Carbon Nanotubes by a CVD Method. Part I: Synthesis and Characterization of the (Mg, Fe)O Catalysts

The controlled synthesis of carbon nanotubes by chemical vapor deposition requires tailored and wellcharacterized catalyst materials. We attempted to synthesize Mg1-xFexO oxide solid solutions by the combustion route, with the aim of performing a detailed investigation of the influence of the synthesis conditions (nitrate/urea ratio and the iron content) on the valency and distribution of the iron ions and phases. Notably, characterization of the catalyst materials is performed using 57Fe Mo¨ssbauer spectroscopy, X-ray diffraction, and electron microscopy. Several iron species are detected including Fe2+ ions substituting for Mg2+ in the MgO lattice, Fe3+ ions dispersed in the octahedral sites of MgO, different clusters of Fe3+ ions, and MgFe2O4-like nanoparticles. The dispersion of these species and the microstructure of the oxides are discussed. Powders markedly different from one another that may serve as model systems for further study are identified. The formation of carbon nanotubes upon reduction in a H2/CH4 gas atmosphere of the selected powders is reported in a companion paper

Carbon Nanotubes by a CVD Method. Part II: Formation of Nanotubes from (Mg, Fe)O Catalysts

The aim of this paper is to study the formation of carbon nanotubes (CNTs) from different Fe/MgO oxide powders that were prepared by combustion synthesis and characterized in detail in a companion paper. Depending on the synthesis conditions, several iron species are present in the starting oxides including Fe2+ ions, octahedral Fe3+ ions, Fe3+ clusters, and MgFe2O4-like nanoparticles. Upon reduction during heating at 5 °C/min up to 1000 °C in H2/CH4 of the oxide powders, the octahedral Fe3+ ions tend to form Fe2+ ions, which are not likely to be reduced to metallic iron whereas the MgFe2O4-like particles are directly reduced to metallic iron. The reduced phases are R-Fe, Fe3C, and ç-Fe-C. Fe3C appears as the postreaction phase involved in the formation of carbon filaments (CNTs and thick carbon nanofibers). Thick carbon nanofibers are formed from catalyst particles originating from poorly dispersed species (Fe3+ clusters and MgFe2O4-like particles). The nanofiber outer diameter is determined by the particle size. The reduction of the iron ions and clusters that are well dispersed in the MgO lattice leads to small catalytic particles (<5 nm), which tend to form SWNTS and DWNTs with an inner diameter close to 2 nm. Well-dispersed MgFe2O4-like particles can also be reduced to small metal particles with a narrow size distribution, producing SWNTs and DWNTs. The present results will help in tailoring oxide precursors for the controlled formation of CNTs

Measurement of fracture toughness of metallic materials produced by additive manufacturing

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