catalytic decomposition of methane at 500 ◦ C. TEM analysis reveals
a wide size distribution of the diameter of the particles centred around two main values. A detailed characterization of the magnetic properties of
the Ni nanoparticles and Ni nanoparticles carbon nanotubes embedded is hereby presented. Both the systems show superparamagnetic behaviour
above the blocking temperature TB . Magnetization data are well fitted by an equation formed by two weighted Langevin functions and display the
correct scaling of M/MS versus H/T for superparamagnetic nanoparticles. The hysteresis loops obtained below TB agree with the ferromagnetism
of single-domain particles, confirmed also by the expected temperature dependence of the coercive field HC . Differences in the coercive fields at
increasing and decreasing applied magnetic fields are to be ascribed to a NiO layer originating an exchange bias with inner Ni. The smallness of
the coercive fields difference (around 5 Oe) confirms that the used preparation method produces a very thin NiO layer around Ni nanoparticles.
© 2005 Elsevier B.V. All rights reserved.

PACS: 61.46.+w; 75.20.−g; 75.50.Tt

Keywords: Carbon nanotubes; Magnetic properties; Catalytically grown carbon

1. Introduction systems and silent rooms to wireless communications has been

increased.
The synthesis and chemico–physical characterization of Different techniques have been adopted to obtain ferromag-
elements as Fe, Co or Ni in nanometric scale is nowadays netic elements with nanometric dimensions: arc discharge [5],
an important topic in materials science not only for their evaporation [6], sputtering [7] and sonochemical method [8].
peculiar properties related to the reduced size but also for their However, the high surface to mass ratio has the consequence
relevance from a technological point of view. Possible potential to increase enormously the reactivity of the nanoparticles that
applications of the nanostructured materials as catalysts (high could prevent their technological use. Therefore, the coating of
value of the surface area), high-density magnetic recording these magnetic nanoparticles by protective layers or the syn-
media and medical diagnostics have been recently emphasized thesis of magnetic particles in carbon capsules has a particular
[1–3]. More recently [4], the use of composites with nano- interest since it can prevent any kind of reaction, particularly the
sized ferromagnetic particles as absorbers of electromagnetic oxidation, provided the temperature is kept close to the room
waves for technological applications starting from radar temperature.
Finally, magnetic nanoparticles can be used as origin for the
growth of carbon nanotubes. This is a new form of carbon config-
∗ Corresponding author. Tel.: +39 06 4991 3849; fax: +39 06 4991 3849. urationally equivalent to two-dimensional graphene sheet rolled
E-mail address: Daniele.Gozzi@uniroma1.it (D. Gozzi). into a tube and can offer amazing possibilities to create future

0925-8388/$ – see front matter © 2005 Elsevier B.V. All rights reserved.
doi:10.1016/j.jallcom.2005.10.012
 D. Gozzi et al. / Journal of Alloys and Compounds 419 (2006) 32–39 33

