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- Differential scanning calorimetry (1)
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Accelerator magnets that can reach magnetic fields well beyond the Nb-Ti performance limits are presently being built and developed, using Nb3Sn superconductors. This technology requires reaction heat treatment (RHT) of the magnet coils, during which Nb3Sn is formed from its ductile precursor materials (a “wind and react” approach). The Nb3Sn microstructure and microchemistry are strongly influenced by the conductor fabrication route, and by the Phase changes during RHT. By combining in situ differential scanning calorimetry, high Energy synchrotron x-ray diffraction, and micro-tomography experiments, we have acquired a unique data set that describes in great detail the phase and microstructure changes that take place during the processing of restacked rod process (RRP), powder-in-tube (PIT), and internal tin (IT) Nb3Sn wires. At temperatures below 450 ° the phase evolutions in the three wire types are similar, with respectively solid state interdiffusion of Cu and Sn, Cu6Sn5 formation, and Cu6Sn5 peritectic transformation. Distinct differences in phase evolutions in the wires are found when temperatures exceed 450 °C. The volume changes of the conductor during RHT are a difficulty in the production of Nb3Sn accelerator magnets. We compare the wire diameter changes measured in situ by dilatometry with the phase and void volume evolution of the three types of Nb3Sn wire. Unlike the Nb3Sn wire length changes, the wire diameter evolution is characteristic for each Nb3Sn wire type. The strongest volume increase, of about 5%, is observed in the RRP wire, where the main diameter increase occurs above 600 °C upon Nb3Sn formation.
The degradation mechanisms of state-of-the-art Nb-Ti/Cu superconductors are described, based on in-situ synchrotron X-ray diffraction measurements during heat treatment. A quantitative description of the Nb-Ti/Cu degradation in terms of critical current density, Cu stabiliser resistivity and mechanical composite strength is presented. In an applied magnetic field a significant critical current degradation is already observed after a 5-minute 400 °C heat treatment, due to variations of –Ti precipitate size and distribution within the Nb-Ti alloy filaments. A strong degradation of the strand mechanical properties is observed after several minutes heating above 550 °C, which is also the temperature at which the formation of Cu-Ti intermetallic phases is detected. Several minutes heating at 250 °C are sufficient to increase the RRR of the strongly cold work strands inside a Rutherford type cable from about 80 to about 240. Heating for several minutes at 400 °C does not cause a significant conductor degradation in self-field and, thus, leaves enough temperature margin for the electrical interconnection of Nb-Ti/Cu conductors with common low temperature solders.