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.
A detailed study of new oxygen carrier materials, Mg–Fe–Al–O, with various loadings of iron oxide (10–100 wt% Fe2O3) is carried out in order to investigate the relationship between material transformation, stability and CO yield from CO2conversion.
Abstract. The M6ssbauer fractionsffor various ferrousand/or ferric-containing oxides and oxyhydroxides, silicates and carbonates were evaluated from the experimental temperature dependence of their center shifts, using the Debye approximation for the second-order Doppler shift. It is concluded that ferrous ions exhibit a lower fraction as compared to ferric ions. Using standard mixtures of e-F%O3 with selected Fe z + or Fe 3 + compounds, it is found that the calculated Fe 3 + fvalues are somewhat overestimated with respect to those of Fe 2 +. Possible explanations for this shortcoming are discussed and it is suggested that a different temperature dependence of the intrinsic isomer shift is the most likely reason. This suggestion is corroborated by analyses of hematite and hedenbergite data which are available for temperatures up to 900 K and 800 K respectively.
Three different magnetic samples with particle sizes ranging from 10 to 30 nm were prepared by wet chemical methods. The powders were heated at 100, 150, 200, and 250 °C during 30 min under air. Ferrous and total iron contents were determined immediately after the synthesis and after the thermal treatments. All samples were characterized by X-ray diffraction, transmission and integral low-energy electron Mössbauer spectroscopy (ILEEMS) at 298 K. These samples are composed of a mixture of individual particles of maghemite and magnetite, which implies that once oxidation starts in this kind of material, it occurs throughout the entire particle volume. The existence of a maghemite/magnetite core-shell model was ruled out. A linear correlation between the average isomer shift and the magnetite content was found, allowing the estimation of the amounts of magnetite and maghemite in an unknown sample without the need of performing chemical analysis.
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