Measuring with high precision the electrical resistance of highly ordered natural graphite samples from a Brazil mine, we have identified a transition at ∼350K with ∼40K transition width. The steplike change in temperature of the resistance, its magnetic irreversibility and time dependence after a field change, consistent with trapped flux and flux creep, and the partial magnetic flux expulsion obtained by magnetization measurements, suggest the existence of granular superconductivity below 350K. The zero-field virgin state can only be reached again after zero field cooling the sample from above the transition. Paradoxically, the extraordinarily high transition temperature we found for this and several other graphite samples is the reason why this transition remained undetected so far. The existence of well ordered rhombohedral graphite phase in all measured samples has been proved by x-rays diffraction measurements, suggesting its interfaces with the Bernal phase as a possible origin for the high-temperature superconductivity, as theoretical studies predicted. The localization of the granular superconductivity at these two dimensional interfaces prevents the observation of a zero resistance state or of a full Meissner state.
Temperature and field dependent measurements of the electrical resistance of different natural graphite samples, suggest the existence of superconductivity at room temperature in some regions of the samples. To verify whether dissipationless electrical currents are responsible for the trapped magnetic flux inferred from electrical resistance measurements, we localized them using magnetic force microscopy on a natural graphite sample in remanent state after applying a magnetic field. The obtained evidence indicates that at room temperature a permanent current flows at the border of the trapped flux region. The current path vanishes at the same transition temperature Tc ≈ 370 K as the one obtained from electrical resistance measurements on the same sample. This sudden decrease of the phase is different from what is expected for a ferromagnetic material. Time dependent measurements of the signal show the typical behavior of flux creep of a permanent current flowing in a superconductor. The overall results support the existence of room-temperature superconductivity at certain regions in the graphite structure and indicate that magnetic force microscopy is suitable to localize them. Magnetic coupling is excluded as origin of the observed phase signal.
In the last 43 years several hints were reported suggesting the existence of granular superconductivity above room temperature in different graphite-based systems. In this paper some of the results are reviewed, giving special attention to those obtained in water and n-heptane treated graphite powders, commercial and natural bulk graphite samples with different characteristics as well as transmission electron microscope (TEM) lamellae. The overall results indicate that superconducting regions exist and are localized at certain internal interfaces of the graphite structure. The existence of the rhombohedral graphite phase in all samples with superconducting-like properties suggests its interfaces with the Bernal phase as a possible origin for the high-temperature superconductivity, as theoretical calculations predict. High precision electrical resistance and magnetization measurements were used to identify a transition at Tc > ∼ 350 K. To check for the existence of true zero resistance paths in the samples we used local magnetic measurements, which results support the existence of superconducting regions at such high temperatures.
Granular superconductivity at high temperatures in graphite can emerge at certain two-dimensional (2D) stacking faults (SFs) between regions with twisted (around the c-axis) or untwisted crystalline regions with Bernal (ABA…) and/or rhombohedral (ABCABCA…) stacking order. One way to observe experimentally such 2D superconductivity is to measure the frozen magnetic flux produced by a permanent current loop that remains after removing an external magnetic field applied normal to the SFs. Magnetic force microscopy was used to localize and characterize such a permanent current path found in one natural graphite sample out of ∼50 measured graphite samples of different origins. The position of the current path drifts with time and roughly follows a logarithmic time dependence similar to the one for flux creep in type II superconductors. We demonstrate that a ≃10 nm deep scratch on the sample surface at the position of the current path causes a change in its location. A further scratch was enough to irreversibly destroy the remanent state of the sample at room temperature. Our studies clarify some of the reasons for the difficulties of finding a trapped flux in a remanent state at room temperature in graphite samples with SFs.
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