Physica C 463465 (2007) 452454

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Eects of heat-treatment on critical current

of BSCCO-2212 superconductor
a,b,*
J.S. Choi , S.Y. Oh a, B.H. Jun a, H.S. Kim b, H.L. Kim c, O.B. Hyun c, C.J. Kim a,*

a
Nuclear Nanomaterials Development Laboratory, Korea Atomic Energy Research Institute (KAERI), 150 Dukjin-dong,
Yusong-gu, Daejeon 305-353, Republic of Korea
b
Department of Metallurgical Engineering Chungnam National University, Daejeon 305-764, Republic of Korea
c
Advanced Technology Center, Korea Electric Power Research Institute (KEPRI), Daejeon 305-380, Republic of Korea

Available online 2 June 2007

Abstract

Bi2Sr2Ca1Cu2Ox (BSCCO-2212) tubes were fabricated by melt and solidication process. BSCCO-2212 powder compact was melted
in a resistance furnace using a Pt crucible and poured in a rotating cylindrical mold. The solidied BSCCO-2212 tube samples were heat-
treated at various temperatures in oxygen atmosphere. The currentvoltage curves at 77 K of the samples were obtained by transport
measurement, and the microstructure was investigated by scanning electron microscope. It was found that the critical current (Ic) of
the BSCCO-2212 samples was dependent on the heating schedule regarding the grain growth of the BSCCO-2212 plates and the forma-
tion of the second phase.
2007 Elsevier B.V. All rights reserved.

PACS: 84.71.Mn

Keywords: Bi2Sr2Ca1Cu2Ox (BSCCO-2212) tube; Melting; Current density

1. Introduction and the grain alignment of BSCCO-2212 are thought to

High Tc bulk superconductors have been studied to real-
ize the various electrical and power storage applications
such as ywheel energy storage, current lead and fault cur-
rent limiter. To apply bulk superconductors to the electric
power applications, the critical electric current density (Jc)
and the current uniformity should be increased to a certain
level.
Much eort has been made on the enhancement of Jc of
BSCCO-2212 bulk and high Jc was achieved in melt-pro-
cessed bulks [1,2]. Although many factors can aect the
current properties of the BSCCO-2212, the formation
be essential for the Jc improvement. Normally, the Jc value
of the melt-processed BSCCO-2212 was higher than that of
the BSCCO-2212 made by conventional powder sintering
method, where grains were poorly connected [3]. It seems
that good grain connectivity is one of the reasons for high
Jc in the melt-processed BSCCO-2212. The Jc at 77 K of
the BSCCO-2212 bulk exceeded 3000 A due to the dense
structure and the grain alignment [4].
In this study, BSCCO-2212 bulk was made by melting
technique and the eect of heat-treatment on electrical
properties of BSCCO-2212 tube was investigated.

*
2. Experimental
Corresponding authors. Address: Nuclear Nanomaterials Develop-
ment Laboratory, Korea Atomic Energy Research Institute (KAERI), 150
Dukjin-dong, Yusong-gu, Daejeon 305-353, Republic of Korea (J.S.
Bi2Sr2Ca1Cu2O8+d (BSCCO-2212) and 10 wt.% SrSO4
Choi). Tel.: +82 42 868 8024; fax: +82 42 868 8275 (C.J. Kim). powders were mixed by hand milling. The addition of
E-mail address: cjkim2@kaeri.re.kr (C.J. Kim). SrSO4 to BSCCO powder is to improve the mechanical

