Journal of Superconductivity and Novel Magnetism

https://doi.org/10.1007/s10948-018-4829-y

ORIGINAL PAPER

AC Susceptibility of BaZrO3 Nanoparticles Added YBa2 Cu3 O7−δ

Superconductor Prepared via Coprecipitation Method
Nurhidayah Mohd Hapipi1 · Soo Kien Chen1,2 · Abdul Halim Shaari1,2 · Mohd Mustafa Awang Kechik1 ·
Kar Ban Tan3 · Kean Pah Lim1 · Oon Jew Lee4

Received: 4 May 2018 / Accepted: 31 July 2018

© Springer Science+Business Media, LLC, part of Springer Nature 2018

Abstract
In this work, magnetic properties of polycrystalline samples YBa2 Cu3 O7−δ added with x mol.% of BaZrO3 (BZO)
nanoparticles (x = 0.0, 1.0, 2.0, 3.0, 5.0, and 7.0) were studied by AC susceptibility (ACS) measurement. The samples were
prepared using coprecipitation (COP) method. X-ray diffraction (XRD) results showed that all the samples were composed
of Y-123 as the major phase and Y-211 as the secondary phase. XRD peak of BZO was also observed in the samples added
with BZO nanoparticles. The intensity of the peak became higher with increasing amount of BZO addition indicating the
presence of increased amount of the unreacted nanoparticles in the samples. The refined lattice parameters indicated that all
the samples have an orthorhombic crystal structure without the occurrence of orthorhombic-tetragonal phase transformation.
Scanning electron microscopy (SEM) images showed that the samples have randomly distributed grains with irregular shape.
The average grain size increased from 0.30 μm for the pure sample to 0.50 μm for the BZO addition of 7.0 mol.%. ACS
measurement showed a slight decrease of onset critical temperature, Tc−onset (< 1 K) with BZO addition. Both phase lock-
in temperature, Tcj , and coupling peak temperature, Tp , remained relatively unchanged for BZO addition up to 3.0 mol.%.
Based on the Bean critical state model, the calculated intergranular critical current density, Jcm , for the pure sample is 1.88
A/cm2 at Tp = 84.8 K. For the sample added with 7.0 mol.% of BZO, Jcm at Tp = 83.6 K is 1.95 A/cm2 .

Keywords YBa2 Cu3 O7−δ · BaZrO3 · Coprecipitation · Superconductivity · AC susceptibility

1 Introduction
YBa2 Cu3 O7−δ (Y-123) is the first high-temperature super-
conductor (HTS) discovered with critical temperature, Tc ,
above the boiling point of liquid nitrogen [1, 2]. Such dis-
covery marked a significant breakthrough in technological
applications as Y-123 can be cooled with a much cheaper
cost using liquid nitrogen instead of liquid helium in order
 Soo Kien Chen
chensk@upm.edu.my
1 Department of Physics, Faculty of Science, Universiti Putra
Malaysia, 43400 Serdang, Selangor, Malaysia
2 Institute of Advanced Technology (ITMA), Universiti Putra
Malaysia, 43400 Serdang, Selangor, Malaysia
3 Department of Chemistry, Faculty of Science, Universiti Putra
Malaysia, 43400 Serdang, Selangor, Malaysia
4 School of Fundamental Science, Universiti Malaysia
Terengganu, 21300 Kuala Terengganu, Terengganu, Malaysia
to carry a high transport current. Over the years, much effort
has been put forward to study HTS with the ultimate aim to
improve Tc and critical current density, Jc . It was found that
one way to increase Jc is to enhance the pinning force [3–5].
This can be done by introducing pinning centers into Y-123
so as to prevent the flux lines from moving when the super-
conductor is carrying electrical current in the presence of
external magnetic field. The pinning capability of undoped
Y-123 is rather weak as reflected in the rapid decrease of its
Jc with applied field presumably due to the lack of effec-
tive pinning centers [6–8]. Defects and nano-inclusions are
among the flux pinning sites [6, 7]. These defects can be
induced by addition of nanoparticles into Y-123 leading to
the formation of strong artificial pinning centers [9, 10].
BaZrO3 (BZO) in the form of nanoparticles is a potential
dopant for enhancing the pinning of HTS since it does
not dope into the Y-123 lattice [11]. Moreover, its high
melting point leads to the smaller particles due to the
slow kinetic growth [3]. Most importantly, BZO has a
large lattice mismatch with Y-123. The strain between the
phases produces defects that enhance the pinning strength
 J Supercond Nov Magn

