Physica C 357±360 (2001) 568±571 www.elsevier.com/locate/physc Magneto-optical imaging of vortex lattice melting transition in Bi2Sr2CaCu2O8y T. Tamegai *, M. Yasugaki, K. Itaka, M. Tokunaga Department of Applied Physics, The University of Tokyo, 7-3-1 Hongo, Bunkyo-ku, Tokyo 113-8656, Japan Received 16 October 2000; accepted 25 November 2000 Abstract Magneto-optical dierential imaging technique is applied to the observation of the vortex lattice melting transition in Bi2 Sr2 CaCu2 O8y . Contrary to the naive expectation, the nucleation of the vortex liquid paddle occurs in a rather inhomogeneous manner. The front of the vortex solid±liquid interface propagates re¯ecting the intrinsic inhomogeneities of the crystal. Direct compositional mapping of the constituent atoms indicates that the change in the chemical composition have some correlation with the behavior of the vortex solid±liquid interface. Changes in the superconducting parameters due to the variation of the local doping level could be the origin of such an eect. Ó 2001 Elsevier Science B.V. All rights reserved. PACS: 74.72.Hs; 74.60.Ge; 74.80.-g Keywords: Magneto-optics; Vortex lattice melting; Bi2 Sr2 CaCu2 O8y 1. Introduction Extensive studies of the vortex matter phase diagram in high temperature superconductors have clari®ed the details of the vortex states [1]. Thermal ¯uctuations drive the vortex lattice to melt into the vortex liquid states at the ®rst-order phase transition [2,3]. In the case of Bi2 Sr2 CaCu2 O8y (BSCCO), the vortex lattice melting transition (VLMT) occurs at low ®elds because of high anisotropy parameter [2], and hence the transition could be aected by many factors such as the geometrical barrier [4] and the disorder in the crystals. How the actual VLMT proceeds over * Corresponding author. Tel./fax: +81-3-5841-8886. E-mail address: tamegai@ap.t.u-tokyo.ac.jp (T. Tamegai). the whole crystal in the presence of such factors would be of great interest. However, this is a rather challenging task, because the change in physical parameters accompanied with the VLMT is very small. Magnetic measurements such as using scanning Hall probe microscope (SHPM) could provide important information. Coexistence of the solid and liquid vortex states is observed using this technique [5]. However, the typical size of the crystal is beyond the scanning range over which SHPM can reliably give meaningful information. Magneto-optical (MO) observations of the magnetic induction pro®le have been used to characterize the pinning properties of superconductors [6]. Lack of ®eld resolution has been a stumbling stone for the application of this technique to the VLMT. A recent study by Soibel et al. has overcome this problem by a sophisticated 0921-4534/01/$ - see front matter Ó 2001 Elsevier Science B.V. All rights reserved. PII: S 0 9 2 1 - 4 5 3 4 ( 0 1 ) 0 0 3 1 0 - 0 T. Tamegai et al. / Physica C 357±360 (2001) 568±571 dierential technique and reports complicated behavior of the phase evolution [7]. In this paper, we report on the dierential MO studies of the VLMT in BSCCO with the emphasis on the relation between the behavior of the solid± liquid interface and the inhomogeneities in the crystal. We make compositional mapping of the crystal after the MO observations, and discuss the in¯uence on the VLMT. Typical forms of the evolution of the vortex solid±liquid interface are described. 2. Experimental Dierential MO images are taken by subtracting images at H Ha dHa =2 and H Ha dHa =2 with dHa 1 Oe [4]. We use a high-speed cooled CCD camera (Apogee 6E) with 1024 1024 pixels and 14-bit resolution. To resolve the magnetization step (0.3 G) accompanied by the vortex lattice melting under the typical background ®eld of 100 Oe, we need to have a light intensity resolution better than 0.1%. This number can be achieved by accumulating more than 106 photons into each CCD pixel. This means that we need to average more than 100 images for each ®eld settings with 14-bit CCD camera. All the procedure including the image acquisition and the setting of the current for the magnet are controlled by a computer. The crystals used in the present study are grown by the ¯oating zone method using an image furnace [8]. They are carefully cleaved to a thickness of about 20 lm and cut into approximate dimensions of 0:5 0:5 mm2 . We always keep edges of the crystal either parallel or perpendicular to the crystal growth direction (a-axis). One of the corners is cut to make it easier to identify the orientation of the crystal. Compositional mappings of the crystals are performed using energy dispersive X-ray spectroscopy after the MO observations. 