Microstructure and superconducting properties of attrition-milled Bi2Sr2CaCu2Ox

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Abstract
The microstructure and superconducting properties of Bi2Sr2CaCu2Ox (Bi-2212) during high-energy attrition milling were investigated in detail by a combination of x-ray diffraction, scanning electron microscopy, transmission electron microscopy, and magnetization techniques. The starting superconducting powder was milled in a standard laboratory attritor using yttria-stabilized ZrO2 balls and a stainless steel tank. After selected time increments, the milling was interrupted and a small quantity of milled powder was removed for further analysis. It was found that the deformation process rapidly refines Bi-2212 into nanometer-size crystallites, increases atomic-level strains, and changes the plate-like morphology of Bi-2212 to granular submicron clusters. At short milling times, the deformation seems localized at weakly linked Bi-O double layers, leading to twist/cleavage fractures along the {001} planes. The Bi-2212 phase decomposes into several bismuth-based oxides and an amorphous phase after excessive deformation. The superconducting transition is depressed by about 10 K in the early stages of milling and completely vanishes upon prolonged deformation. A deformation mechanism is proposed and correlated with the evolution of superconducting properties. The practical implications of these results are presented and discussed.