Y211 7 mol.% BZO

(011)
BZO

7 mol.% BZO
5 mol.% BZO

5 mol.% BZO
3 mol.% BZO
Intensity (a.u.)

Intensity (a.u)
3 mol.% BZO
2 mol.% BZO

2 mol.% BZO
1 mol.% BZO
1 mol.% BZO
(103)

0 mol.% BZO
(013)

Y123
(123)
(113)
(010)

(206)
(020)
(014)

(213)
(200)

(130)
(214)

(026)
(121)
(100)

(102)

(115)

(303)
(106)
(004)

(007)

(118)
(032)
20 25 30 35 40 45 50 55 60 65 70 75 80 29.6 29.8 30.0 30.2 30.4 30.6 30.8 31.0
2 (degree) 2θ (degree)
(a) (b)

Fig. 1 a X-ray diffraction patterns of Y-123 +x mol.% of BZO samples. b The XRD patterns of the peak corresponding to the (0 1 1) plane of
BaZrO3 in the Y-123 +x mol.% of BZO samples

[3]. Previously, Awano et al. studied the crystal growth coprecipitation (COP) method in order to produce smaller
conditions of Y-123 and Y-123-BZO bulk composite. grain size, higher purity, and homogeneous powders with a
Unidirectional crystal growth was successfully induced by well dispersion of BZO nanoparticles [14]. By doing so, the
applying uniaxial pressing to the samples [12]. Jha and feasibility of using COP method for large-scale production
Khare reported the fabrication of polycrystalline Y-123- of Y-123-BZO composite can be evaluated in addition to
BZO composite from a mixture of Y-123, ZrO2 , and BaCO3 studying the structural and superconducting properties of
using conventional solid-state reaction method. They found the samples.
a significant improvement in Jc and pinning force attributed
to the increased defect density as a result of BZO
addition [13]. In Y-123-BZO films, similar improvement 2 Experimental Details
was observed ascertaining the role of BZO in creating
effective flux pinning centers [5, 9]. The enhancement in Sample preparation was undertaken using COP method.
both Jc and pinning force is accompanied by a marginal Appropriate amounts of yttrium (III) acetate tetrahydrate,
degradation in Tc . Y(CH3 COO)3 .4H2 O (99.9% Alfa Aesar), barium acetate,
Motivated by the positive effect of BZO towards Jc , Ba(CH3 COO)2 (≥ 99% Alfa Aesar), and copper acetate
we prepared a series of polycrystalline Y-123 bulks doped monohydrate, Cu(CH3 COO)2 .H2 O (≥ 99% Sigma Aldrich)
with BZO. Compared to the previous studies as mentioned with the stoichiometric ratio of Y/Ba/Cu (1:2:3) were
before, we used commercial nanosized BZO particles as dissolved in 500-ml acetic acid (solution A). Meanwhile,
a dopant. Moreover, the samples were prepared using oxalic acid was dissolved in a mixture of distilled water

Table 1 Lattice parameters of

a-, b-, and c-axis and unit cell BZO x (mol.%) Lattice parameters (Å) Volume (Å3 )
volume for Y-123 +x mol.% of
BZO samples a-axis b-axis c−axis

0.0 3.8242 ± 0.0002 3.8827 ± 0.0003 11.6701 ± 0.0012 173.28

1.0 3.8242 ± 0.0003 3.8809 ± 0.0004 11.6643 ± 0.0013 173.12
2.0 3.8252 ± 0.0002 3.8818 ± 0.0003 11.6625 ± 0.0013 173.17
3.0 3.8233 ± 0.0002 3.8812 ± 0.0003 11.6626 ± 0.0012 173.06
5.0 3.8243 ± 0.0003 3.8805 ± 0.0003 11.6639 ± 0.0012 173.11
7.0 3.8251 ± 0.0002 3.8809 ± 0.0004 11.6592 ± 0.0013 173.08
J Supercond Nov Magn

