IOP PUBLISHING

SUPERCONDUCTOR SCIENCE AND TECHNOLOGY

Supercond. Sci. Technol. 20 (2007) 827831

doi:10.1088/0953-2048/20/8/018

The effect of nano-alumina on structural

and magnetic properties of MgB2
superconductors
Intikhab A Ansari1 , M Shahabuddin1,2, Khalil A Ziq3 , A F Salem3 ,
V P S Awana4 , M Husain1 and H Kishan4
1

Department of Physics, Jamia Millia Islamia (Central University), New Delhi 110025, India
Department of Physics, College of Science, King Saud University, PO Box-2455, Riyadh
11451, KSA
3
Department of Physics, College of Science, King Fahad University of Petroleum and
Minerals, Dehran, KSA
4
National Physical Laboratory, Dr K S Krishnan Marg, New Delhi 110012, India
2

E-mail: intikhabansari@yahoo.com

Received 2 May 2007, in final form 17 June 2007

Published 13 July 2007
Online at stacks.iop.org/SUST/20/827
Abstract
Nano-Al2 O3 doped Mg1x Alx B2 with 0  x  6% were synthesized by
solid state reaction at 750 C in Fe tube encapsulation under a vacuum of
105 Torr. Resistance measurement shows that the Tc decreases with x and
zero resistivity for x = 0 and 6% are obtained at 38 and 35 K, respectively.
XRD measurement shows that the lattice parameter and cell volume also
decrease monotonically with increasing doping levels. From this we infer
that the Al has been substituted in the lattice of MgB2 at Mg sites. Resistivity
measurement shows a systematic decrease in Tc with doping which also
confirms the substitution of Al. Magnetization studies in the temperature
range from 4 to 35 K and in the magnetic field up to 9 T shows a significant
increase in the irreversibility field (Hirr ), critical current density (Jc ) and
remanent magnetization (MR ) with increasing concentration of the Al2 O3
nanoparticle. At low fields we have observed large vortex instabilities
(known as a vortex avalanche) associated with all doped samples. The
vortex-avalanche effect is reduced with increasing temperature and vanishes
near 20 K. The results are discussed in terms of local-vortex instabilities
caused by doping of Al2 O3 nanoparticles.
(Some figures in this article are in colour only in the electronic version)

1. Introduction
The recent discovery of superconductivity at 40 K in
MgB2 [1, 2] stimulates scientific interest due to its simple
electronic structure and low fabricating cost. It has the highest
transition temperature (Tc ) of the metallic superconductors.
A previous study [3] shows the low critical current density
Jc , due to the poor grain connection as well as lack of flux
pinning centres in this material. Hence, it is essential to
prepare MgB2 superconductors with high Jc values. Several
attempts have been made to improve the pinning behaviour
in superconducting MgB2 , such as high energy ion beam
0953-2048/07/080827+05$30.00

irradiation [4, 5] and nanoparticle doping [612]. Nanoparticle

substitution seems to be the best and optimized practical route.
To date, many attempts to increase Tc via chemical
substitution have been shown to be unsuccessful and have
resulted in the decrease or loss of superconductivity [13].
Transition metal doping on MgB2 was reported to be
favourable in increasing Jc and irreversibility fields in bulk
samples [21]. This was attributed to the enhanced pinning
properties and improvement of the sample density promoted
by excellent grain connectivity.
Several anomalous materials have been substituted on
Mg sites such as Al [13, 14], Li [15, 16], 3d transition

2007 IOP Publishing Ltd Printed in the UK

827

I A Ansari et al

Table 1. Variation of a -lattice parameter, c-lattice parameter, cell

volume and transition temperature Tc with regard to doping level x
for nano-alumina-doped MgB2 .