0921-4534/$ - see front matter 2007 Elsevier B.V. All rights reserved.
doi:10.1016/j.physc.2007.05.036
 J.S. Choi et al. / Physica C 463465 (2007) 452454
properties of the melt-processed BSCCO-2212 bulk and to
control the viscosity of the high temperature melt [5].
The powder mixture was put in a Pt crucible or alumina
crucible, then the crucible was placed at the center of the
electric furnace and was heated to 1200 C. The powder
mixture was fully melted after 2 h holding at 1200 C.
The melt was taken out of the furnace and then poured into
a cylindrical mold rotating at a speed of 2520 rpm, pre-
heated at 550 C for 2 h. For easy separation of the
BSCCO-2212 bulk from the mold, a releasing agent was
sprayed on the inner wall of the cylindrical tube. After
pouring the BSCCO-2212 melt, the mold was furnace-
cooled to room temperature, and then the tube was sepa-
rated from the cylindrical mold. The dimension of the tube
was 30 mm in diameter and 150 mm in length.
The phase formed after the solidication of the melt in a
mold was identied by X-ray diraction as a semi-amor-
phous phase due to the slow kinetics of the melt to
BSCCO-2212 phase. To understand the eect of heat-treat-
ment on the development of microstructure and phase
changes, the tubes were heat-treated at 750850 C for
120 h in oxygen atmosphere.
The currentvoltage curves at 77 K of the BSCCO-2212
bulks were obtained by a four probe method. The critical
electric current (Ic) and critical electric current density
(Jc) were estimated from the IV curves. The phase formed
in the BSCCO-2212 bulks was analyzed by X-ray dirac-
tion (XRD) and scanning electron microscope (SEM).
3. Results and discussion
Fig. 1 shows the BSCCO-2212 tube fabricated by melt
and solidication process. The silver tapes were attached
on both ends of the tube to measure the current properties.
The outer and inner radius. and length of the tube are
30 mm, 26 mm and 150 mm, respectively. The tube surface
was almost smooth, but small voids were often observed
Fig. 1. Photo of the BSCCO-2212 tube fabricated by melt and solidica-
tion process.
453
due to the trapped gas during solidication of the melt.
In addition to the surface voids, cracks were also often
observed, depending on the melting and solidication con-
dition. At an optimized processing condition, with low vis-
cosity of the melt and high preheating temperature for the
mold, cracks were rarely developed.
Fig. 2 shows the IV curves of the BSCCO-2212 tubes
heat-treated at (a) 800 C and (b) 810 C for 120 h. The
voltage drop was measured at four parts of the tubes;
two points near both ends and two points near center to
understand the Ic homogeneity. The maximum Ic of the
tube heat-treated at 800 C was lower than the Ic of the
tube heat-treated at 810 C. The Ic uniformity calculated
from the dierence between the measured value at specic
distance and the end-to-end value for the tubes prepared at
800 C and 810 C were 8% and 12%, respectively. The
average Ic at 77 K of two tubes were 604 A and 832 A,
respectively. The Jc values at 77 K of the tubes prepared
at 800 C and 810 C were 197 A/cm2 and 240 A/cm2,
respectively. Not illustrated here, the tube prepared at
820 C showed the lower current properties than the tube
prepared at 810 C. It implies that the processing window
to achieve a high Ic and Jc is as narrow as 10 C.
Fig. 2. Currentvoltage curves of the BSCCO-2212 tube prepared at
(a) 800 C and (b) 810 C.
454 J.S. Choi et al. / Physica C 463465 (2007) 452454

Fig. 3. XRD patterns of the BSCCO-2212 tubes prepared at (a) 800 C

and (b) 810 C.

Fig. 3 shows the XRD diraction patterns for the sur-

faces of the tubes prepared at 800 C and 810 C. As can
be seen in Fig. 3, main peaks of both patterns are
BSCCO-2212 phase. The XRD analysis result shows the
formation of 2212 phase in both tubes was almost identical.
Fig. 4 shows the SEM images observed from the fracture
surface of the tube prepared at 800 C (a) and 810 C (b),
respectively. As can be seen in Fig. 4a, many plate-like
grains that are considered as the 2212 phase were observed.
The grain morphology observed in this study is similar to
that observed in other literature [6]. The plate-like grains
are also observed in the tube prepared at 810 C, but the
plate-like grains seems to be more uniformly distributed
Fig. 4. SEM fracture surfaces of the BSCCO-2212 tubes prepared at (a)
in the whole sample. Not illustrated here, the microstruc- 800 C and (b) 810 C.
ture of the tube prepared at 820 C was slightly dierent
from the two tubes shown. In addition to the development
of the plate-like grains, many second phase particles Acknowledgement
formed which is thought to give a negative eect on the
current property. This research was supported by Electric Power Industry
R&D program funded by the Ministry of Commerce,
4. Conclusion Industry, and Energy, Republic of Korea.

BSCCO-2212 tubes were made by melt and solidica- References

tion technique using BSCCO and 10 wt.% SrSO4 powders.
The optimum condition to make high Ic BSCCO tube was
studied. The melting and preheating temperature of a mold
were found to be important to get a high Ic; preheating at
550 C for 2 h, and melting at 1200 C with a rotating
speed of 2520 rpm. The BSCCO-2212 tubes prepared at
800 C and 810 C showed critical electric current density
(Jc) at 77 K of 197 A/cm2 and 240 A/cm2, respectively.
The high Jc of the BSCCO tube prepared at higher temper-
ature is thought to be attributed to the enhanced formation
of the 2212 plate-like grains.
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