3. Results and discussion Ideally, the nucleation of the vortex liquid phase starts at the center of the crystal and the 569 vortex solid±liquid interface propagates in a concentric manner. However, the actual nucleation does not start from the center nor expands regularly as shown in Fig. 1(a)±(d) for BSCCO #1. In this case, the nucleation starts at slightly o the center (Fig. 1(a)) and the interface propagation making complicated patterns. In these ®gures, white regions indicate the location where the vortex lattice has melted with the increase in H from Ha to Ha dHa . A broader white region means that the vortex liquid region expands more easily, whereas the white region can be discontinuous when the boundary is completely pinned. Actually, such a pinning of the boundary can be seen at several locations in the crystal (Fig. 1(c) and (d)). Fig. 2 shows the scanning electron micrograph of BSCCO #1. It is clear that this crystal has no apparent defect on the surface. Microanalyses of the chemical compositions using energy dispersive X-ray spectroscopy have been performed along the vertical and horizontal lines on the crystal. The area of each mapped region is 5 5 lm2 . We plot the compositional ratio of Sr to Cu along the two lines. The error bar is estimated by the standard deviation of 10 measurements at the same location. It should be noted that if the same analysis is applied to SrTiO3 , the ratio of Sr to Ti is 1 within an error of 1%. So the variation of the Sr/Cu ratio re¯ects the actual variation of the composition. A close inspection of the relation between the chemical composition variation and the boundary propagation reveals that there is a certain correlation. For example, Sr/Cu ratio decreases abruptly at x 160 lm in Fig. 2(b). At the same location, left protrusion of the solid±liquid interface is disturbed. Another example is that the upward interface motion is pinned at around y 250 lm (see scale in Fig. 2(c)) in Fig. 1(c). Almost at the same location, the Sr/Cu ratio increases sharply as shown in Fig. 2(c). Variation of the chemical composition would lead to the local change in the superconducting parameters. This, in turn, changes the local melting ®eld and disturbs the interface propagation. It is not easy to say what the increase in Sr/Cu ratio leads to, since depending on the absolute number and the location of the strontium atoms, changes in the above ratio can make the system either overdoped or underdoped. 570 T. Tamegai et al. / Physica C 357±360 (2001) 568±571 Fig. 1. Dierential MO images of the vortex lattice melting transition in BSCCO #1 at T 70 K and at (a) 101 Oe, (b) 102 Oe, (c) 103 Oe and (d) 104 Oe. stripes have some curvature. In other words, they form arc-like structures. One of the possible origins for such structures would be related with boundary of the grown crystallite and the molten region during the crystal growth. Actually the radius of the arc is about 15 mm and is consistent with the direct observation of the boundary after the crystal growth. Considering the slow speed of the crystal growth (0.2 mm/h), it would be possible to have chemical inhomogeneities parallel to the growth direction. Finally, it should be stressed that the inhomogeneities that we have described in this paper have almost no eect on the critical state ®eld pro®le at low temperatures. So, they are considered to be very weak perturbation. Fig. 2. (a) Scanning electron micrograph of BSCCO #1. Spatial dependence of compositional variation of the ratio of Sr to Cu along (b) horizontal and (c) vertical dotted lines in (a). 4. Summary In some of the crystals the vortex liquid nucleates along a stripe-like region as shown in Fig. 3 for BSCCO #2. The direction of the stripe is perpendicular to the crystal growth direction and the The dierential MO imaging technique reveals the complicated nucleation and propagation of the vortex solid±liquid interfaces. The inhomogeneities of the chemical composition frozen in the T. Tamegai et al. / Physica C 357±360 (2001) 568±571 571 Fig. 3. Dierential MO images of the vortex lattice melting transition in BSCCO #2 at T 70 K and at (a) 99 Oe, (b) 100 Oe, (c) 101 Oe and (d) 102 Oe. crystal during the growth in¯uences the propagation of the interfaces. In some cases, the interfaces are found to follow one-dimensional arc-like structures perpendicular to the growth direction, which are considered to be related to the boundary between the crystallite and molten region during the crystal growth. Acknowledgements The authors acknowledge A. Soibel and E. Zeldov for stimulating discussion. 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