Figure 1. XRD patterns of 0%, 2%, 4% and 6% nano-alumina-doped

MgB2 .

metals [1719] and 4d transition metals [20]. Slusky et al

[13] reported that on Mg1x Alx B2 , Al substitutes up to x =
0.1, beyond which a two-phase region is observed possessing
the same AlB2 structure with unlike c parameters. Li et al
[14] shows the two structural phase transitions at x = 0.17
and 0.75 in Mg1x Alx B2 . Several reports reveal that microsized Al doping is detrimental to the superconductivity of
MgB2 [13, 2628]. In contrast, some reports [16, 29] showed
that Jc values of MgB2 were enhanced slightly by a small
amount of micro-sized Al doping. Evidently, we observed the
two contradictory results about the Al-doped MgB2 system.
In this paper, we discussed the synthesis of nano-Al2 O3
doped MgB2 samples and investigated their structures as a
function of doping concentration. The effect of doping level
on the magnetization of the samples as a function of field at
different temperatures was discussed. We observe that the
doping of nano-alumina has improved the superconducting
properties.

2. Experimental details
Mg1x Alx B2 (x = 0%, 2%, 4% and 6%) were prepared
by a solid state reaction method under a high vacuum using
Mg powder (99.5% purity), amorphous B powder (99.99%
purity) and nano-alumina powder (99.99% purity, particle size
20 nm) from Sigma Aldrich in stoichiometric ratio. These
starting materials were mixed and ground in an agate mortar
and pestle at room temperature for 1 h. The mixed powders
were pressed by a hydraulic press into the form of pellets with
dimensions of 20 10 3 mm3 . These pellets with different
concentrations of Al (i.e. with different x ) were placed in
separate soft iron crucibles and sealed inside the quartz tube
under a high vacuum of 105 Torr. Finally, the sintering was
828

x (%)

a (A)

c (A)

)
V (A

Tc (K)

0.0
2.0
4.0
6.0

3.086
3.085
3.083
3.082

3.524
3.522
3.351
3.351

29.063
29.037
27.589
27.576

38.0
36.5
36.1
35.0

carried out at 750 C for two and half hours in the box furnace.
The samples were taken out of the furnace and quenched into
liquid nitrogen (LN2 ). As a result of this we find a bulk
polycrystalline and moderately porous compound of nanoalumina-doped MgB2 . For the synthesis of a vacuum-annealed
MgB2 sample we follow the method of [31].
The phase constituent was investigated using XRD with
Cu K radiation in a 2 range of 20 80 . The lattice
parameters were obtained from the peak positions of the
XRD plots. Resistivity measurements were carried out by
the standard four-probe technique. The DC magnetizations
of these samples were measured using a PAR-4500 Vibrating
Sample Magnetometer (VSM). Temperature was monitored
using a C-glass thermometer with accuracy better than 0.05 K.
The weight of all the samples used in the present study were
kept at 4555 mg. The irreversibility field (Hirr ) is obtained
from the lowest magnetic field at which the magnetization is
reversible.

3. Results and discussion

Figure 1 shows the XRD pattern of 0%, 2%, 4% and 6% nanoalumina-doped MgB2 , respectively. MgO peaks are clear in all
samples and the intensity increases with the increase of doping
percentage.
Since sintering was done in a vacuum there is no chance
of oxygen from air. It might come from Al2 O3 during the
sintering process and reacted with Mg to form MgO. Another
source of oxygen might be B2 O3 which has been seen in
amorphous boron powder. No Al-rich phase and other impurity
phases have been seen as is clear from figure 1. The cell
volume and lattice parameters of the sample decreases with
increase of the doping level as is clear from table 1. It is
well known that the diameter of Al3+ and Mg2+ is 0.675 and
respectively. Thus a decrease in lattice parameters
0.860 A,
and cell volume is due to the partial occupation of Al at
Mg sites. These observations clearly endorse that Al atoms
partially occupy the sites of Mg in the MgB2 lattice.
Figure 2 demonstrates the temperature dependence of
resistivity for the 0, 2, 4 and 6% nano-alumina-doped MgB2
system. The inset shows the temperature dependence of
resistivity in the vicinity of 1060 K. It is observed that all
the samples reveal the metallic resistivity down to 40 K and
go to the sharp superconducting transition around 38 K. The
= 0 varies from 3538 K as nano-alumina concentration (x)
increases from 0 to 6%. The Tc decreases systematically with
increasing x . The normal resistance of the samples increases
with increasing the percentage of x as is clear from figure 2.
Around 40 K the (T ) follows a power law with a minute
positive slope. Residual resistivity ratio (RRR) values decrease

The effect of nano-alumina on structural and magnetic properties of MgB2 superconductors