nanoelectronics devices, circuits, and computers through further of the complete substitution of Ar with CH4 also amu = 40 was added to the
circuitry integration. previous set.
We prepared either Ni nanoparticles, mostly in the amor- After about 16.9 h from the Ar/CH4 substitution, the reactor was cooled
down to room temperature at 300 ◦ C/h keeping still the same CH4 flow-rate. The
phous state, and carbon nanotubes embedding Ni nanoparticles final mass gain,
m, entirely attributable to the formation of MWCNTs, was
using the Ni nanoparticles as “seeds” for the growth of carbon 0.06347 g. The solid reaction product was recovered from the reactor, washed
nanotubes (randomly oriented). We present, here, the informa- thoroughly with NaOH ∼2 M to remove the silica support, then with deionised
tion obtained on these two systems by transmission electron water and acetone and finally dried under vacuum. The combustion analysis of
microscopy (TEM) and magnetic measurements as well as some MWCNT recovered gave: C = 95.4 ± 0.3%, H = 0.2 ± 0.1% and Ni up to 100,
i.e., cNi = 4.4 ± 0.3%.
experimental evidences on the multiwalled carbon nanotubes, The structural investigation was carried out by means of transmission elec-
MWCNT, growth. tron microscope (TEM) model JEOL JEM 2010 FEEM 200 KV from JEOL Ltd.
The samples for TEM analysis were firstly finely dispersed in isopropanol and,
2. Experimental then, exposed to ultrasonic vibrations to decrease the aggregation. The diam-
eter distribution has been evaluated over more than 1000 particles. X Pert Pro
Ni nanoparticles were synthesized according to the method developed by diffractometer by Philips, working at Cu K␣1 wavelength, was utilized for XRD
Hou and Gao [9], i.e., by reducing Ni acetylacetonate by NaBH4 in a mono- analyses.
surfactant system. The combustion and ICP (Ion Coupled Plasma) analyses Magnetic measurements were performed using a Quantum Design SQUID
of the product after centrifugation and vacuum drying gave the composition: MPMS magnetometer in the 5–350 K temperature range and in applied µ0 H
C = 5.8 ± 0.3; H = 1.0 ± 0.1; N = 0.4 ± 0.1; Ni = 4.6 ± 0.1 and inorganic inert magnetic fields between ±5.5 Tesla (T). Additional magnetization measure-
residuals up to 100. All the figures are given by wt.%. The catalyst for the ments up to 9 T were obtained by a Maglab2000 equipment (extraction method)
growth of MWCNTs was prepared through a dispersion of the Ni nanoparticles from Oxford Instruments Inc.
over high surface area (960 ± 1 m2 g−1 ) MCM-41 mesoporous silica. To do this
0.18371 g of the synthesized material, i.e., 0.0084 ± 0.0002 g of Ni nanopar-
3. Results
ticles were suspended in 30 ml of n-hexane and 0.55098 g of MCM-41 silica
were soaked in the suspension under stirring at room temperature. The stir-
ring was continued until the surfactant liquid became transparent. Then, the 3.1. Kinetics of MWCNT growth
temperature was gently raised up to about 70 ◦ C and kept constant until to the
solvent full evaporation. The solid catalyst was recovered and dried under vac- The ionic intensities of the amu set acquired by the QMS is
uum. Thus, the Ni nanoparticle concentration, ccat , in the catalyst dispersion is
reported in Fig. 2. On the left scale are reported the amu of CH4
1.5 ± 0.4 wt.%.
The quantity, q, of 0.15548 g of Ni nanoparticle dispersion in MCM-41 silica (amu = 16) and its fragments as well as amu = 40, i.e., Ar. The
was placed in a fixed bed catalytic micro reactor (Fig. 1). The catalyst was heated ionic intensity of H2 is reported on the right scale. The origin of
up to 500 ◦ C at 300 ◦ C/h in an Ar stream. When at 500 ◦ C, Ar was substituted the time scale is fixed at the time when the valve of Ar becomes
by CH4 at 5 cm3 min−1 at STP. The kinetics of reaction: off and the valve of CH4 is opened (see Fig. 1). At the time
CH4 (g) → C(nano) + 2H2 (g) (1) origin the micro reactor is already at 500 ◦ C. The time at which
the catalyst sees CH4 without Ar is the time corresponding to
was monitored by a Balzers Quadstar© quadrupole mass spectrometer, QMS, the disappearing of Ar signal. This occurs at time t* . When the
operating in multiple ion detection, MID, mode. The admission of the reacted gas
system is cooled down at room temperature, the rate of reaction
mixture into the QMS chamber was realized by a system (see Fig. 1) constituted
by a stainless steel capillary (1 m long × 150 ␮m i.d.), a rough vacuum pumping (1) goes rapidly to zero and, accordingly, the ionic intensities
and a dosimeter valve (Balzers UDV 040). The capillary was maintained at related to methane and hydrogen change with opposite trends,
150 ◦ C and at fixed pressure gradient (1 bar rel. at the inlet and 1 mbar at the as expected. The final ionic intensity of H2 cannot be zero it
outlet). Methane utilized was 97.5% with 2.5% of H2 . being the main impurity of CH4 used.
Because from preliminary experiments it was confirmed that only reaction
(1) takes place, only amu corresponding to CH4 (and its fragments CH3 , CH2 ,
CH, C) and H2 were set for the MID detection. In order to establish, the time

Fig. 2. Ionic intensities from QMS during the MWCNT growth. Time t* is the
Fig. 1. Schematic view of the experimental assembly for MWCNT growth. time at which Ar is completely replaced by CH4 .
34 D. Gozzi et al. / Journal of Alloys and Compounds 419 (2006) 32–39

Fig. 3. TEM of Ni nanoparticle after preparation.

