Journal of Alloys and Compounds 810 (2019) 151884

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Journal of Alloys and Compounds

journal homepage: http://www.elsevier.com/locate/jalcom

Flux pinning properties of YBCO added by WO3 nanoparticles

Y. Slimani a, *, M.A. Almessiere a, b, E. Hannachi c, **, A. Manikandan d, R. Algarni a, b,
A. Baykal e, F. Ben Azzouz b, f
a
Department of Physics Research, Institute for Research & Medical Consultations (IRMC), Imam Abdulrahman Bin Faisal University, P.O. Box 1982,
Dammam, 31441, Saudi Arabia
b
Department of Physics, College of Science, Imam Abdulrahman Bin Faisal University, P.O. Box 1982, Dammam, 31441, Saudi Arabia
c
Laboratory of Physics of Materials - Structures and Properties, Department of Physics, Faculty of Sciences of Bizerte, University of Carthage, Zarzouna,
7021, Tunisia
d
Department of Chemistry, Bharath Institute of Higher Education and Research (BIHER), Bharath University, Chennai, 600073, Tamil Nadu, India
e
Department of Nanomedicine, Institute for Research & Medical Consultations (IRMC), Imam Abdulrahman Bin Faisal University, P.O. Box 1982, Dammam,
31441, Saudi Arabia
f
Basic and Applied Scientific Research Center, Imam Abdulrahman Bin Faisal University, P.O. Box 1982, Dammam, 31441, Saudi Arabia

a r t i c l e i n f o a b s t r a c t

Article history: In this work, non-added and tungsten oxide nanoparticles (noted WO3-NPs) added to YBa2Cu3Oy (noted
Received 29 May 2019 Y-123) samples were produced using solid-state reaction approach. The structure, morphology, electrical
Received in revised form and magnetic properties were examined by the help of X-ray diffraction (XRD), scanning electron mi-
13 August 2019
croscope (SEM) and physical properties measurement system (PPMS), respectively. XRD showed that the
Accepted 14 August 2019
Available online 15 August 2019
orthorhombic Y-123 phase was successfully formed. SEM investigations showed the existence of bright
nano-entities embedded within the Y-123 matrix for added sample, which are not seen in the non-added
one. The measurements of electrical resistivity verified the manifestation of superconductivity in various
Keywords:
YBa2Cu3Oy
products. The intragranular and intergranular critical current densities were calculated from the mea-
WO3 nanoparticles surements of DC magnetization and AC susceptibility. The strength of pinning centers in the prepared
Structure products was evaluated. The obtained findings reveal that WO3-NPs are powerful to improve the flux
Critical current density pinning capacity and superconducting properties of Y-123 material.
Flux pinning © 2019 Elsevier B.V. All rights reserved.

1. Introduction both electrical transport and magnetic properties. With a view to

Possessing some advantageous characteristics as simplicity of
the synthesis procedure, critical normal-superconductor transition
temperature (Tc) above of that of liquid nitrogen, significant density
of critical current (Jc) and relatively strong property of flux trapping,
nontoxic …, the YBa2Cu3O7-d superconductor is considered as the
most elegant copper oxide material for various applications such as
transmission lines, superconducting permanent magnets … [1].
Since its discover in 1987 [2] till this day, YBa2Cu3O7-d gained great
attention from scientific community to strengthen its ability to
carry Jc under applied magnetic fields and benefit wholly of its
potential. The granular nature structure of YBa2Cu3O7-d depresses
* Corresponding author.
** Corresponding author.
E-mail addresses: yaslimani@iau.edu.sa, slimaniyassine18@gmail.com
(Y. Slimani), hannechi.essia@gmail.com (E. Hannachi).
heighten the electrical transport properties, extensive theoretical
and experimental studies were carried out to control the serious
causes of Jc deterioration namely the grain boundaries and the
vortices dynamics [3e5].
The control of microstructure is the greatest challenges to
overcome these serious nuisances and achieve considerable values
of Jc in granular system. For this reason, various method and tech-
niques have been employed to produce supplementary trapping
centers other than those exist naturally in the matrix that impede
the vortex displacement. It is widely accepted that the adequate
trapping center size must be almost identical to the super-
conducting coherence length (x) [6]. However, others reported that a
trapping center size similar to the penetration depth [7] is preferred.
Controversies about the best size of trapping center are attributed to
the preparation process, growth mechanism and generated defects.
Addition of foreign phase of appropriate material and size is one of
the successful approaches to develop efficient artificial trapping
centers. Various nanostructures with different physical properties

