Abstract
Single crystals of Pb 2Sr 2(Y 1- x Ca x )Cu 3O 8+δ have been grown from PbO-NaCl and PbO-KCl flux. Different temperature runs were performed to optimize the growth. A temperature gradient in the crucible is necessary to get crystals of Pb 2Sr 2(Y 1- x Ca x )Cu 3O 8+δ with reproducible sizes of more than 2X2X1 mm 3. Crystal growth in air yields a lot of large crystals but with broad transitions in magnetic susceptibility. The best results were obtained in an atmosphere of 3% O 2 in N 2. The crystals can be extracted from the flux very effectively by a solution of acetic acid in methanol. Neutron diffraction experiments confirm a low mosaicity and well defined lattice constants. High resolution energy dispersive X-ray (EDX) measurements show a very good homogeneity of the cations with a lateral resolution of 15 nm to 1 μm. The Y-to-Ca ratio has a stable value of 2:1. In high resolution transmission electron microscopy no crystal defects could be detected.
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