3.2. XRD and TEM

Fig. 5. (A) TEM micrograph of MWCNTs with Ni nanoparticle embedded. A
tip shape nanoparticle attached to a MWCNT is shown in the inset. (B) XRD
In Fig. 3, a typical HREM image of Ni nanoparticles is spectrum of Ni-MWCNTs at Cu K␣1 radiation. Lines of a reference graphite
reported, while in Fig. 4 the size distribution histogram of the syn and fcc Ni are from PCPDFWIN version 2.2, June 2001 data base (ICPDS-
Ni nanoparticles is presented. This figure displays a wide distri- ICDD), respectively, #87-0712 and #75-1621.
bution of particle diameters centered around two main values:
about 70% of the particles has a diameter of about 5 nm, while
only about 25–30% of the particles present a diameter between a double Gaussian function, reported as dot line in the same
10 and 20 nm. This bimodal distribution has been fitted with Fig. 4: we obtain two mean diameters of the particles, namely
d1 = 4.6 nm and d2 = 15.4 nm.
The XRD spectrum of the Ni nanoparticles displays no peaks
originating from the face-centred cubic (fcc) Ni structures show-
ing that a great part of Ni is in the amorphous state. Only peaks
due to the inert inorganic residuals coming from the synthesis
appear.
Ni nanoparticles embedded in MWCNTs are shown in
Fig. 5A. Each MWCNT carries at one of its ends a Ni nanopar-
ticle. The analysis of the distribution of Ni nanoparticles in
MWCNTs, not reported here, gives the same bimodal result.
Differently from the Ni nanoparticles, the XRD spectrum of Ni-
MWCNTs, reported in Fig. 5B, shows clearly the fcc features of
the Ni nanoparticles linked to MWCNTs, as well as the typical
finger print of a hexagonal graphite structure. The comparison
with one of the closest spectra reported in the ICPDS data base
gives the indication that the graphene planes in MWCNTs, d0 0 2
spacing, are separated 75 pm more than graphite assumed as ref-
Fig. 4. Size distribution histogram of Ni nanoparticles as obtained from the erence. The presence of Ni features that appear as weak signals,
TEM analysis. because Ni concentration is low, but in the expected intensity
 D. Gozzi et al. / Journal of Alloys and Compounds 419 (2006) 32–39 35

Fig. 6. Temperature dependence of the magnetization of: (a) Ni nanoparticles and (b) Ni nanoparticles in MWCNT obtained at 5 and 50 mT.

pattern, confirms that the transition amorphous/crystalline at

the temperature of the CH4 decomposition has been promoted
during the heating of the Ni nanoparticles. The absence of no
preferential orientation suggests that transition leads only to
polycrystalline nanoparticles.

3.3. Magnetic measurements

Fig. 6 shows the temperature dependence of the magnetiza-

tion between 5 and 300 K of the Ni nanoparticles (a) and Ni
nanoparticles in carbon nanotubes (b), respectively. The data
were taken in zero-field-cooling (ZFC) and field-cooling (FC)
conditions at two different applied magnetic fields, i.e., 5 and
50 mT. ZFC and FC curves show a bifurcation that decreases at
increasing magnetic fields. Furthermore, the ZFC curves show
a large decrease of the magnetization: this decrease, quite evi-
dent in Ni nanoparticles, is less strong in nano Ni in MWCNT
(note in Fig. 6, the behaviour of ZFC curve at 50 mT where the
magnetization is nearly constant below the bifurcation point).
This last behaviour may be due to weak magnetic interactions
in the system as we will discuss in the following. We observe
also that the magnetization values for Ni nanoparticles are lower
with respect to the values of nano Ni in MWCNT in the same
field and temperature conditions.
In the low temperature regime, the Ni nanoparticles and Ni
nanoparticles in MWCNT show hysteretic behaviour like ferro-
magnetic systems: the hysteresis loops at different temperatures
have been performed after a ZFC procedure and with a thin field
span (≤1 mT) up to 0.011 T. They are presented in Fig. 7a and b,
respectively. For Ni nanoparticles, we observe hysteresis loops
decreasing at increasing temperature with relatively low values
of the magnetization (4 emu/gNi at 0.2 T and 5 K). Once closed,
the magnetization doesn’t saturate, but increases continuously
with a slope, which depends on the applied temperature. On the
contrary, Ni nanoparticles in MWCNT display larger hysteresis Fig. 7. Magnetization loops of: (a) Ni nanoparticles and (b) Ni nanoparticles in
loops saturating at relatively high values (12 emu/gNi at 0.4 T MWCNT at selected temperatures.
36 D. Gozzi et al. / Journal of Alloys and Compounds 419 (2006) 32–39