Fig. 2 The W-H plots for Y-123 0.0021 7 mol.% BZO

+x mol.% of BZO samples. Fit 0.0020
to the data, the lattice strain and 0.0019
0.0019 y = 0.00022x + 0.00231
the crystallite size have been
0.0019
extracted from the slope and 0.0022
5 mol.% BZO
y-intercept of the linear fitted 0.0021
curves 0.0021
y = 0.00023x + 0.00243
0.0020

β tot cosθ
0.0020
0.0020 3 mol.% BZO
0.0019
0.0019
0.0019
y = 0.00022x + 0.00228
0.0018
0.0021 2 mol.% BZO
0.0021
0.0020
0.0019
0.0019
y = 0.00022x + 0.00233
0.0019
0.0020 1 mol.% BZO
0.0019
0.0019
y = 0.00022x + 0.00228
0.0019
0.0018
0.0022 0 mol.% BZO
0.0021
0.0021
0.0020
y = 0.00024x + 0.00245
0.0020
1.1 1.2 1.3 1.4 1.5 1.6 1.7 1.8 1.9 2.0

4 sinθ

and 2-propanol with the ratio of 1:1.5 (solution B). Both using the commercial AC susceptometer of CryoBIND
solutions were stirred at 300 rpm for 2 h before being cooled (cryogenic balanced inductive detector) SR830 at the
in an ice bath until the temperature dropped to below 10 ◦ C. frequency of 219 Hz and applied field of 0.5 Oe.
Then, solution A was mixed with solution B and the
resultant co-precipitant was collected via filtration process
for drying at 100 ◦ C for 12 h. The obtained dried powders 3 Results and Discussion
were ground and subsequently calcined in air at 900 ◦ C
for 24 h (denoted as calcined Y-123). After calcination, 3.1 XRD Analysis
appropriate amount of BaZrO3 (BZO, > 50 nm, 98.5%,
Sigma-Aldrich) was added to the calcined Y-123 powders Figure 1a shows the XRD patterns of the pure and BZO-
according to the concentration of 1.0, 2.0, 3.0, 5.0, and added samples. Most of the peaks were indexed to Y-123
7.0 mol.%, respectively. Then, the mixture was ground and with orthorhombic crystal structure and Pmmm space group
pressed into a circular pellet (about 2-mm thickness and 13-
mm diameter) by using a hydraulic press with an applied
pressure load of 5 tons. Lastly, the pellets were sintered at Table 2 Crystallite size and lattice strain for Y-123 +x mol.% of BZO
920 ◦ C for 15 h and slowly cooled to 650 ◦ C at the rate of samples calculated using Williamson-Hall method. The average grain
size of the samples was calculated from the selected 100 grains of the
1 ◦ C/min for 8 h (annealing process) before further cooling SEM image
to room temperature. The sintering and annealing process
were done under a constant oxygen flow. Undoped samples BZO x Williamson-Hall Average grain size,
were also prepared for the purpose of comparison. (mol.%) D (μm)
Phase formation and crystal structure of the samples
Crystallite size Lattice strain
were checked by x-ray diffraction (XRD) method using
(nm) (%)
the PW 3040/60 MPD X’Pert Pro Panalytical Philips DY
1861 x-ray diffractometer with Cu-Kα radiation source. 0.0 56.57 0.024 0.30
The scanning was carried out in the 2θ range of 20◦ –80◦ 1.0 60.79 0.022 0.30
with the increment step size of 0.03◦ . Morphology of the 2.0 59.49 0.022 0.39
grains and the elemental analysis were undertaken using a 3.0 60.79 0.022 0.39
scanning electron microscope (SEM-LEO 1455 VPSEM) 5.0 57.04 0.023 0.45
equipped with energy-dispersive x-ray spectrometer (EDX). 7.0 60.00 0.022 0.50
Superconducting properties of the samples were measured