Figure 2. Temperature dependence of the resistivity of the nano

Al2 O3 doped MgB2 system. Inset shows the temperature dependence
of the resistivity curve in the vicinity of 060 K.

from 3 to 1.82 with the increase of the doping level. The

main effect of substitution of Al for Mg is to fill the hole
bands with electrons and leads to an increase of scattering
in and bonds. Thus the temperature dependence of
electrical resistivity of the samples helps us to understand the
electronphonon interaction, which is accurately described by
the BlochGruneisen integral [22, 23], and our results on the
(T ) behaviour of MgB2 system bear a resemblance to those
earlier reported [24, 25]. Our (T ) measurements, i.e. change
in Tc and normal resistance, also systematically support that
the nano-alumina has occupied the Mg sites homogeneously.
Magnetization measurements are presented in figures 3
and 4. In figure 3, we present the hysteresis loops measured

at 4.2 K for all samples. One can clearly observe two

different behaviours. Below 2 T, a large unstable behaviour
is clearly seen in figure 3, usually in both branches of the
hysteresis loops. Above 2 T, the loops follow the normal
behaviour commonly seen in hysteresis loops. This unstable
behaviour, commonly referred to as a vortex avalanche, has
been observed in various high temperature superconducting
samples with high critical current density.
Local heating causes tiny regions in the sample to turn
normal, causing a sudden rush of the trapped flux to these
areas. As a result a sudden drop in the magnetization is
observed. Moreover, the remanent magnetization is reduced
accordingly, as can be seen from these hysteresis loops
presented in figure 3. In all doped samples, the magnetization
above 2 T is higher than the magnetization of the pure
sample, indicating higher trapped flux in the doped samples.
However, since no vortex avalanche is observed in the pure
sample, the magnetization below 2 T is higher than that of the
doped samples. We have repeated the same measurements at
higher temperatures at which the vortex avalanche completely
disappears, namely at 20 K. The results are presented in
figure 4. Nearly all hysteresis loops for the doped samples are
wider than the loops for the pure sample at all fields.
All hysteresis loops (figures 3 and 4) indicate wider
loops in all doped samples: at low temperatures (<20 K)
the vortex avalanches (>2 T). At higher temperatures
similar results can be seen nearly for all doped samples.
This indicates higher critical current density and higher flux
trapping in nearly all doped samples. It is interesting to
observe that vortex instability is maximum in the highest doped
samples (6% Al2 O3 ), where the normal state resistivity is also
maximum. An avalanche of flux jumps in polycrystalline
MgB2 superconductor has been reported by some of us in [30].
Figure 5 illustrates the Hirr versus T plot for the nanoalumina-doped MgB2 system. It is also noted that the

Figure 3. Hysteresis loops at 4.2 K for all MgB2 samples doped with various concentrations of Al2 O3 nanoparticles. The vortex avalanche is
clearly shown below 2 T for all doped samples.

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I A Ansari et al

Figure 4. Hysteresis loops at 20 K for all MgB2 samples doped with various concentrations of Al2 O3 nanoparticles. The vortex avalanche has
completely vanished.

Acknowledgments
The work is partly supported by King Saud University, College
of Science-Research Center project nos. Phys/2005/33 and
Phys/2007/34.

References

Figure 5. Temperature dependence of irreversibility field Hirr for the

Mg1x Alx B2 sample.

irreversibility field has increased in all doped samples in

comparison to the pure sample. The maximum increase was
achieved in the 2% Al2 O3 doped sample as is clear from
figure 5.

4. Conclusion
In summary, we have successfully synthesized nano-Al2 O3
doped Mg1x Alx B2 (x = 0%, 2%, 4% and 6%) and
investigated the doping effect of nanoparticles on the
superconducting properties of MgB2 bulk material. We have
observed that the lattice parameter, cell volume and Tc decrease
monotonically with increasing doping level. Magnetization
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the hysteresis loops in MgB2 samples doped with Al2 O3
nanoparticles. We also observed an increase in vortex
avalanches in doped samples that persists up to 20 K in samples
doped with 6% Al2 O3 . Hysteresis loop measurements also
reveal a significant increase in the irreversibility field (Hirr ) as
a result of doping.
830

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