a b s t r a c tRaman spectroscopy is used to investigate magnetite nanoparticles dispersed in two types of bcyclodextrin suspensions. An approach is presented for characterization of the magnetic core in liquid surrounding at room temperature and atmospheric pressure. The effect of elevating laser power on the structural stability and chemical composition of magnetite in the ferrofluids is discussed. The data are compared with data from dry by-products from the fluids. Powder samples undergo total phase transition from magnetite to hematite at laser power of 1.95 mW. The same nanoparticles in the fluid undergo transformation at 9 mW, but no hematite positions appear throughout that investigation. The Raman spectra revealed that the main phase of the magnetic core in the fluids is magnetite. That is indicated by a strong and non-diminishing in intensity peak at 670 cm. A second phase is present at the nanoparticle's surface with Raman spectroscopy unveiling maghemite-like and small fractions of goethite-like structures. The Fourier transform infrared spectroscopy investigations confirm deviations in the surface structure and also point to the fact that the oxidation process starts at an early stage after formation of the nanoparticles. The analyses of the infrared data also show that b-cyclodextrin molecules retain their cyclic character and the coating does not affect the oxidation process once the particles are evicted from the fluids. A Mössbauer spectroscopy measurement on a ferrofluidic sample is also presented.
The reduction in H 2 /CH 4 atmosphere of aluminum-iron oxides produces metal particles small enough to catalyze the formation of single-walled carbon nanotubes. Several experiments have been made using the same temperature profile and changing only the maximum temperature (800-1070°C). Characterizations of the catalyst materials are performed using notably 57 Fe Mössbauer spectroscopy. Electron microscopy and a macroscopical method are used to characterize the nanotubes. The nature of the iron species (Fe 3+ , R-Fe, γ-Fe-C, Fe 3 C) is correlated to their location in the material. The nature of the particles responsible for the high-temperature formation of the nanotubes is probably an Fe-C alloy which is, however, found as Fe 3 C by postreaction analysis. Increasing the reduction temperature increases the reduction yield and thus favors the formation of surface-metal particles, thus producing more nanotubes. The obtained carbon nanotubes are mostly single-walled and double-walled with an average diameter close to 2.5 nm. Several formation mechanisms are thought to be active. In particular, it is shown that the second wall can grow inside the first one but that subsequent ones are formed outside. It is also possible that under given experimental conditions, the smallest (<2 nm) catalyst particles preferentially produce double-walled rather than single-walled carbon nanotubes.
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