Superconductivity of Carbon Materials - Unstable Phases

Different intercalated carbon systems: K$\text{}_{x}$C$\text{}_{60}$, Rb$\text{}_{x}$C$\text{}_{60}$ as well as highly oriented pyrolytic graphite + potassium with unstable structural and superconducting behavior were investigated with the EPR and magnetically modulated microwave absorption techniques. Three characteristic, well-separated EPR signals were observed for A$\text{}_{x}$C$\text{}_{60}$ (A = K or Rb) systems at the early stages of doping process. We ascribed these signals to C$\text{}_{60}^{+}$, C$\text{}_{60}^{1-}$, and C$\text{}_{60}^{3-}$ radicals. Evolution of the EPR spectrum characterizes different phases of K$\text{}_{x}$C$\text{}_{60}$ system including superconducting one. Two superconducting phases with T$\text{}_{c}^{(1)}$=(21±0.5) K (unstable) and T$\text{}_{c}^{(2)}$=(18.5±0.5) K (final, stable) were distinctly separated for K$\text{}_{x}$C$\text{}_{60}$ system. For C$\text{}_{60}$ intercalated by rubidium a similar evolution of EPR spectrum is observed. Prior to well-defined superconducting Rb$\text{}_{3}$C$\text{}_{60}$ phase was created, strong instabilities of the magnetically modulated microwave absorption signal were observed at the narrow part of the doping process. For potassium intercalated highly oriented pyrolytic graphite, EPR oscillations below 100 K were observed as well as Josephson hysteresis loops were registered at 5 K.