amount of CH4 converted in MWCNT. Therefore, some facts

should be taken into account: (i) constant response uncertainty
of QMS on long times especially when considering low ionic
intensity values like that in the case of H2 ; (ii) H2 is already
present in CH4 ; (iii) variable composition occurring before t* .
In the previous reasoning, we assumed that all carbon produced
grows as MWCNTs. This agrees well with TEM analysis. There-
fore, to evaluate quantitatively the conversion, η, of methane in
MWCNT, equation below has been used:


iH2 /2fH2
η = 4 × 100
0 iCHi /fCHi + iH2 /2fH2 T


iH2 /2fH2
− 4 × 100 (2)
0 iCHi /fCHi + iH2 /2fH2 T room

where i and f stand, respectively, for ionic intensity and calibra-

tion factor. The second term on the right side of Eq. (2) represents
the apparent conversion at room temperature due to the H2 con-
tent in the feeding methane. The summation is extended to all
the ionic species of CH4 measured by QMS. Data calculated
through Eq. (2) are plotted in Fig. 9. By comparing Fig. 9 with
Fig. 2, it appears clear that there is a time interval, after t* , and
lasting until t0 , during which the slope of iH2 decreases. This
could be attributed to some consumption of H2 by the catalyst.
At this stage, it is difficult to establish the real process or pro-
cesses occurring. It is reasonable to associate this phenomenon
to both the reduction of some NiO, coating the Ni nanoparticles,
and chemisorption and/or absorption of H2 by the nanoparticles
themselves.
The ratio, γ, between the weight, w, of Ni consumed by the
embedding in MWCNTs and quantity, w0 , of Ni in the catalyst
dispersion q is given by:
w cNi
m
γ= = ≤1 (3)
Fig. 8. Normalized magnetization (M/MS ) as a function of H/T for Ni nanopar- w0 ccat q
ticles (a) at T = 270, 300 K and for Ni nanoparticles in MWCNT (b) at T = 250,
300 K. For both plots, the solid line is the fit with a weighted sum of two Langevin In the present experiment, γ = 1.2 ± 0.5. The large value of the
functions, as described in the text. error comes from the calculation of the absolute maximum error
using the respective errors on cNi and ccat . In practice, γ can be
considered close to 1. This leads at least two considerations: (a)
and 5 K) and showing no temperature dependence. Also, the
remanent magnetization (MR ) and the coercive field (HC ) are
larger for nano Ni in MWCNT with respect to Ni nanoparticles
in the same temperature conditions.
High temperature magnetization data normalized to the sat-
uration magnetization MS , are reported as a function of the H/T
ratio together with the Langevin fit of the data in Fig. 8a and b,
respectively.

4. Discussion

4.1. MWCNT growth

Assuming that the observed experimental curves reported in

Fig. 2 are only due to reaction (1), the growth rate of MWCNT
would be simple proportional to the ionic intensity of H2 . This is
true even if being approximate in order to evaluate correctly the Fig. 9. Conversion of methane in MWCNT as function of time.
 D. Gozzi et al. / Journal of Alloys and Compounds 419 (2006) 32–39 37

practically, all the Ni nanoparticles into the MCM-41 dispersion

are suitable to allow the growth of MWCNT. In fact, looking
at Fig. 9, it appears clear that before stopping the reaction the
rate of CH4 conversion, i.e., MWCNT formation rate, is already
decreasing; (b) in contrast, the low value of η indicates that a
large number of preferential paths are expected to be formed
in the catalytic bed of the microreactor due to the high specific
volume of MWCNT produced during the reaction progress.
It has been shown [10] that using a catalyst of different chem-
ical nature and micrometer sized, MWCNT growth occurs on
self-generated tip-shaped single crystal nanoparticles. In the
present case, looking at Fig. 5, it appears clear that most of
the Ni nanoparticles are round shaped except for a few excep-
tions as reported in the inset of same Fig. 5. As stated before
(see Section 3.2), no evidence here exists that a MWCNT grows
on a single crystal catalyst nanoparticle. It could be inferred
that a different growth mechanism is at working here though
the main chemical process (CH4 catalytic decomposition) and
experimental conditions are exactly the same.

