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A series of samples along the composition lines Bi2+xSr2_A:Cu0>, and Bi2Sr2_xCu0j, have been used to study the structural modulation, chemistry, and superconducting properties of pseudo-tetragonal Bi 2 Sr 2 Cu0 6 (2201). The 2201 phase can be formed from crystallization of thin glassy platelets. The sample displayed a strong crystallographic (00/) orientation which made it possible to determine incommensurate modulations near (00/) reflections using a conventional x-ray 8-28 scan. From the crystallization of the 2201 phase, it was found that structural modulation was intrinsic to the phase, and ordering of the structure required a long time at high temperature. High temperature in situ x-ray diffraction of a 2201 Bi2Sr! 85CuOy platelet showed that the modulation existed at 875 °C in O 2 (r meU « 892 °C in O 2 ). These suggest that the structural modulation cannot be caused solely by oxygen ordering and that metal-ion displacement must be involved. By removing 0.04 to 0.05 oxygen atom per formula unit from Bi 2 Sr 2 Cu0 v and Bi2Sr! . 85 Cu0j,, the c* components of the modulation changed from 0.31 to 0.26 and from 0.38 to 0.31, respectively, while the b* component of the modulation remained approximately 0.2. This demonstrates that oxygen, while not the sole cause, does play a role in the formation of the structural modulation. However, the invariance of bmoi with respect to the change in oxygen content does not support the model that explained the modulation by inserting extra oxygen in the BiO plane. By varying metal-ion concentrations of Bi and Sr we found that both the lattice parameters and the modulation vectors depended more on the Bi/Sr ratio than on the Sr concentration alone. As the Bi/Sr ratio increased from 1.0 to 1.35, the modulation lines moved toward the (00/) reflections. The corresponding superstructural periodicities were calculated to vary from ~ l / 5 b* + 0.32 c* to ~ l / 5 b* + 0.63 c*. Effects of oxygen content and metal-ion concentration on the 2201 phase formation and the superconducting properties will also be discussed.

I. INTRODUCTION Bi based superconducting compounds form a hierarchy of structures described by a generic formula Bi2Sr2Can_iCun02H+4. Since the discovery by Maeda,1 much effort has been made to synthesize single phases of 2212 and 2223 with a well-defined superconducting transition temperature (Tc). Even though the Bi system does not have the volatility problem that exists in Tl based superconducting compounds, it has been difficult to obtain single phases due to intergrowth of two or more phases even in single crystals. Without single phase samples, the precise structural determination and chemistry studies would be very complicated. Pseudo-tetragonal Bi 2 Sr 2 Cu0 6 phase (2201), first discovered by Michel et al.,2 has a unit cell with a « b « 5.4 A, and c ss 25 A.3"6 The superconducting

^Current address: Department of Metallurgical Engineering and Materials Science, Carnegie Mellon University, Pittsburgh, Pennsylvania 15213. 844

http://journals.cambridge.org

J. Mater