(ICSD: 01-078-2144). The peaks with high intensity of Y-
123 were observed at 2θ ≈ 32.6◦ and 2θ ≈ 32.9◦ that
correspond to the Miller indices of (0 1 3) and (1 0
3), respectively. Some minor peaks were indexed to Y-
211 (ICSD: 01-079-0697) indicating the presence of such
(a)
(c)
(e)
Fig. 3 SEM images of Y-123 samples added with a 0.0 mol.% b 1.0 mol.% c 2.0 mol.% d 3.0 mol.% e 5.0 mol.% f 7.0 mol.% of BZO at × 5000
magnification. Inset = EDX spectrum for each sample
J Supercond Nov Magn
second phase in the samples. The intensity for Y-123 and
Y-211 decreased as the addition of BZO nanoparticles was
increased. A peak which was indexed to BZO (ICSD: 01-
074-1299) with its Miller indices of (0 1 1) at 2θ ≈30.2◦
started to appear at 1.0 mol.% BZO addition. Figure 1b
(b)
(d)
(f)
J Supercond Nov Magn

shows that the intensity of the BZO peak became higher 1.2 Y123
Y123 + 1 mol.% BZO
with the increasing of BZO addition indicating the increased 1.0 TP Y123 + 2 mol.% BZO
amount of the unreacted nanoparticles. 0.8
Y123 + 3 mol.% BZO
Y123 + 5 mol.% BZO
Table 1 shows the lattice parameters of a−, b−, and c- Y123 + 7 mol.% BZO

Normalized susceptibility (a.u.)

0.6
axis together with the unit cell volume obtained by refining χ"
0.4
the XRD data of the samples using the software HighScore
0.2
Plus. It is obvious from the lattice parameters that all the
0.0
samples have orthorhombic crystal structure and there is Tcj
-0.2
no orthorhombic-tetragonal phase transformation. However,
the lattice parameters of b- and c-axis became smaller after -0.4
Tc-onset
BZO addition as compared to that of the pure sample. The -0.6

distortion of lattice parameter in the b-axis is probably due -0.8

χ'
to the removal of oxygen in copper-oxygen chains (CuO) -1.0

causing the strain energy that retains the chain direction 78 80 82 84 86 88 90 92 94

along the b-axis to diminish [15]. Temperature (K)
The crystallite size and lattice strain of the samples were
Fig. 4 Temperature dependence of the ACS for the Y123 +x mol.%
calculated according to the Williamson-Hall plot [16]: of BZO samples

Kλ
Btot = Bstrain + Bsize = 4Cε tan θ + (1)
Lcos θ 3.2 Microstructure Analysis

where Cε = lattice strain, Bsize = particle size broadening,
Bstrain = strain broadening, L = crystallite size, K =
dimensionless shape factor (0.9), λ = x-ray wavelength for
the Cu-Kα radiation (1.5406 Å), and θ = Bragg angle (in
degree). Then (1) is multiplied by cos θ to yield:
Kλ
Btot cos θ = 4Cε sin θ + (2)
L with 7.0 mol.% BZO nanoparticles. The increased grain
Hence, by plotting the graph of Btot cos θ against 4 sin θ
(Fig. 2), the lattice strain, Cε of the sample can be obtained
from the slope (gradient) while the crystallite size can be
estimated from the intercept (Kλ/L).
Table 2 shows the crystallite size and the lattice strain for
all the samples. It is apparent that the crystalline size of the
samples added with BZO nanoparticles is bigger compared
to that of the pure sample. Meanwhile, the lattice strain
decreased slightly only from 0.024% (0.0 mol.%) to 0.022%
(7.0 mol.%).
Figure 3 shows the SEM images taken on the fractured
surfaces of the pellets at × 5000 magnification. It can be
clearly seen that all the samples have randomly oriented
grains with irregular shape. Table 2 shows the average
grain size of the samples. The average grain size was
calculated based on 100 grains using the ImageJ software.
The average grain size for the pure Y-123 sample is 0.30
μm and it increased up to 0.50 μm for the sample added
size is probably due to the dispersion of BZO nanoparticles
between the grains of Y-123 that promoted the grain growth
[17].
The EDX spectra in Fig. 3 (insets) confirmed the
presence of yttrium (Y), barium (Ba), copper (Cu), and
oxygen (O) for all the samples. Table 3 shows that the
atomic ratio of Y/Ba/Cu is 1:2:3 with different oxygen
ratios indicating the dominant Y-123 phase for all the
samples. However, the increased atomic ratio for Ba is most
likely due to the increasing unreacted BZO as shown in
the XRD patterns (Fig. 1). No Zr was detected suggesting