https://doi.org/10.1016/j.jallcom.2019.151884
0925-8388/© 2019 Elsevier B.V. All rights reserved.
2 Y. Slimani et al. / Journal of Alloys and Compounds 810 (2019) 151884

including conductor, semi-conductor, insulator, magnetic, super-
conductor with various shapes like nanowires, nanoparticles,
nanotubes were included in YBa2Cu3O7-d and different results on the
flux trapping properties were announced [8e18].
It is well established that the grain boundaries acting as weak-link
consists a main problem that drastically weakness the transport
properties and damages the phase coherence of superconductors
[19]. The grain boundaries passivation is one of the efficient ap-
proaches proposed to overcome the problem of drop of transport
properties in system with granular structure. Passivation of grain
boundaries may be attained by inclusion of appropriate conductive
metals as silver, gold, aluminum …, and thus enhancement of critical
current density Jc was achieved [20e23]. Also, it was proved that
perovskite compounds as BaZrO3 and BaTiO3 inserted in YBa2Cu3O7-
d compound occupy spaces between grains to form hence compos-
ites with advantageous mechanical and electrical transports prop-
erties [24,25]. Lately, systematic investigations on the impact of
tungsten oxides (WO3) in nanoparticles (NPs) forms added to YBa2-
Cu3O7-d was reported [26]. It is mentioned that nano-WO3 entities
inclusion in the YBa2Cu3O7-d during the second stage of heat treat-
ment leads to produce composites YBa2Cu3O7-d/(WO3)x. Morpho-
logical examinations reveal that the nano-WO3 adhere the grains to
fill empties. Analyses show that both crystal structure, super-
conducting coherence transition temperature and starting transition
temperature of YBa2Cu3O7-d are not changed by the WO3 nano-
entities inclusions. Although Jc measured at 77 K was enhanced
and the flux trapping mechanism by normal centers was amplified
by the WO3, it is more informative to describe the intragranular and
intergranular behaviors of our composites by magnetic studies. The
variation of magnetic flux owing to the magnetization of material
may be measured in either a constant magnetic field (DC-magneti-
zation) or time dependent magnetic field (AC-magnetization).
We propose in this work to analyze YBa2Cu3O7-d/(WO3) com-
posites by DC and AC magnetic measurements at different tem-
peratures from 77 K to 10 K. These analyses provide more specifics
of tungsten oxide nanoparticles (WO3-NPs) effect on super-
conducting properties and enable us to estimate useful super-
conducting physical parameters, like field and temperature
dependence of magnetization critical current density (Jcm), inter-
granular critical current density (Jc,inter), strength of pinning cen-
ters, type of Josephson junction, etc.
2. Experimental details
diffractometer (CuKa radiation). The morphological observations
were done by SEM (FEI Titan G2 80-300). The measurements of
electrical resistivity, ac susceptibility and dc magnetization were
done using Quantum Design PPMS DynaCool 9.
3. Results and discussion
3.1. Structural examination
Fig. 1 illustrates XRD patterns of both prepared samples. XRD
analyses indicated predominantly Y-123 phases (orthorhombic
structure and Pmmm space group) and a neglected Y2BaCuO5 (Y-
211) phase as seen at 2q z 28.9 . XRD investigations does not reveal
any shift in position of various peaks and hence no detrimental
effects on the orthorhombicity were noticed with WO3-NPs doping.
The Y-123 lattice parameters equal to a z3.8182 Å, b z 3.8834 Å
and c z 11.6696 Å are practically unaffected with WO3-NPs addi-
tion. Deep details of XRD analyses were discussed in our previous
publication [26].
3.2. Morphological investigation
Fig. 2 presents SEM images of non-added and WO3-NPs added to
Y-123 samples. Granular structure with Y-123 phase dominance
was perceived for both samples. The average grains size reduced
with the WO3-NPs inclusion. Compared to non-added sample, it is
noticed that the WO3-NPs leads to reduce the porosity. A closer look
for WO3-NPs added to Y-123 sample (Fig. 2c) showed the existence
of bright nano-entities embedded within the Y-123 matrix, which
are not seen in the non-added one.
3.3. Electrical resistivity measurements
Fig. 3 presents variations of the normalized electrical resistivity
(r/r300K) versus temperature for non-added and WO3-NPs added
samples. Both samples indicated metal-like behavior in the normal
state above the onset critical transition temperature T on
c . The normal
state resistivity showed comparable magnitudes (Table 1) and
decreasing trend (Fig. 3) for both samples. T on
c temperature is prac-
tically unaffected with WO3-NPs addition. Afterward, single sharp
transitions to superconductivity at the offset critical transition
off
temperature T c (critical transition temperature at which the

