Materials Science-Poland, 31(4), 2013, pp.

501-505
http://www.materialsscience.pwr.wroc.pl/
DOI: 10.2478/s13536-013-0134-4

Synthesis and characterization of Co2FeAl Heusler

alloy nanoparticles
A RVIND K UMAR , P. C. S RIVASTAVA∗

Department of Physics, Banaras Hindu University, Varanasi-221005 (U.P.), India

Heusler alloy Co2 FeAl (CFA) nanoparticles have been synthesized by reducing a mixture of the precursors: CoCl2 ·6H2 O,
Fe(NO3 )3 ·9H2 O and AlCl3 ·6H2 O under H2 atmosphere. XRD, SEM and TEM techniques have been used for the characteri-
zation of the prepared material. XRD and SAED data from TEM show the formation of mixed phases of L21 , B2 and A2 type
crystal structure of the alloy. The estimated particle size from XRD data and TEM micrograph has been found in the range of
10 nm to 50 nm. The saturation magnetization has been found of 115 emu/g from M-H characteristics which is close to its bulk
value of saturation magnetization. Chemical composition of the elements has also been estimated from EDAX, which shows a
ratio of Co:Fe:Al as 2.12:1.06:0.81.
Keywords: Heusler alloy; nanoparticles; Co2 FeAl; M-H characteristics
© Wroclaw University of Technology.

1. Introduction was first predicted in Heusler alloys by De Groot

et al. [12]. Half metallic ferromagnets are the com-
Nanomaterials and nanoparticles based devices pounds which show semiconducting behaviour for
have recently attracted much attention and are of one type of spin channel at Fermi surface and
great interest for research due to their unique size metallic behaviour for other type of spin channel
and interesting chemical and physical properties as at Fermi surface. Half metallic compounds (which
compared to bulk materials [1]. The high surface have 100 % spin polarization at Fermi surface) can
to volume ratio of nanoparticles introduces many be used potentially in spintronics devices [12, 13].
size dependent phenomena and interesting chem- Among the half metallic ferromagnets, Heusler al-
ical, electronic, magnetic and mechanical prop- loy, especially Co-based Heusler alloy has attracted
erties [2, 3]. Synthesis of magnetic nanoparti- high attention due to its interesting magnetic prop-
cles is a hot topic now due to their potential ap- erties such as high Curie temperature and high sat-
plication in the fields of medicine, pharmaceu- uration magnetization [14, 15].
tics, in ferrofluids, engineering, material science,
There are several ways to synthesize Heusler al-
high density magnetic data storage, high frequency
loy such as arc-melting of elements in noble gas
electronics, high performance permanent magnets
atmosphere or mechanical alloying method [16–
and magnetic refrigerants [4, 5]. There are dif-
21]. There are few reports on synthesis of Heusler
ferent routes to synthesize nanomaterials such as
alloy by chemical route. Sapkota et al. [22] syn-
laser ablation [6] hydrothermal synthesis [7], sol-
thesized Heusler alloy Co2 FeAl nanowires and
gel [8], ultrasonic-assisted wet chemical route [9],
studied their structural and magnetic properties.
co-precipitation [10] and CVD processes [11].
Basit et al. [23] synthesized Co2 FeGa nanopar-
Among various classes of magnetic nanoparti- ticles chemically and investigated their structure,
cles, Heusler alloys, which show half metallicity morphology and magnetic properties. Recently,
is of interest due to their significant spin polariza- Du et al. [24] synthesized Co2 FeAl nanoparticles
tion of 100 % at the Fermi surface. Half metallicity by co-precipitation route and studied their mag-
netic and structural properties. In this report, we
∗ E-mail: [email protected] have used chemical route to synthesize Heusler

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502 A. Kumar, P. C. Srivastava

