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Journal of the Aceh Physics Society (JAcPS), Vol. 4, no. 1 pp. 4-7, 2015 ISSN online: 2355-8229

Synthesis and Microstructure Properties of

(Bi,Pb)2Sr2Ca1Cu2OyCeramic Superconductors
Nurmalita*, Zuraini, Evi Yufita, Fauzi
Department of Physics, Faculty of Mathematics and Natural Sciences, Syiah Kuala University,

Banda Aceh 23111, Indonesia

Received December, 2014, Accepted March, 2015

Properties of (Bi, Pb)2Sr2Ca1Cu2Oyceramic superconductors were prepared by the melt textured growth
methods in order to investigate the effects of the slow cooling time on the microstructure. Phase analysis of the
samples by X-ray diffraction (XRD) has been carried out to assess the effects of the slow cooling time. From XRD
analyses, the addition to the sample of the slow cooling time degrades formation of the high-Tc Bi-2212 phase.
The possible reasons for the observed degradation in the microstructure properties due to the slow cooling
time addition were discussed.

Keywords:Superconductor, melt textured growth, slow cooling

Introduction material increases with increasing time

Sintering Bi-based ceramic superconductors (Nurmalita, 2011). Likewise, it has the general
formula Bi2Sr2Can−1CunOy(n=1, 2 and 3) which was with
discovered in 1987
the critical is very of the Bi-2212 material
temperature
which shows an increase with increasing time
interesting to research because of the superiority of these characteristics (Nurmalita, 2012). In
general, its rate in cooling technology and industrial applications also plays an important role in
power transmission (Akimitsu, J., et al, 1987). Has as is the case with chemical doping in the formation of
It is known that this superconducting material high critical temperature superconducting materials.
has low power passing characteristics, is able Crystallization of the dominant material occurs during
to carry large magnetic fields and currents, the processslow cooling. Increased cooling rate
in addition to superior optical properties and is known to increase the volume fraction of other Bielectronic
crystals. Referring to the composition of 2212 and enhancing the formation of its chemical Tc phase, this
Bi-based superconductor consists of low in materials made using the solid state
three different phases, namely the Bi-2201 phase reaction method (Cetinkara et al, 2003). In this
n=1, Tc≈20 K), Bi-phase2212 (n=2, Tc≈85K)and Bi paper we report how the cooling rate
phase 2223 (n=3, T≈110 K) (Ghahfaroki, SEM et al, influences the microstructural properties of Bi
2010). In this Bi-based family, the Bi-2212 phase is superconducting samples1.6PB0.4Sr2Ca2Cu3Oy.
more interesting to study due to its better
thermodynamic stability properties, lower weak- Methodology
link problems (Berdan, O., et al, Sample synthesis and XRD pattern recording
2011), and relative cation doping is not carried out in the FMIPA Materials Physics laboratory which
affects the stoichiometry of the atomic content Syiah Kuala University. Samples are made by
Oxygen in the language. Under different sintering methodmelt-textured growth. The starting material
conditions, differences in state characteristics occur consists of oxides (Bi2O3, Pb3O4, and CuO) and
superconductive of the pure compound BiSrCaCuO carbonate (SrCO3, CaCO3) mixed with or
doped with Pb, namely BiPbSrCaCuO composition nominal Ms1.6PB0.4Sr2Ca2Cu3Oy.
(Yilmazlar et al, 2007). Research on influence The mixture was calcined at 800°C
length of sintering time to volume fraction for 24 hours. Furthermore, the temperature of the Bi-2212
superconducting mixture made using the method lowered to room temperature then crushed
melt texture-growthshows that purity manually. The resulting powder is then pressed
4

* Corresponding Author:nurmalitapatra@unsyiah.ac.id http://www.jurnal.unsyiah.ac.id/JAcPS

Journal of the Aceh Physics Society (JAcPS), Vol. 4, no. 1 pp. 4-7, 2015 ISSN online: 2355-8229