2.1. Synthesis

The non-added and tungsten oxide nanoparticles (WO3-NPs)

added to Y-123 samples were produced through solid-state reac-
tion approach with two sintering steps. Firstly, precursors of
nominal composition YBa2Cu3O7
d were produced starting from
high purity powders of Y2O3, BaCO3 and CuO obtained from Sigma
Aldrich. The reactants were weighed with respect to the stoichio-
metric ratios and ground properly in an agate mortar to get ho-
mogeneously mixed powders. This mixture was pressed into
pellets. The obtained pellets were calcined at 950  C for 12 h.
Finally, x ¼ 0.05 wt% of WO3-NPs (30 nm in size) from the total
mass of sample was added to the calcined precursor. The mixture
was ground, compacted into pellets and then sintered at 950  C for
8 h. As reference, a non-added (x ¼ 0.0 wt%) Y-123 sample was also
prepared under the same condition.

2.2. Characterization techniques

The structure of the synthesized samples was analyzed by Fig. 1. XRD patterns of non-added (x ¼ 0.00 wt%) and WO3-NPs added (x ¼ 0.05 wt%)
investigating their XRD patterns via Bruker D8 Advance to Y-123 samples.
 Y. Slimani et al. / Journal of Alloys and Compounds 810 (2019) 151884 3

Fig. 2. SEM images of (a) non-added and (b,c) WO3-NWs added to Y-123 samples.

and WO3-NPs added to Y-123 samples performed at different

temperatures (77e10 K) and an applied magnetic field ranging
between e 6 and þ6 T. It is discerned that the magnetization is
enhanced with WO3-NPs inclusion. Obviously, the hysteresis width
is wider for added sample. Hence, higher applied fields are required
for WO3-NPs added Y-123 sample in order to close M(H) loops than
the pure one. This finding implies that the irreversibility field (Hirr;
field at which M(H) loops collapses [28]) is enhanced with WO3-
NPs incorporation, which indicate stronger flux pinning capability
with WO3-NPs addition. Indeed, the enhanced connectivity among
grains, the reduced porosity as well as the formation of proficient
pinning centers resulted from WO3-NPs inclusion are the mostly
factors that improve the magnetic and electrical properties. From
M(H) loops, magnetization critical magnetic field Jcm values versus
applied magnetic field H were deduced using Bean model as follow
[29,30]:

Fig. 3. Variations of the normalized electrical resistivity (r/r300K) as a function of

temperature for non-added and WO3-NPs added to Y-123 samples. The inset shows an 20 DM
enlarged view of the superconducting transition. Jcm ¼ (1)
að1
a=3bÞ
Where DM is magnetization hysteresis width, a and b are the
Table 1
sample dimensions. Fig. 5 presents variations of Jcm(H) measured at
Superconducting parameters extracted from the electrical resistivity measurements.
different temperatures for both prepared samples. Obviously, WO3-
off
x content r300K (mU.cm) T on
c (K) Tc (K) NPs addition provides much slower descents of Jcm under applied
0.00 wt% 2.15 94.6 92.0 field, showing a diminishing of the sensitivity to H. At different
0.05 wt% 2.09 94.6 91.7 temperatures, it is noticed that the Jcm(H) values are improved with
WO3-NPs inclusion. For example, at 77 K, the Jcm values for non-
added Y-123 sample are found to be equal to 2920.3 and
resistivity become equal to zero) were observed. T offc showed a slight 33.5 A cm
2 at H ¼ 0 and 1 T, respectively. The Jcm values at T ¼ 77 K
decrease from 92.0 K to 91.7 K for non-added and WO3-NPs added are enhanced for added sample to be around 9138.1 and
samples, respectively (inset of Fig. 3). The single sharp transition and 576.6 A cm
2 at H ¼ 0 and 1 T, respectively. At 77 K, the improve-
the almost unchanged critical transition temperatures suggest the ment was found to about 3.1 and 17.2 times with WO3-NPs addi-
domination of Y-123 phase and the enhanced connectivity among Y- tions at H ¼ 0 and 1 T, respectively. These findings revealed that
123 grains [27]. These results are consistent with the SEM results. WO3-NPs addition could improve the flux pinning capacities and
intragranular properties. This indicates that WO3-NPs could create
efficient pinning centers and strengthen the connectivity between
3.4. Magnetic properties analysis grains, which lead to improve the Jcm values. Hence, the inclusion of
WO3-NPs as efficient pinning centers could be considered as a
Fig. 4 displays magnetic hysteresis loops M(H) of the non-added significant route to achieve better performances of flux pinning.
4 Y. Slimani et al. / Journal of Alloys and Compounds 810 (2019) 151884

