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Authors Accepted Manuscript

Enhancement of magnetic relaxation behavior by

texturing in Bi2212 superconducting rods

M. Ozabaci, O. Kizilaslan, G. Kirat, M.A. Aksan,

M.A. Madre, A. Sotelo, M.E. Yakinci


PII: S0272-8842(16)00307-2
DOI: http://dx.doi.org/10.1016/j.ceramint.2016.02.046
Reference: CERI12237
To appear in: Ceramics International
Received date: 8 November 2015
Revised date: 29 January 2016
Accepted date: 7 February 2016
Cite this article as: M. Ozabaci, O. Kizilaslan, G. Kirat, M.A. Aksan, M.A.
Madre, A. Sotelo and M.E. Yakinci, Enhancement of magnetic relaxation
behavior by texturing in Bi2212 superconducting rods, Ceramics International,
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Enhancement of Magnetic Relaxation Behavior by Texturing in Bi-
2212 Superconducting Rods

M.Ozabaci1*, O. Kizilaslan2, G. Kirat3, M.A. Aksan3, M.A. Madre4, A. Sotelo4, M.E. Yakinci1,2

Scientific and Technological Research Center, SEM/EDX Lab. nn University, Malatya, Turkey
Faculty of Engineering, Department of Biomedical Engineering, nn University, Malatya, Turkey
Faculty of Arts and Sciences, Department of Physics, nn University, Malatya, 44280, Turkey
Instituto de Ciencia de Materiales de Aragn (ICMA), CSIC-Universidad de Zaragoza, Maria de Luna,
3, 50018, Zaragoza, Spain

*Corresponding author. Tel.:+90 4223774956. E-mail address: muratozabaci@yahoo.com



Time decay of magnetization, known as magnetic relaxation, is crucial for both

fundamental and applied point of view in bulk high temperature superconductors (HTS) by
setting the limits to the HTS devices stability. Melt-processed Bi2Sr2Ca1Cu2-xGaxO8+ rods (Bi-
2212, x = 0, 0.1) were used to study the effect of both grain alignment and substitution on
the samples critical current density, relaxation and pinning behavior. The magnetic field has
been applied both perpendicular and parallel to the rods growth axis to determine the effect
of grain alignment. It has been found that Ga substitution reduces grains orientation and
sizes leading to lower magnetic properties. The peaks of the curves, which indicate the
temperature dependence of the samples magnetic relaxation rate (S), have been observed in
the 7-35 K temperature range. Characteristic pinning energy (Ue/kB) of samples was
determined using the formalism developed by Maley. The change of pinning energy as a
function of magnetization has been found to be exponential between 3 and 60 K, which is in
agreement with the collective creep theory.
Keywords: BSCCO superconductors, Magnetic relaxation, Pinning energy, Texturing, Laser
processing, Alignment.

1. Introduction

Technological applications of high temperature superconductors (HTSs) require both

high critical current density (Jc) and high critical field (Hc2). These two parameters are closely
related with the high anisotropic nature of HTSs. HTSs texturing aims to increase Jc and Hc2
and decrease anisotropy by strengthening the intergranular junctions, leading to the
enhancement of superconducting currents [1-4]. Floating zone, melt casting and hot forging
routes are among the most applied methods for texturing HTSs [5-7]. Introduction of
artificial defects, with sizes matching the coherence length, is another method for raising Jc
values. These defects can be produced by doping, cation substitution, or ion irradiation,
producing nanometric ones in the first two cases or columnar defects in the last approach
[8-13]. Taking into account these different possibilities, it has been reported that properly
processed HTSs can reach critical current densities as high as 106 Acm-2 below 77 K [14].
Magnetic relaxation properties of high temperature superconductors are another
critical issue that can significantly affect superconductors magnetic performance envisaging
technological applications. The main source of magnetic relaxation is the magnetic flux lines
motion by thermal activation or, when they are at ultralow temperatures by quantum
tunneling of vortices [15, 16]. Magnetic relaxation studies on HTSs have been mostly
performed to elucidate vortex dynamics and related flux pinning parameters in the materials
[17-19]. HTSs doping using different types of impurities (magnetic or nonmagnetic), as well
as various fabrication and measurement conditions, have often been utilized to tune up their
pinning properties. These studies have shown that grains connectivity and alignment
influence not only Jc, but also the pinning and, in turn, the materials relaxation behavior [20-
In this study, the Laser Floating Zone (LFZ) technique was used to fabricate pure and
Ga-doped Bi-2212 superconducting ceramics in form of long cylindrical rods with 2 mm
diameter. The main goal of this work is determining the magnetization decay with time and
establishing the magnetic relaxation rate as a function of the applied magnetic field and
temperature. Additionally, the dependence of the effective pinning energy, Ue, on the
magnetization will be studied to understand the vortex dynamics in the LFZ rods.