Table 3 The atomic

percentages and atomic ratios BZO x (mol.%) Atomic % Atomic ratio Y/Ba/Cu/O
measured from the EDX
spectra for Y, Ba, Cu, and O Y Ba Cu O
elements, respectively
0.0 6.21 9.85 16.37 67.57 1.0:1.6:2.6:10.9
1.0 6.07 12.18 19.57 62.18 1.0:2.0:3.2:10.2
2.0 7.12 14.54 22.66 55.68 1.0:2.0:3.2:7.8
3.0 5.66 12.67 15.33 66.34 1.0:2.2:2.7:11.7
5.0 6.14 14.53 19.34 60.00 1.0:2.4:3.1:9.8
7.0 4.87 13.02 15.90 66.21 1.0:2.7:3.3:13.6
 J Supercond Nov Magn

Fig. 5 Real part of ACS for

Y-123 +x mol.% of BZO 0.0
samples

-0.2
Tc-onset
Tcj

Normalized χ' (a.u.)

-0.4

-0.6

Y-123
Y-123 + 1 mol.% BZO
-0.8
Y-123 + 2 mol.% BZO
Y-123 + 3 mol.% BZO
Y-123 + 5 mol.% BZO
-1.0 Y-123 + 7 mol.% BZO

78 80 82 84 86 88 90 92 94
Temperature (K)

the negligibly small amount of the element beyond the
detection limit of the EDX. Such phenomenon has also been
reported elsewhere in BZO-doped Y-123 films prepared by
a metal organic deposition method using solutions with
trifluoroacetates (TFA) and Zr salts [8].
3.3 Superconducting Properties
Figure 4 shows the temperature dependence of the real (χ  )
and imaginary (χ  ) parts of ACS for all the samples. The
real part (χ  ) of the AC susceptibility (ACS) (Fig. 5) shows
two transitions labeled asTc−onset and Tcj . Tc−onset is due
to transition within the grains (intra-grain) while Tcj is due
to superconducting coupling between grains (inter-grain)
[18]. Table 4 shows that both Tc−onset and Tcj decrease
gradually and slightly only (≤ 1 K) with increasing of
BZO nanoparticles addition from 0.0 to 7.0 mol.%. Such
marginal decrease of Tc−onset is in good agreement with
previous finding [3, 13, 19]. In fact, Tcj remained relatively
unchanged for addition up to 3.0 mol.%. Above the addition
level of 3.0 mol.%, the small decrease of Tcj indicates that
the weakening of intergranular coupling is not severe and
this is most probably due to the increasing impurities at the
grain boundaries of Y-123 samples [20].
The imaginary part (χ  ) of ACS in Fig. 6 exhibits a
broad peak known as coupling peak temperature, Tp , which
corresponds to the hysteretic energy dissiation as a result
of AC losses at inter-grain region. The second peak near Tc
(intrinsic peak) for all the samples is not apparent and this
could be due to a number of reasons such as insufficient
total grain volume and grain sizes of the order of penetration
depth, λ [18, 21]. The Tp value for pure sample is 84.8 K
and it is almost constant up to 3.0 mol.% BZO (Table 4).
However, Tp shifted to lower temperature for 5.0 and 7.0
mol.% BZO additions due to the further weakening of
intergranular coupling between the grains [22]. This is
supported by the decreasing ratio of Tp /Tc−onset as shown in
Table 4 [23, 24].
The value of Josephson’s current, Io , can be calculated
according to the Ambegaokar-Baratoff theory [25] using the
following equation:
 