4.2. The low T magnetic properties of Ni nanoparticles and

nano Ni in MWCNT
Fig. 10. High field hysteresis loop of Ni nanoparticles at 5 K.
The starting point for the analysis of the magnetic proper-
ties of the two systems, i.e., Ni nanoparticles and nano Ni in
carbon nanotubes, is the observation of their common super- Fig. 7b), on the contrary, below the blocking temperature, behave
paramagnetic behaviour in addition to the analysis of the mag- like a ferromagnetic system: a saturation is reached and the tem-
netic differences between crystalline and amorphous magnetic perature has low or null effect.
nanoparticles. A small difference between HC− and HC+ , i.e., the coercive
Magnetic nanoparticles behave like single domain particles fields obtained with decreasing and increasing applied magnetic
depending on the size of the particle: on the basis of the magnetic fields, is observed in both systems at all the measured tempera-
domain theory [11,12], the critical radius is strongly related to tures. This difference may be attributed to the existence of a very
the saturation magnetization of the material, its exchange con- narrow NiO layer around the Ni particle, which can create an
stant and anisotropy constant. So, it is possible to calculate it exchange bias between ferromagnetic Ni and antiferromagnetic
and for Ni the value is RC = 21.3 nm. In the amorphous state, a NiO [14]. In our case, the smallness of
HC = (HC+ + HC− )/2
magnetic nanoparticle behaves like a perfect superparamagnet at (around 5 Oe) suggests that the synthesis here adopted has
all temperatures: no hysteresis cycle is observed nor a saturation the result to prepare metallic nanoparticles less oxidized with
value at high-applied magnetic fields [13]. respect to other preparation routes also in comparison with other
The hypothesis that our Ni nanoparticles are mainly formed results [15].
by amorphous particles is suggested by the absence of Ni peaks From the theory of superparamagnetism, it is possible to
in the XRD measurements and it was also confirmed by other obtain the blocking temperature from the temperature depen-
experimental evidences. The hysteresis cycle at 5 K up to 9 T is dence of the coercive field using the equation [14,16]:
displayed in Fig. 10. At very low fields, we have a sharp increase   1/2 
due to the crystalline fraction of the Ni nanoparticles, which T
HC = HC0 1 − (4)
behaves like a ferromagnet. The continuous increase of the TB
magnetization above 0.2 T is the superparamagnetic behaviour
of the amorphous Ni. It should be pointed out that also at where HC0 is the coercivity at 0 K.
9 T the saturation limit is not reached, as expected for a pure The expected low temperature linear dependence of the coer-
superparamagnet. cive fields with respect to the root of the temperature is presented
This hypothesis explains also the hysteresis cycle behaviours for Ni nanoparticles in nanotubes in Fig. 11 while in the inset
of Ni nanoparticles presented in Fig. 7a. The hysteresis cycle the data for Ni nanoparticles are reported. From these data, one
is due to the small fraction of crystalline Ni nanoparticles and could obtain the blocking temperatures TB = 74 and 68 K, for Ni
the continuous increase of the magnetization after the cycle is nanoparticles and nano Ni in MWCNT, respectively. We remark
due to the rotation of the magnetic moments of the amorphous anyway that these temperature values are meaningless since in
Ni towards the applied field: this rotation is more effective at systems where a size distribution of the nanoparticles is present,
lower temperatures due to the lower thermal energy opposing a distribution of the blocking temperatures is expected, being
to the magnetic field effect. Ni nanoparticles in MWCNTs (see TB proportional to the volume of the nanoparticle through the
38 D. Gozzi et al. / Journal of Alloys and Compounds 419 (2006) 32–39

by the wide size and blocking temperature distributions hinder-

ing any further analysis.