2. Experimental
Bi2Sr2Ca1Cu2-xGaxO8+ (x = 0, 0.1) powders were prepared by the classical solid state
route from commercially available Bi2O3 (Panreac, 98+ %), SrCO3 (Panreac, 98+ %), CaCO3
(Panreac, 98.5+ %), CuO (Panreac, 97+ %) and Ga2O3 (Alfa Aesar, 99.99 %) powders. The
powders were weighed in the appropriate proportions, mixed, and ball-milled using agate
balls and acetone media for 30 min at 300 rpm to obtain a homogeneous mixture. The
obtained suspension was dried using IR radiation in order to totally evaporate the acetone.
The resulting mixture was then subjected to a two step thermal treatment consisting in
heating at 750 oC and 800 oC for 12 h, with an intermediate manual milling. After cooling, the
powder was ground and isostatically pressed at approximately 200 MPa in form of cylinders
(1.53 mm diameter and 120 mm long), following the procedure described in previous works
The obtained cylinders were subsequently used both as feed and seed in a LFZ
system described elsewhere [25]. The texturing process was performed using a continuous
power Nd:YAG laser ( = 1,064 nm), under air, and 15 mm h-1 growth rate. Due to the fact
that Bi-2212 compounds melt incongruently, after laser processing it is necessary to perform
a thermal treatment to recover the Bi-2212 superconducting phase. This annealing process
consisted in two steps: 60 h at 860 OC to produce the Bi-2212 phase from the secondary
ones, followed by 12 h at 800 OC to adjust the oxygen content and maximize electrical
properties and a final quench in air to room temperature [26]. The so produced bars were
finally cut to obtain samples having the adequate dimensions for their characterization.
Phase analysis has been performed by powder XRD utilizing a Rigaku RadB X-ray
powder diffractometer (Cu K radiation) with 2 between 5O and 65O. Magnetic hysteresis
and the time decay of magnetization were measured using a 9 T Quantum Design PPMS
system. The magnetic hysteresis cycles were determined between 8 T at 5 and 25 K.
Magnetic relaxation experiments were carried out cooling the sample to the desired
temperature under zero magnetic field (ZFC). At that temperature, magnetic field was
applied to the sample, kept constant for 500 s, and measuring the decrease of magnetization
as a function of time. This process was repeated at several temperatures (3, 4, 5, 7, 10, 15,
20, 30, 40, 50, 60 K) at a fixed 1500 Oe applied magnetic field, using both perpendicular and
parallel orientations with respect to the growth axis.

3. Results and Discussion
3.1 Critical current density
Figure 1 displays the magnetic critical current densities, Jcmag, of samples as a function
of the applied magnetic field at two different temperatures, doping levels and applied
magnetic field directions. Jcmag values have been calculated by using Beans critical state
model [27]:

