Ja. Schlueter et al., SYNTHESIS, SUPERCONDUCTIVITY AND ESR CHARACTERIZATION OF RB3C60 CRYSTALS, Physica. C, Superconductivity, 216(3-4), 1993, pp. 305-314
A one-step doping process of C60 crystals with three equivalents of ru
bidium to produce Rb3C60 crystals was developed. The T(c)'s for all Rb
3C60 crystalline samples (aprproximately 30.5 K) were higher than thos
e of the powder samples (28 to 29.6 K), but consistent with the report
ed four-probe resistivity result for a doped C60 crystal (transition m
idpoint = 30.2 K). High superconducting shielding fractions (between 6
0 and 90%) and sharp magnetic transition widths (DELTAT10-90 between a
pproximately 3 K and 0.7 K) were observed for the samples doped with R
b at temperatures of 300 to 450-degrees-C. The doping process, as well
as the composition, of these samples were studied with the use of an
ESR spectrometer. Two major components, RbC60 and Rb3C60, were quantit
atively characterized. The superconducting shielding fractions of thes
e samples were found to be linearly correlated with the Rb3C60 content
obtained from ESR measurements. Higher-temperature doping ( > 400-deg
rees-C) favored the formation of Rb3C60 at the expense of severe C60 c
rystal fragmentation. The optimal doping condition to produce Rb3C60 c
rystals was found to be around 300-degrees-C.