Growth and analysis of C nanotubes on ceramic polymer-additives.

C nanotubes are synthesized by catalytic route on ceramic supports (Al2O3, MgO and CaO), usually utilized for polymer reinforcing/flame-retardancy, aiming at nanotube-based hybrid preparation. Chemical vapor deposition is carried out in i-C4H10+H2 atmosphere over 17 wt% Fe-catalysts upon different conditions. In order to clarify the influence of support material, calcination (450 degrees C or 750 degrees C) and reduction temperature (500 degrees C or 600 degrees C) of the catalysts, and synthesis temperature (600 degrees C or 700 degrees C), catalysts utilized and nanotubes obtained are systematically investigated by the use of several analysis techniques (electron microscopy, X-ray diffraction, thermo-gravimetry and Raman spectroscopy). The results obtained show that, in the considered range of variation, support material is the most influential parameter. The most catalytically active alumina supports allow achieving higher yields, but involve larger metallic inclusions and lower crystalline quality. Remaining supports behave oppositely. The reasons for such differences are discussed in the light of the current assessments on the nanotube growth and the results obtained are compared with those available in literature for similar catalysts.

Morphological modification of MWCNT functionalized with HNO3/H2SO4 mixtures.

The acidic oxidation with HNO3/H2SO4 mixtures is widely reported as an effective method to functionalize multi-walled carbon nanotubes (MWCNT). Although effective, a bad control of the oxidation conditions frequently cause serious modifications of carbon nanotube network, limiting further potential applications. Investigations about the effect of functionalization operating conditions on the morphological, chemical and chemical-physical properties of MWCNT can be useful for a proper setting of oxidation reactions of MWCNT according to their specific applications. In this work the effect of HNO3/H2SO4 ratio on the morphological and chemical-physical properties and on the degree of functionalization of MWCNT was investigated. Electron microscopy, thermogravimetric, X-ray diffraction, titration and water dispersion analyses clearly revealed that the increase of the amount of concentrated sulphuric acid in the HNO3/H2SO4 mixture lead to an increase of the amount of functional groups on the MWCNT surface but also to an increase of structural damage in terms of tube cutting and generation of additional defects in the graphitic network of pristine

Optimized CVD production of CNT-based nanohybrids by Taguchi robust design.

Taguchi's robust design method is for the first time employed to optimize many aspects of the production of nanohybrids based on C nanotubes by iron-catalyzed chemical vapor deposition in i-C4H10 + H2 atmosphere. By analyzing the outcomes of the catalytic process in terms of selectivity, carbon yield, purity and crystalline arrangement of the hybrid-forming nanotubes, the influence is ranked of the following parameters: synthesis temperature (500-700 degrees C), support material (alumina, magnesia or sodium-exchanged montmorillonite), calcination- (450-750 degrees C) and reduction-(500-700 degrees C) temperatures of the 15 wt% Fe-catalyst. In the experiments initially performed for this purpose, the growth process had, on average, scarce selectivity (2 in a scale 1-5) and poor yield (130 wt%); carbonaceous deposits exhibited unsatisfactory graphitization degree (Raman D/G intensity ratio > 1.5) and contained large amounts of metal impurities (14 wt%) and amorphous carbon (5 wt%). The indications emerging from Taguchi approach to the process optimization are critically examined. The experimental conditions chosen for carrying out test experiments allow achieving excellent selectivity (5) or large yield (760 wt%), hybrids with well-graphitized nanotubes (D/G intensity ratio < 0.6), nearly free of metallic (0.3 wt%) or amorphous (0.4 wt%) inclusions, with consequent possibility of satisfying the different requisites that the specific application to be addressed may require.

Influence of carbon source and Fe-catalyst support on the growth of multi-walled carbon nanotubes.

Catalytic activity of iron based catalysts in the production of multi-walled carbon nanotubes (MWCNTs) has been investigated. The effect of the carbon source (ethane or isobutane), catalyst support (Al2O3 or SiO2), iron loading, catalyst reduction temperature and reaction temperature on yield and quality of carbon products has been examined. The structural and morphological properties of catalyst and carbon products obtained have been analyzed by means of scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM), Raman spectroscopy (RS), thermogravimetric analysis (TGA) and X-ray powder diffraction (XRD). The iron-based catalysts supported on alumina seem to be efficient systems for the production of carbon nanotubes from chemical vapor deposition (CVD) of isobutane with very interesting yields. The opportune calibration of reaction parameters, such as iron loading and reaction temperature, can in fact drive the synthesis toward the formation of high quality CNTs.