where M is the width of the magnetization loop at the applied magnetic field and d is the
cylindrical sample diameter, assuming supercurrent flow within the whole sample. The
highest Jcmag values, 4.63x105 Acm-2 and 2.19x105 Acm-2 have been obtained in the x=0.0 and
x=0.1 Ga-substituted samples, respectively. The magnetic field dependence of Jcmag of all the
samples displayed a decreasing trend when the magnetic field was increased, independently
of the Ga content and the samples orientation. Moreover, Ga substitution led to Jcmag values
around one half of the determined in unsubstituted samples. Additionally, Jcmag is decreased
when the temperature is increased, as expected.
The decrease of Jcmag with Ga substitution can be explained considering the XRD
spectra shown in Figure 2. In this figure, it can be clearly observed that the major peaks
correspond to the Bi-2212 phase in all cases. On the other hand, Ga-addition promotes the
formation of small amounts of Bi-2201 phase. Therefore, it can be concluded that Ga
introduction decreases the Bi-2212 phase proportion by promoting the formation of the low-
Tc secondary phase, Bi-2201. Since the coupling of superconducting carriers occurs in Cu-O
planes, a substitution for the Cu directly affects the superconducting correlation in the
system. Therefore, it can be deduced that the formation of the Bi-2201 due to Ga
substitution might cause the break-up of singlet cooper pairs (pair breaking effect).
Magnetic anisotropy can be easily observed when the magnetic field is applied in
different directions, as it was illustrated in Figure 1. As a consequence, it is clear that Jcmag is
higher when the field is perpendicularly applied to the growth axis of the rod, compared
with the parallel one. The reason of this difference is due to the fact that the LFZ technique
provides well aligned grains with ab-planes parallel to the growth direction. Since good
texture was obtained along the axial direction, Jcmag easily flows in this direction while it is

decreased when it has to circulate around the rod. Moreover, the behavior of Jcmag depends
not only on the applied field direction but also on the measurement temperature. The
difference on parallel and perpendicular Jcmag at 5 K significantly decreases at 25 K, due to
the increased thermal energy in the structure. This energy degrades the pinning ability of
samples and decreases the alignment effect on Jcmag values.
The samples texture is illustrated in Figure 3, where SEM images of the different
samples are shown. These images show very similar microstructure to the previously
obtained in similar systems [28]. Moreover, when comparing both micrographs, it can be
easily seen an increased grain misorientation together with a decrease in their sizes when Ga
is added. This result is in agreement with the decrease of the Jcmag upon Ga substitution.

3.2 Magnetic relaxation investigations

Figure 4 shows the time dependence of non-equilibrium magnetization in the two

different samples orientations. In the figure, it can be observed that magnetization is
changed almost linearly with , as expected.
The slope of curve allows determining the normalized magnetic
relaxation rate: , which lets understanding the vortices motion in
these samples. The temperature dependence of magnetic relaxation for 1500 Oe applied
magnetic field, as a function of samples orientation, is displayed in Figure 5. Due to the non-
linear behavior of S, the relaxation cannot be explained using the thermally activated flux-
creep theory proposed by Kim-Anderson. A detailed analysis of Bi-2212 single crystals
relaxation behavior can be found in Ref. [29].
The sharp peak observed in the S-T curve corresponds to the transition between two
different pinning regimes. The pinning of individual flux lines takes place below the
temperature at which the S-T curve reaches the maximum value. A single vortex line pins to
point defects with a certain characteristic energy. Above the temperature of this maximum,
the collective pinning of small flux bundles begins and gradually grows into large bundles.
Moreover, in the figure it can be observed that the temperature at which this maximum
value appears is modified with sample orientation with respect to the applied magnetic field.
It has been found that perpendicular orientation shifts this maximum from 7 K (for the
parallel one) to around 35 K. This difference is due to fact that the ab-planes of grains allow

larger shielding currents than the ones in the c-direction (see Figure 6a). As mentioned
previously, LFZ texturing causes an important grain growth and their alignment along the
growth axis. As a consequence, the number of grain boundaries along this plane is greatly
reduced, leading to the increase of Jc along the growth axis and thus producing higher
screening currents (electrical current whirling around each flux line). In the case of the field
parallelly applied with respect to the ab-plane, the current mostly flows along the c-axis and
encounters a higher number of grain boundaries due to the intrinsic nature of Bi-2212 phase
(see Figure 6b). The preferential growth of this phase is along the ab-plane, which allows the
production of grains easily exceeding 100 m in the a-, or b-direction using the LFZ
technique [30]. On the other hand, they are in the range of tenths of nm in the c-direction
producing a drastic raise on the number of grain boundaries which cause a decrease of Jc in
this direction.
These intrinsic properties of Bi-2212 phase clearly explain the higher peak value
when the field is applied perpendicular to the growth direction. The J dependence as a
function of pinning energy has been determined in previous works [21]. It is well known
from collective creep theory that the pinning energy is nonlinearly proportional to J. In this
case, it can be deduced that the grain alignment causes stronger pinning energy, leading to
an increase of temperature at which the peak in S-T curve appears.
In order to investigate the effect of grain alignment on the pinning energy, U(J), it has
been calculated using Maley's method, which has been demonstrated to be adequate to
calculate the effective pinning energy, Ue, from the experimental data [31]:

| |

where A is a time independent constant which is a function of the average hopping velocity,
kB is Boltzman constant and T is the measurement temperature. In this study, the A value
has been taken as 18 in agreement with the data obtained in previous works [32,33]. A
correlation between the characteristic pinning energy, Ue/kB, and magnetization, M, is
shown in Figure 7. In this figure, it can be easily seen that the pinning energy is increased
when the magnetization is decreased. The decay of with increasing magnetization is
almost exponential and it is in good agreement with the collective creep theory [15]. It is
worth mentioning that Ue/kB is higher when the applied field is perpendicular to the rod

growth axis, which is consistent with the previous discussions. On the other hand, in order to
determine if these results are reproducible, a second set of data are presented in Figure 7b
for the x=0.1 Ga-substituted sample. As it can be easily observed, Ga-substitution is
detrimental for the magnetic properties and the pinning energy, as expected from the
previous results. Although Ga substitution was expected to produce better pinning
properties (by formation of small, non-superconducting phases which could act as effective
pinning centers), when compared to undoped Bi-2212 [34,35], it has been found that the
texture degradation and the formation of higher amount of low temperature Bi-2201 phase
avoid the possible pinning improvements promoted by Ga doping.

4. Conclusion

In this work, magnetic relaxation experiments were carried out to investigate the
vortex dynamics in Bi-2212 textured rods. The Jc dependence with the grain alignment was
also investigated in detail. A clear magnetic anisotropy has been observed in all the samples,
which show different properties as a function of the applied field direction (parallel or
perpendicular to the growth axis). This effect can be clearly observed due to the good grain
orientation (ab-plane parallel to the growth direction) obtained when the samples are
processed through the LFZ method. These characteristics are clearly reflected in the
microstructural observations. On the other hand, it has been found that Ga substitution
leads to the decrease of the superconducting characteristics of samples, inducing grains
misalignment, smaller sizes and higher amount of secondary phases. In spite of these issues,
the texturing process has been shown to be a crucial tool to improve the magnetic relaxation
properties. The peak in S-T curves has been shifted from 7 K to 35 K, for parallel and
perpendicular orientations, respectively. In addition, it was found that pinning energy
follows a nonlinear J-dependence, as expected from the collective creep theory, and that the
characteristic pinning energy was increased by texturing.

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Figure 1. Magnetic field dependence of magnetic critical current density, Jcmag, in
Bi2Sr2Ca1Cu2-xGaxO8+ textured rods, for x a) 0; and b) 0.1, at 5 and 25 K between 08 T
applied field.

Figure 2. Powder XRD patterns of Bi2Sr2Ca1Cu2-xGaxO8+ textured rods, for x a) 0; and b) 0.1.

Figure 3. SEM images of longitudinal polished cross sections performed on Bi2Sr2Ca1Cu2-

xGaxO8+ textured rods, for x a) 0; and b) 0.1.

Figure 4. Time dependence of the non-equilibrium magnetization | | measured under
H=0.15 T at different temperatures. Magnetic field was applied both a) perpendicular ()
and b) parallel (//) to the growth axis of the undoped textured rods.

Figure 5. Temperature dependence of the normalized magnetic relaxation rate, S, under

H=0.15 T applied magnetic field along the two different directions of the undoped textured

Figure 6. Schematic representation of the grain orientation, applied magnetic field and
critical current flowing through the textured rods.

Figure 7. Characteristic pinning energies, of Bi2Sr2Ca1Cu2-xGaxO8+ textured rods, for

a) 0; and b) 0.1, as a function of magnetization along the two different applied magnetic field
directions at several temperatures.