alloy Co2 FeAl (CFA) nanoparticles by reducing 3. Results and discussion

a methanol impregnated mixture of CoCl2 ·6H2 O,
Fe(NO3 )3 ·9H2 O and AlCl3 ·6H2 O. The synthe- 3.1. XRD study
sized powder material has been characterized by The XRD pattern of the synthesized powder has
X-ray diffraction (XRD), scanning electron mi- been shown in Fig. 1. The observed peaks have
croscopy (SEM), and transmission electron mi- been identified with the JCPDS data. There are two
croscopy (TEM) as well as energy dispersive X-ray peaks observed at 2θ of 45° and 65° which are
analysis (EDAX) to determine its chemical struc- identified and indexed as (220) and (400) lattice
ture, morphology, microstructure and composition. planes of Co2 FeAl alloy phase. Diffraction pattern
Magnetic property has been measured by recording of full-Heusler alloy, which is in chemical form of
M-H characteristics using a VSM facility. X2 YZ can be divided into odd superlattice, even
superlattice diffraction and fundamental diffrac-
tion [25]. For odd superlattice diffraction, peaks are
2. Experimental details
obtained at odd hkl values. Only L21 crystal struc-
The Co2 FeAl nanoparticles were synthesized as ture displays odd superlattice diffraction. For even
follows. The first step was the decomposition and superlattice diffraction, peaks are obtained at hkl
reduction of CoCl2 ·6H2 O, Fe(NO3 )3 ·9H2 O and values which satisfy h + k + l = 4n + 2, where n is
AlCl3 ·6H2 O precursors. For synthesis of Heusler a positive integer. Both B2 and L21 structures show
alloy Co2 FeAl nanoparticles, a solution of pre- even superlattice. For fundamental diffraction, hkl
cursors CoCl2 ·6H2 O (2.3710 g), Fe(NO3 )3 ·9H2 O values satisfy the relation h + k + l = 4n. This type
(2.0130 g), and AlCl3 ·6H2 O (1.2029 g) was of diffraction has been shown by A2, B2 and L21
prepared in 200 ml methanol. All chemicals, types of crystal structures. So the observed peaks of
CoCl2 ·6H2 O (>99%), Fe (NO3 )3 ·9H2 O (>99%), the synthesized CFA nanoparticles at 2θ of 45° and
and AlCl3 ·6H2 O (>97%) were purchased from 65° correspond to mixed phases of L21 , B2 and A2
SDFCL, sd fine-CHEM Limited, India and were structure. In A2 structure all the constituents ran-
used without any further purification. The solu- domly occupy the lattice sites.
tion was sonicated for 5 min. Methanol was re- Crystallite size, σ , has also been estimated
moved using a rotary evaporator. The obtained from the Scherrer relation [26]; σ = 0.9λ (ω ·
solid was dried at 80 °C for 2 h. The solid was then cos θ )−1 , where ω is the full width at half max-
gently ground to powder and annealed at 850 °C imum (FWHM) of the diffraction peak, λ is the
for 5 h under H2 atmosphere with a flow rate of wavelength of the X-ray source (of CuKα ; λ =
50 ml/min. The samples were naturally cooled to 1.54060 Å, in our case) and θ is the Bragg angle.
room temperature and collected for the analysis. The FWHM has been found to be of 0.1968° and
0.1800° from XRD pattern. The FWHM values
The chemical structure was characterized by
have been used to estimate the crystallite size
X-ray diffraction (X’Pert Pro PANalytical diffrac-
which has been found to be of 46 nm and 53 nm.
tometer) technique using CuKα (λ = 1.54060 Å)
radiation source. Surface morphology of the syn-
3.2. Morphological study
thesized powder of Co2 FeAl alloy was character-
ized by SEM (Philips-XL 20) technique. To an- The morphology of the as synthesized pow-
alyze the microstructure of the synthesized alloy, dered sample of Co2 FeAl alloy has been observed
TEM examination with Tecnai 20G2 was carried with SEM. Fig. 2 shows the SEM micrograph of
out. The composition of the alloy was determined synthesized powder of Co2 FeAl alloy. The SEM
from EDAX, attached with TEM facility. Magnetic micrograph shows formation of granular like mor-
properties were characterized by M-H characteris- phology. The grain size, estimated from SEM mi-
tics using a vibrating sample magnetometer (EV7 crograph has been found to range from 80 nm to
VSM, ADE technologies) facility. 500 nm. The SEM micrograph shows an agglom-

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 Synthesis and characterization of Co2 FeAl Heusler alloy nanoparticles 503

(Fig. 3(a)) has been indexed as (222), (330) and

(531) crystal planes which also confirms the forma-
tion of Co2 FeAl alloy. Particle size has also been
estimated from the TEM micrograph which clearly
shows the formation of nanoparticles with the size
varying from 10 nm to 50 nm. The particle sizes are
in good agreement with crystallite size estimated
from XRD data. Fig. 3(b) shows the particle size
distribution histogram for the synthesized Co2 FeAl
nanoparticles which has been estimated from the
TEM image (Fig. 3(a)).
The composition of the synthesized powder
of Co2 FeAl Heusler alloy was estimated from
EDAX, attached with TEM facility. Fig. 4 shows
the EDAX spectrum of the observed nanoparticles
which clearly shows the presence of Co, Fe and
Fig. 1. X-ray diffraction pattern of the synthesized Al elements. The observed Cu peak in the EDAX
Co2 FeAl nanoparticles.
spectrum is due to copper grid that was used for
mounting the sample in the TEM machine. The ra-
tio of Co:Fe:Al comes out to be as 2.12:1.06:0.81
which is nearly 2:1:1.

