Researchers report the measurements of the I(sub c)(T) of the 102 K phase. They also discuss briefly the composition of the lattice parameters and the ac susceptibility relation to the grain size and microstructure

Kostadinov, I. Z.

Mateev, M.

Michov, M.

Skumriev, V.

Tsakin, E.

English

NASA Technical Reports Server

N92-21627
NOVEL SUPERCONDUCTING PHASES OF TL-BASED
COMPOUNDS
I.Z.Kostadinov, M.Mateev, M.Michov, V.Skumriev and E.Tsakin
Faculty of Physics, Sofia University, 1126 Sofia, BULGARIA
1. Introduction
The interest in novel superconducting compounds has been attracted, recen-
tly, by the Pb-containing High Temperature Superconductors (HTS) [1-5]. The
larger part of work has been done on Bi-Pb type HTS [6,7]. The Tl-based HTS,
howeever, are also of considerable importance because of their highest critical
parameters (T¢, He) [8,9]. Due to the dangerous properties of TI the research
in this area is progressing more slowly. The list of the stable phases of TI-Ba-
Ca-Cu-O HTS is still incomplete. The T1-Pb firs were studied mostly in the
compound TI-Pb-Sr-Ca-Cu-O [10] and less in the family T1-Pb-Sb-Ca-Ba-Cu-O
[11]. The substitution of TI with Pb is intended to stabilize some phases with
high To. We found phases with Te ffi 82, 90, 102 and 121 K. Here we report
the measurements of the I¢(T) of the 102 K phase. We also discuss briefly the
influence of the composition on the lattice parameters and the a.c. susceptibility
relation to the grain size and microstructure.
2" Experiment_!
The nitrates solution of the metals TI, Pb, Sb, Ba, Ca, Cu of starting
composition TIo.TaPbo.28bo.oaCa_Ba3Cu4 was dried and decomposed at 780°C.
Pellets were prepared under 1-2 kbars pressure and annealed at different
temperatures from S20°C to 915°C. The highest critical temperature phase was
found to be the 121 K. It was prepared by a 3 rain annealing at 8910C in oxigen
atmosphere. The lattice parameters of this tetragenal phase are a = b -- 3.84
A and c = 31.96 ),. The average composition of the pellets of this type found
by SEM analysis was (TI, Pb)l -Ca2 -Ba4.1 -Cua.e -O, the TI-Pb ratio
being 4.4. We should mention here that a slight change in the composition
lead to different e-parameter of the tetragonal elementary cell. For example
the composition (TI + Pb h - Cau.s - Ba2.s - Cu4.4 - 0 with the ratio TI:Pb
equal to 3.17 has a cell length of 32 )_. The X-ray powder diffraction pattern is
practically the same as the one of the first mentioned compound but the peak at
low angles being quite well pronounced is slightly displaced. We mention here
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this observation in order to illustrate the similarity of the T1-Pb system to solid
solutions compounds.
We turn next to another phase with lower Tc = 102 K but the same
starting composition prepared by annealing first at 820°C for 3 rain in oxigen
atmosphere. After quenching and grinding the pellet was annealed for 6 rain at
915°C. The result was an remarkably homogeneous sample with sharp transition
at Te - 102 K. This phase was studied by SEM and in the/_m range it has the
microstructure shown on Fig. 1.
Fig. 1.
SEM microstructure of the 102 K ceramic sample. Large voids are seen and
are absent
This crystals free structure is closely related to the a.c. susceptibility of the
sample measured at different magnetic fields.
3. A.C.Susceptibility
The real X_ and imaginary Xn parts of the magnetic susceptibility were
measured simultaneously at different temperatures upon warnfinff. The s.c.
field amplitude was between 24 A/m and 800 A/m, the frequency being 10 Hz.
160 ORIG!I_tAL PAC'_
BILACK AND WHITE PHOTOGRAPH
The sample was in the form of a prism (2 × 4 × 10 ram). In order to minimize
the demagnetization effect, the a.c. field was chosen to be parallel to the length
of the sample. Corrections for the demagnetization were performed [12]. On
2b the temperature dependence of the susceptibility XI andFig. 2a and Fig.
x#sre presented.
0.2 i
0.0
-0.2
-0.4
-0.6 -,
-0.8 -
-1.0
-1.2 li iillilil li=l I i iil I Iltill I III lili lil iii ill lllli li lilli I lii
0.00 20.00 40.00 60.00 80.00 100.00 120.00
T(K)
Fig.2a.
Temperature dependence of X# measured at fields 24 A/m - curve a; 240 A/m -
curve b; 2400 A/m - curve c and 8000 A/m - curve d
The complete diamagnetic shielding is demonstrated by the value .1 of XI
(or Xs = 0) below 60 K at low magnetic fields. At higher fields, however, the
situation is entirely different.
The x_(T) curves are well above the low field one with complete absence of
common part. Two stage behaviour in X_ is not seen also, in contrast with the
typicalceramicHTSlike YBaOuO.
161
0.25
0.20
0.15
: 0.10
x
0.05
-0 O0
.!
-0.05 ,iii,ii,,i,,,,,,,,,,,,,,,,,Jil,,,,,,,,,l*,*,,,,,,i,,,,,,,,,
0.00 20.00 40.00 60.00 80.00 100.00 120.00
T(K)
Fi .
Temperature dependence of X# measured at the same fields as X' (Fig. 2a)
The second peak in X" is also absent in agreement with the xI(T) depe-
ndence. The _um value of X# (in fields between about 24 A/m and about
2400 A/m), at which the magnetic field penetrates completely the coupling ma-
trix is in agreement with the larger part of the data reported for ceramic samples
[13]. It k worth mentioning that strong field dependence of the X# mswlm.m
suggesting usually Joseplmon type grains coupling was not obeerved, at least
in the fields range of measurement. In principle, the observed behaviour can
happen in the case when the contributions to the susceptibility of the grains
and the coupling matrix are not well temperature-separated. To our knowledge
this situation is not valid in our case.
The a.c. susceptibility data were used recently by several authors to estimate
the transport critical current. Based on Kim's critical state model a method for
determining the temperature dependence of the intergranular critical current
has been developped by Chen et al.[12]. Using this method and neglecting
the volume fraction of the grains the temperature dependence of the transport
critical current It(T) has been reconstructed of Fig. 3 from the measured
162
susceptibilities.
350.0
300.0
250.0
CN
"_'150.0
100.0
50.0
0.0
%
'N'N"
0 20 40 60 80 1O0 120
T(K)
Fig. 3.
Critical current temperature dependence of the 102 K phaso.
In conclusion we briefly enumerate the results reported here. First we
mention the observed variety of phases of the superconducting compound
TI-Pb-Sb-Oa-Ba-Ou-O. Among them we concentrated our afention here
on the 102 K phase, which being homogeneous appears to have monocrystalline-
like micmstructure, complete diamagnetic shielding and specifle behaviour of
the complex susceptibility (Fig. 2 a,b). Final},, we mention the reconstruction
of the critical current temperature dependence It(T) shown on Fig. 3 from the
measured susceptibilities.
163
.o
3.
4.
w
1
1
8.
9.
10.
11.
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Novel superconducting phases of Tl-based compounds

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