4.3. The high T magnetic properties of Ni nanoparticles

and nano Ni in MWCNT

In the theory of superparamagnetism, the magnetization fol-

lows the Langevin function:
 
M µH kB T
= coth − (8)
MS kB T µH

where MS is the saturation magnetization, H the magnetic field,

kB the Boltzmann constant, T the temperature and µ is the aver-
Fig. 11. Linear dependence of the coercivity HC for Ni nanoparticles in
age magnetic moment of the nanoparticles.
MWCNT with respect to T1/2 . In the inset, the same linear dependence is reported The fit of both our magnetic data with a single Langevin
for Ni nanoparticles. function was, anyway, disappointing. In fact, the wide distribu-
tion of particle sizes in our samples resulting in a distribution
of magnetic moments requires the use of a weighted sum of
relation: Langevin functions [18] or at least the sum of two Langevin func-
KV  tion related to the bimodal size distribution function observed in
TB = (5) our samples [19]. In such way, a good fit of the magnetization in
25kB
the whole field range was obtained and the results of the fit are
where K is the magnetic anisotropy energy per unit volume. shown, as solid line, in Fig. 8a and b for Ni nanoparticles and
So, by using the bimodal size distribution obtained by TEM nano Ni in MWCNT, respectively.
analysis, we have calculated the TB values corresponding to the For Ni nanoparticles, we find from the fit that 71% of our
two mean size values of the Ni nanoparticles in MWCNT: in particles carry a mean magnetic moment µ1 = 17 000µB while
this case, the crystallization of the nickel (Tcr = 333 ◦ C) [17] is for 29% the mean magnetic moment µ2 is 150 000µB . Since the
complete due to the higher working temperature applied for the experimental magnetic moment of the single particle is related
synthesis of the nanotubes (500 ◦ C). By the relationships: to the volume of the particle by the following equation:
TB (HC ) = 0.72TB1  + 0.28TB2 , µ = MS V  (9)
 
TB1  V1  r1  3
= = = 0.0266 (6) where MS is the saturation magnetization of bulk nickel, our
TB2  V2  r2  values are consistent, under the hypothesis of spherical shape
where TB (HC ) is the blocking temperature obtained from the fit of the particles, with diameters of r1 = 4.2 nm and r2 = 8.8 nm,
of Fig. 11, r1 and r2 are the mean radii of the bimodal distribu- respectively.
tion obtained from TEM and coefficients 0.72 and 0.28 are the On the other hand, for Ni nanoparticles in nanotubes, we
weights of the two types of nanoparticles obtained from the inte- obtain a similar distribution of the two magnetic moments and
gration of the areas of the two peaks reported in the histogram hence of the dimensions: around 76% of Ni nanoparticles in
of Fig. 4. The calculated two different mean blocking tempera- nanotubes have µ1 = 16 000µB and 24% have µ2 = 150 000µB .
tures are: TB1  = 6 K and TB2  = 230 K. This analysis, showing These values lead to r1 = 4.1 nm and r2 = 8.8 nm.
the existence of a high blocking temperature, explains why the In both the systems, a good agreement with the TEM results,
merging of the ZFC and FC curves, that must happens at TB , is i.e., the mean radius value and the percentage, is obtained from
observed above T = 200 K. the Langevin fit.
Finally, from Eq. (4), we obtain HC0(1) = 29 mT for Ni
nanoparticles and HC0(2) = 48 mT for Ni in MWCNT. It should 5. Conclusions
be noted that both values are well below the value of 95 mT
obtained from the equation: The present work belongs to a research program oriented to
K1 functionalise CNTs by single or polycrystalline metallic or inter-
HC0 = 0.64 (7) metallic nanoparticles that have by themselves relevant physical
MS
and/or chemical properties such as electrical, electronic, mag-
for randomly oriented and non interacting particles, using netic, catalytic, piezoelectric and so on. The first objective is
the saturation magnetization MS = 541 emu/cm3 and taking to check if and how the CNTs change their properties or the
for the anisotropy constant K1 the low temperature value changes are only at expenses of the embedded nanoparticles.
(K1 = −8 × 105 erg/cm3 ). Weak magnetic interactions could Next step is to envisage and test some specific application in the
decrease the HC0 . In our case, the HC0 calculation is affected field of the nanotechnologies.
 D. Gozzi et al. / Journal of Alloys and Compounds 419 (2006) 32–39 39

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