−8 Tc−onset2
Io = 1.57 × 10 (3)
Tc−onset−Tcj

Table 4 Coupling peak

temperature, Tp , onset critical BZO x (mol.%) Tp (K) Tc−onset (K) Tp /Tc−onset Tcj (K) Io (μA) Jcm (A/cm2 )
temperature, Tc−onset , phase
lock-in temperature, Tcj , 0.0 84.8 90.6 0.935 86.6 31.69 1.88
Josephson current, Io and 1.0 84.9 90.6 0.937 86.5 31.45 1.78
intergranular critical current 2.0 84.5 90.5 0.934 86.5 32.08 1.78
density, Jcm for Y-123 +x
mol.% of BZO samples in 3.0 84.7 90.2 0.939 86.5 34.94 1.86
applied AC field of 0.5 Oe 5.0 82.9 89.8 0.924 85.6 30.56 1.79
7.0 83.6 89.9 0.929 85.8 30.54 1.95
J Supercond Nov Magn
Fig. 6 Imaginary part of ACS
for Y-123 +x mol.% of BZO
samples
Normalized χ" (a.u.)
Table 4 shows that the Io increased up to 3.0 mol.% but
decreased slightly for 5.0 and 7.0 mol.% BZO nanoparticles
addition. The intergranular critical current density, Jcm at
Tp can be estimated using the Bean critical state model [26]
and the relation between the Jcm at Tp and applied magnetic
field, HAC can be written as below [27, 28]:
HAC
Jcm (Tp ) =
(ab)1/2
where 2a × 2b is the cross-section for rectangular bar-
shaped sample. Table 4 shows that the Jcm for the pure
sample is 1.88 A/cm2 at Tp of 84.8 K. As the addition
increased to 7.0 mol.%, Jcm at Tp = 83.6 K is 1.95
A/cm2 . It is anticipated that Jcm can be further increased by
optimization of heat treatment and amount of BZO addition.
4 Conclusion
YBa2 Cu3 O7−δ superconductors with addition of x mol.%
BZO nanoparticles (x = 0.0, 1.0, 2.0, 3.0, 5.0, and 7.0)
were prepared via co-precipitation method. All the samples
were indexed to Y-123 as the major phase and Y-211 as the
secondary phase. Refinement of XRD data also indicated
that the samples have orthorhombic crystal structure. SEM
images showed that the average grain size increased from
0.30 μm for the pure samples to 0.50 μm for BZO
addition of 7.0 mol.%. The onset critical temperature,
Tc−onset decreased slightly only (< 1 K) as a result of
BZO addition. The phase lock-in temperature, Tcj , and
coupling peak temperature, Tp , for all the samples remained
relatively unchanged for BZO addition of up to 3.0 mol.%
Y-123
1.0
Y-123 + 1 mol.% BZO
Y-123 + 2 mol.% BZO
Y-123 + 3 mol.% BZO
0.8 Y-123 + 5 mol.% BZO
Y-123 + 7 mol.% BZO
0.6
0.4
0.2
0.0
78 80 82 84 86 88 90 92 94
Temperature (K)
above which the intergranular coupling between the grains
was weakened. The intergranular critical current density
Jcm at Tp = 83.6 K is 1.95 A/cm2 for BZO addition of
7.0 mol.% compared to Jcm (84.8 K) = 1.88 A/cm2 for
the pure sample. Our future work is focused on further
enhancing Jcm through optimizing heat treatment conditions
and amount of BZO addition.
(4)
Funding Information This work was financially supported by the
Universiti Putra Malaysia through the Putra-Grant (Vote no.:
9552300). N. M. Hapipi would like to acknowledge financial support
from the Ministry of Education Malaysia through the MyMaster
scholarship and Universiti Putra Malaysia under the Graduate
Research Fellowship (GRF).
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