Fig. 4. M(H) hysteresis loops performed at T ¼ 77 down to 10 K and H ¼ - 6 to þ 6 T for

the (a) non-added and (b) WO3-NPs added to Y-123 samples. Fig. 5. Variations of Jcm(H) performed at various temperatures for (a) non-added and
(b) WO3-NPs added to Y-123 samples.

The strength of pinning centers was evaluated by categorizing

them into strong (SP) and weak pinning (WP) centers. Therefore, ineffective and overcame by the thermal fluctuations at the vicinity
Jcm values were investigated via the theoretical predictions for SP of this temperature. Till higher temperatures, just the strongest
and WP [31e33]: pinning centers still proficient. The superconducting parameters
deduced from magnetic measurements are listed in Table 2. It is
 2 ! noticed that the J SP WP
cm ð0Þ and J cm ð0Þ values are influenced by WO3-
 NPs incorporation. J cm ð0Þ and J WP
SP
J SP
cm ðTÞ ¼ J SP
cm ð0Þexp
3 T T* (2) cm ð0Þ are improved with WO3-NPs
inclusion. This is principally attributed to the nano-entities incor-
porated into the Y-123 matrix, the strengthening of grains con-
  nectivity and the generated defects. In view of that, WO3-NPs
T
J WP
cm ðTÞ ¼ J WP
cm ð0Þexp
(3) inclusion could be considered as efficient pinning centers to
T0 strengthen the flux pinning capacity of Y-123 superconductors.
To determine the intergranular coupling characteristics, mea-
Where J SP WP
cm ð0Þ and J cm ð0Þ are Jcm values estimated at 0 K for SP and surements of ac-susceptibility, c, were explored for both non-
WP contributions, respectively. To and T* are characteristic tem-
added and WO3-NPs added to Y-123 samples. The variations of
peratures. Generally, the pinning centers for HTS materials are the
real c0 and imaginary c00 parts of c ¼ c0 þ ic00 curves versus tem-
sources of disorder in the sample. SP centers are principally
perature performed under various magnetic fields ranging from 1
resulted from columnar defects and the interfaces among nano-
to 10 Oe and a frequency f ¼ 1 kHz are presented in Fig. 7. The
phases and superconducting matrix [34e36]. WP centers are c
critical T co temperature, designated by the temperature when c0
largely due to the defects generated by inclusion of nanophases 00
and c become equal zero, is practically unaffected to the change of
[34e36]. The Jcm(T) experimental data (scatter symbols) at H ¼ 1 T
the H for both samples. The formation of peak in c00 curves is
are illustrated in Fig. 6. Obviously, the SP contribution dominates
originated from the energy losses caused by the penetration of
for higher temperatures, whereas the WP contribution dominates
magnetic flux in the intergranular networks of weak links [35]. In
for lower temperatures range. The deflection temperature between
line with Bean model [29], a maximum loss occurs once H pene-
SP and WP contributions is perceived around 30 K, wherein the
trate up to the center of the product and hence peak in c00 is
energy of pinning barriers of some pinning centers became
 Y. Slimani et al. / Journal of Alloys and Compounds 810 (2019) 151884 5

observed. The separation of intergranular and intragranular loss

peaks on temperature scale indicate generally weak coupling
grains. Nonetheless, the prepared samples showed merging of both
intragranular and intergranular loss peaks, which indicate strongly
coupled grains. It is obvious that the amplitude of intergranular loss
peak Tp reduces with WO3-NPs incorporation in Y-123, which
reveal an improvement in flux trapping and grains coupling [33].
Moreover, Tp shifts to lower temperature with increasing H. The Tp
shifting with H is employed to determine the temperature depen-
dence of intergranular critical current density Jc,inter. In line with
Bean model [29], Jc,inter at Tp is expressed as below for a sample
having the shape of rectangular bar of cross section 2a  2b:

