Physica C 212 (1993) 271-273
North-Holland
PHYSICA
Increase of Tc in HgBa2CuOy by reducing treatment
Makoto Itoh, Ayako Tokiwa-Yamamoto, Seiji Adachi and H. Yamauchi
Superconductivity Research Laboratory, lnternationaISuperconductivity Technology Center, 10-13Shinonome l-chome, Koto-ku.
Tokyo 135, Japan
Received 13 May 1993
The superconductivity of HgBa2CuOr annealed in various reducing as well as oxidizing atmospheres was investigated. The as-
sintered HgBa2CuOespecimens prepared by solid state reaction starting with mono-oxides of Hg, Ba and Cu exhibited supercon-
ductivity at 90 K. It was found that the superconductivity critical temperature (To) increased up to 96 K after a reducing treat-
ment of the as-sintered specimen, whereas annealing of the specimen in high-pressure oxygen gas resulted in a decrease of To.
1. Introduction
Since the discovery of high-To superconducting
cuprates [ 1 ], many studies on a variety of related
compounds have been reported. It has been revealed
that the two-dimensional CuO2 sheet is essential for
high-Tc superconductivity, and Tc's are dependent
on various factors such as the number of CuO2 sheets
between the charge reservoir blocks (e.g. (Bi-O)2,
T1-O, Cu-O chain), the carrier concentration in the
sheet and so on. One of the most important factors
is the coordination number of the Cu ion in the sheet.
The values for Tc of superconducting cuprates which
contain CuO6 octahedra sheets are ~40 K, except
for that of TIzBa2CuO6, i.e. To~90 K [2,3].
Putilin et al. [ 4 ] synthesized the Hg-based "1212"
cuprates, HgBa2LnCu207 (Ln = La, Nd, Eu, Gd, Dy,
Y) and demonstrated the utility of a Hg-O mono-
layer as a new charge reservoir block. Recently, they
found that a Hg-"1201" cuprate, HgBa2CuOy,
showed superconductivity at 94 K [ 5 ]. This value of
T~ is as high as that of TIzBazCuO6 compared with
those of other cuprate superconductors which con-
tain CuO6 octahedra sheets. They investigated its
crystal structure by X-ray powder diffraction, and
oxygen content, y, by iodometric titration. The Hg
ion in HgBazCuOy was found to have a "stick"-type
coordination, i.e. coordination number=2, and the
oxygen content of the sample, y, was determined to
be ~4.08. They speculated that the excess oxygen
ions of 0.08 per formula unit were located in the Hg
layer and introduced holes into the CuO2 sheets for
superconductivity to occur. However, Putilin et al.
did not report superconducting properties of other
samples with different amounts of oxygen. As a pre-
liminary study, we investigated the post-annealing
effect on the superconducting properties of Hg-
BazCuO.v samples in various atmospheres.
2. Experimental
Samples with a stoichiometric nominal composi-
tion of HgBa2CuOy were prepared by a conventional
solid state reaction method using powders of HgO
(yellow, 99.99%), BaO (99%) and CuO (99.99%).
Mixing was performed in a dry box to prevent the
powders from absorbing CO2 and moisture. Pelle-
tized samples were placed in a gold tube and then
encapsulated in a quartz tube evacuated to a pres-
sure of approx. 10 -4 Torr. The samples were heated
at 700-750°C for 15-60 min. Subsequently, the
samples were annealed for 6 h in flowing Ar gas or
in high-pressure oxygen gas of 270 arm. The prod-
ucts were examined by X-ray powder diffraction
(XRD) with Cu Kct radiation, and the unit cell di-
mensions (for the resultant Hg-" 1201" phase) were
determined by a least squares method. Weight
changes of the samples before and after the anneal-
ing were checked. The DC magnetic susceptibility
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