3.3. Magnetization (M-H) study

The magnetic property of as synthesized
nanoparticles of CFA alloy was investigated with
a vibrating sample magnetometer (VSM). Fig. 5
shows the M-H characteristics of CFA powder. M-
H characteristics of CFA alloy show ferromagnetic
nature with a small value of remanence and co-
ercivity. The coercivity, estimated from M-H loop
is found to be of 65 Oe. The coercivity (Hc ) has
been estimated as Hc = (H+ − +
c − Hc )/2, where Hc
Fig. 2. Scanning electron microscopy (SEM) micro- −
and Hc are +ve and −ve coercive fields. The
graph of the synthesized Co2 FeAl nanoparticles. value of remanence (Mr ) has been estimated at the
zero field intercept at the magnetization axis and
eration of smaller grains to transform into bigger found to be of 7.56 emu/g (inset of Fig. 5). The
grains. For a better resolution of morphological de- room temperature saturation magnetization of syn-
tails, TEM has been used. thesized CFA alloy is of 115 emu/g. This value of
Fig. 3(a) shows the TEM micrograph of the syn- saturation magnetization is close to the value given
thesized powder of Co2 FeAl alloy. The insets in by Slater-Pauling rule [14, 15, 27].
Fig. 3(a) show the selected area electron diffrac- According to Slater-Pauling rule, magnetic mo-
tion (SAED) of the Co2 FeAl alloy powder and the ment per unit cell is given by M = Nv − 24, where
high resolution image of the marked portion on the Nv is the number of valence electrons in one unit
TEM micrograph. A typical SAED pattern shown cell. The value of Ms obtained for CFA nanoparti-
in the inset of Fig. 3(a) clearly reveals the poly- cles different from the bulk value seems to be due
crystalline nature of the alloy. The SAED pattern to mixed phases of L21 , B2 and A2 type structure.

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504 A. Kumar, P. C. Srivastava

(a)

Fig. 3.Fig. 3. (a) Transmission

(a) Transmission electronelectron microscopy
microscopy (TEM) micrograph
(TEM) micrograph of the synthesized
of the synthesized Co2FeAl the
Co2 FeAl nanoparticles;
insets show the selected area electron diffraction pattern and high resolution image of marked portion and
nanoparticles;
(b) Particle sizethe insets show
distribution the from
histogram selected area electron
TEM image diffraction pattern and high
(Fig. 3(a)).

resolution image of marked portion and (b) Particle size distribution histogram from TEM

image (Fig.3 (a)).

The composition of the synthesized powder of Co2FeAl Heusler alloy was estimated

from EDAX, with attached TEM facility. Fig. 4 shows the EDAX spectrum of the observed

nanoparticles which clearly shows the presence of Co, Fe and Al elements. The observed Cu

peak in the EDAX spectrum is due to copper grid that was used for mounting the sample in

the TEM machine. The ratio of Co: Fe: Al comes out to be as 2.12: 1.06: 0.81 which is nearly

2:1:1.
Fig. 5. Magnetization (M-H) characteristics of the syn-
thesized Co2 FeAl nanoparticles.

Fig. 4. Energy dispersive X-ray analyzed (EDAX)

spectrum of the synthesized Co2 FeAl nanopar- mated from XRD. The magnetization behaviour of
ticles. CFA nanoparticles shows ferromagnetic behaviour
at room temperature with a saturation magnetiza-
4. Conclusions tion of 115 emu/g, which is close to bulk value of
CFA alloy as reported by Slater-Pauling curve.
In this report, the synthesis and characterization
of Heusler alloy Co2 FeAl nanoparticles have been Acknowledgements
demonstrated. XRD and SAED results confirm the The authors are grateful to Advanced Centre for Materi-
formation of CFA alloy phases (L21 , B2 and A2). als Science, IIT Kanpur, India for providing the magnetiza-
tion measurements facility. One of the authors (A. Kumar) also
TEM analysis shows the formation of nanoparti- wants to acknowledge the financial support received from the
cles size ranging from 10 nm to 50 nm which University Grants Commission, New Delhi, India in the form
is in good agreement with crystallite size esti- 7 of junior research fellowship (UGC-JRF).

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 Synthesis and characterization of Co2 FeAl Heusler alloy nanoparticles 505

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