  H*
Jc;inter Tp ¼ pffiffiffiffiffiffiffiffiffiffiffi (4)
ab

H * is the magnetic field amplitude. The deduced values of Jc,inter by

using equation (4) are presented in Fig. 8. It is well-known that
Jc,inter versus temperature is expressed as follow [35,37]:
Fig. 6. Temperature dependence of Jcm measured H ¼ 1 T of non-added and WO3-NPs
added to Y-123 samples. Solid and dashed lines correspond to the fitting using
!n
  Tp
equations (2) and (3). Jc;inter Tp ¼ Jc;inter ð0Þ 1
off (5)
Tc
off
T c corresponds to the critical transition temperature at which the

Table 2
Superconducting parameters deduced from magnetic measurements.

x J WP
2
c (A.cm ) J SP
2
c (A.cm ) T o (K) T * (K) J c;inter ð0Þ(A.cm
2) n
content

0.00 wt% 91492 10249 10.25 64.26 906.7 1.54

0.05 wt% 99044 13704 12.20 74.45 1224.9 2.43

Fig. 7. Variations of the real c0 and imaginary c00 parts of ac susceptibility against temperature for non-added and WO3-NPs added to Y-123 samples performed under various
applied magnetic fields ranging from 1 to 10 Oe and a frequency f ¼ 1 kHz.
6 Y. Slimani et al. / Journal of Alloys and Compounds 810 (2019) 151884
Fig. 8. Temperature dependence of Jc;inter (symbols) for non-added and WO3-NPs
added to Y-123 samples. Solid lines correspond to the fit using equation (5).
resistivity become equal to zero. Jc;inter ð0Þ and n are fitting param-
eters. The extracted Jc;inter ð0Þ and n values are listed in Table 2. It is
interesting to note that Jc;inter ð0Þ value is improved with WO3-NPs
addition revealing better intergranular properties. Jc;inter ð0Þ in-
creases from 906.7 A cm
2 for non-added sample to 1224.9 A cm
2
for WO3-NPs added to Y-123 sample, which accord with M(H)
measurements. In polycrystalline HTS materials, non-
superconducting regions are separating the superconducting
grains and determine the temperature dependence of Jc;inter . Thus,
the increase in Jc;inter ð0Þ with WO3-NPs incorporations is ascribed to
the induced enhancement of the connectivity among Y-123 grains
and the generated defects that provoke a strengthening of flux
pinning capacities. The deduced n values are found to be around 1.5
and 2.4 for non-added and WO3-NPs added to Y-123 samples,
respectively. An obtained n ¼ 1:5 value between 1 and 2 is typical
for superconductor-insulator-normal metal-superconductor (SINS)
Josephson junction [35]. Nevertheless, superconductorenormal
metalesuperconductor (SNS) Josephson junction is the character-
istic of WO3-NPs added to Y-123 sample [38,39]. The obtained
result is not unexpected because the WO3-NPs are metal oxides,
providing metallic links among grains.
4. Conclusion
The impact of tungsten oxide nanoparticles (WO3-NPs) addition
on the structure, morphology, intragranular and intergranular
properties of Y-123 superconductor has been investigated. XRD
confirmed the successful development of Y-123 phase without
altering its orthorhombic structure. Morphology investigation with
SEM revealed the distribution of nano-sized entities into Y-123
matrix for WO3-NPs added sample. The manifestation of super-
conductivity in various samples was verified via the electrical re-
sistivity measurements. Magnetization hysteresis loops were
performed at different temperatures ranging. From these mea-
surements, intragranular critical current density (Jcm) was deduced
and strength of pinning centers was evaluated by categorizing
them into SP and WP centers. At different temperatures, it is
noticed that the Jcm(H) values are improved with WO3-NPs addi-
tion. Interestingly, the improvement at 77 K was found to about 3.1
and 17.2 times with WO3-NPs additions at H ¼ 0 and 1 T, respec-
tively. As well, Jc,inter was deduced by analyzing measurements of AC
susceptibility. Jc;inter showed also an increasing tendency with
WO3-NPs addition. The obtained findings indicated that the WO3-
NPs could create efficient pinning centers and enhance the
connectivity between grains, strengthening the flux pinning ca-
pabilities and thus improve the Jcm and Jc,inter values.
Acknowledgments
This work was supported by the Institute for Research & Medical
Consultations (Projects application No. 2017-IRMC-S-3 and No.
2018-IRMC-S-2) and the Deanship of Scientific Research (Project
application No. 2018-209-IRMC) of Imam Abdulrahman Bin Faisal
University (Saudi Arabia).
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