into pellets. The pellets are then sintered at a that the Bi-2212 phase formed in the sample is
temperature of 930oC until completely melted and partially oriented. The results of calculating the
then subjected toslow cooling. Timeslow coolingFor volume fraction of Bi-2212, the percentage of oriented
each sample it was chosen differently, namely for the phase and impurity are shown in Table 1. The sample
first sample for 130 hours and for the second sample with a slow cooling time of 140 hours had a volume
for 140 hours. Finally, XRD pattern analysis and SEM fraction value of 53.1%, the percentage of oriented
photos were carried out on both samples. phase was 15.3% and the impurity obtained was 46.
9%. The impurities formed are the Bi-2201 phase and
Results and Discussion the Bi-2223 phase.
1. XRD spectrum of a sample with a slow cooling
time of 130 hours.
The XRD pattern for the sample with slow
cooling of 130 hours is shown in Figure 1.
Based on the XRD pattern shown in Figure 1, it
can be seen that most of the peaks have hkl
values for the Bi-2212 phase. The Bi-2212
phase formed was 71.6% and the others were
impurities such as the Bi-2201 phase and the
Bi-2223 phase. The spectrum peak which has
the index hkl=00l with l an even number,
indicates that the Bi-2212 phase formed in the
sample is oriented. The results of calculating
Figure 1. XRD spectrum of samples with
the volume fraction, percentage of oriented
slow cooling time 130 hours.
phase and impurities are shown in Table 1.
From the results of these calculations it
appears that a slow cooling time of 130 hours
produces a Bi-2212 phase volume fraction
value of 71.6%, the percentage of oriented
phase is 44.3% and impurity of 28.4%.

Table 1. Recap of Calculation Results Data

Sample characteristics
Ms2Sr2 Ms2Sr2
Sample Name
Ca1Cu2Oy Ca1Cu2Oy
Slow cooling (hours) 130 140
Final temperature (⁰C) 820 815
P (%) 44.3 15.3 Figure 2. XRD spectrum of Bi-2212 sample
FV (%) 71.6 53.1 with a slow cooling time of 140 hours
Impurity (%) 28.4 46.9
3.Comparison of XRD pattern results for samples with
2. XRD spectrum of the sample with a slow cooling slow cooling times of 130 hours and 140 hours
time of 140 hours From the results of this research, it can be seen that the
XRD pattern for samples withslow cooling 140 formation of the Bi-2212 phase from both samples is
hours are shown in Figure 2. XRD pattern with influenced by timeslow cooling, where this can be seen from
timeslow cooling140 hours shown in Figure 2, it the calculation results of the volume fraction values, the
can be seen that some of the peaks that have percentage of oriented phase and different impurities for
value have appearedhklfor the Bi-2212 phase. the two samples which are shown in Table 1. The results of
Spectrum peaks that have an index hkl=00l with l the calculation of the volume fraction values and the
an even number indicating anyway percentage of oriented phase obtained in

* Corresponding Author:nurmalitapatra@unsyiah.ac.id http://www.jurnal.unsyiah.ac.id/JAcPS

Journal of the Aceh Physics Society (JAcPS), Vol. 4, no. 1 pp. 4-7, 2015 ISSN online: 2355-8229

the sample with a slow cooling time of 130 hours peak hkl=00l which has an effect on the value
shows a better value than the sample overall oriented phase percentage. This is in
with a slow cooling time of 140 hours, namely 71.6% accordance with the results obtained in previous
and 44.3%, and the lowest impurity was also research even though the synthesis method is
obtained in the sample with a slow cooling time of different (Yuliati, T., 2010)
130 hours, namely 28.4%.
Based on the results of XRD pattern analysis Conclusion
calculations, it can be concluded that the longer the slow From the results of this research it can be concluded that
cooling time, the lower the volume fraction and oriented the BSCCO phase 2212 superconducting material has been
phase percentage values and the lower the impurity. successfully made using the methodMelt Textured-
increase. Based on previous researchGrowth, where the longer the slow cooling timeslow cooling
is directly proportional to the volume fraction and in
percentage
the sinteringofprocess,
orientedthephase, will of oriented
percentage
phase and volume fraction become lower as well
but this is achieved until the slow impurity increases. For a cooling value of 120 hours (Nurmalita,
2002). After the percentage of oriented phase and volume fraction, this research was carried out
by varying high levels were obtained from samples with a slow
slow cooling time of 130 hours and 140 hours then the cooling time of 130 hours, namely 71.6% and 44.3%
volume fraction and phase percentage values and low impurities were also obtained from samples
orientation is decreasing. As for the one with a slow cooling time of 130 hours, that is 28.4%. resulting
in the volume fraction value decreasing or
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* Corresponding Author:nurmalitapatra@unsyiah.ac.id http://www.jurnal.unsyiah.ac.id/JAcPS

Journal of the Aceh Physics Society (JAcPS), Vol. 4, no. 1 pp. 4-7, 2015 ISSN online: 2355-8229

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* Corresponding Author:nurmalitapatra@unsyiah.ac.id http://www.jurnal.unsyiah.ac.id/JAcPS