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Abstract
C60 nanorods with hexagonal cross sections are grown using a static liquid–liquid interfacial precipitation method in a system of C60/m-dichlorobenzene solution and ethanol. Adding water to the ethanol phase leads instead to C60 tubes where both length and diameter of the C60 tubes can be controlled by the water content in the ethanol. Based on our observations we find that the diameter of the rods/tubes strongly depends on the nucleation step. We propose a liquid-liquid interface growth model of C60 rods and tubes based on the diffusion rate of the good C60 containing solvent into the poor solvent as well as on the size of the crystal seeds formed at the interface between the two solvents. The grown rods and tubes exhibit a hexagonal solvate crystal structure with m-dichlorobenzene solvent molecules incorporated into the crystal structure, independent of the water content. An annealing step at 200 °C at a pressure <1 kPa transforms the grown structures into a solvent-free face centered cubic structure. Both the hexagonal and the face centered cubic structures are very stable and neither morphology nor structure shows any signs of degradation after three months of storage.
Highlights
One dimensional fullerene structures in the nano- and sub-micrometer range are attractive materials due to their excellent properties suitable for applications in electronic devices, solar cells, optical switching devices, etc. [1,2,3,4,5,6,7,8,9,10]
Distinct grain boundaries are visible in the image which indicates that the annealing step, which evaporates the solvent molecules, transforms the structure from single crystalline to crystalline regions where the lattice planes are slightly disoriented relative to each other. This is even clearer by the streaks in the Fast Fourier Transform (FFT) diffractogram pattern of the high-resolution TEM (HRTEM) images, which are well known to run perpendicular to the grain boundaries, and by the broadening of the peaks in the XRD pattern of the annealed rods compare to the pure C60
In order to check the stability of the crystal structure and morphology of the grown C60 structure, the characterization of the samples was done within an interval of three months after the growth, where the samples were kept in their original bottles
Summary
One dimensional fullerene structures (rods and tubes) in the nano- and sub-micrometer range are attractive materials due to their excellent properties suitable for applications in electronic devices, solar cells, optical switching devices, etc. [1,2,3,4,5,6,7,8,9,10]. The interface may either be influenced by hand shaking or ultra-sonication or left undisturbed during the synthesis process The latter is referred to as static LLIP growth [24]. Miyazawa and Hotta [24,25] have shown that the length of C60 nanowhiskers, synthesized by the hand shaking LLIP method, increased by adding water to isopropyl alcohol (IPA) in a system of IPA and C60-saturated toluene solution. In their experiments the water destabilizes the grown structures.Increasing the water content of IPA above a critical amount (2.3 mass%) only leads to granular C60 precipitates. The structure and morphology of the grown tubes and rods are stable for more than three months under ambient conditions
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