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Multi-layer graphene (MLG) sheets were obtained by exfoliation of natural graphite flakes in chloroform. Dispersions with concentration up to 19 mg/mL were prepared. Statistical measurements of MLG sheet sizes by transmission electron microscopy showed average width and length of ~340 nm and 860 nm, respectively. MLG/chloroform dispersions were used to prepare poly(lactic acid) (PLA)/MLG composite fibrillar membranes by electrospinning. A homogeneous distribution of MLG into the fibers was observed by optical and scanning electron microscopies. The presence of MLG leads to the decrease in the diameter distribution of the fibers, which presented average diameter values below 500 nm. Isothermal kinetic crystallization of PLA showed to be influenced by the electrospinning process and the content of MLG sheets, which acts as nucleating agents.

In this work, it is demonstrated how a novel technique based on temperature-programmed chemical vapor deposition (TPCVD) can be used to investigate the synthesis of carbon nanotubes (CNTs) from methane on a classic catalyst FeMo(x)/MgO (x = 0.07, 0.35 and 1.00). TPCVD monitors carbon deposition by measuring H2 formed during CH4 decomposition and affords information on the different catalytic species, deactivation process, reaction kinetics and carbon yields. The obtained results showed for FeMgO catalyst a simple TPCVD peak related to the production of carbon beginning at 760 degrees C with maximum at 800 degrees C followed by a rapid deactivation resulting in a low carbon yield. The addition of Mo to Fe/MgO catalyst completely changes the TPCVD profile with the formation of a new catalytic species active at temperatures higher than 900 degrees C, which is stable and continuously decomposes CH4 to produce high carbon yields. Raman, TG/DTG, Mössbauer, SEM, TEM, XRD and TPR analyses suggested that this active catalytic phase is likely related to Fe-Mo and Fe-Mo-C phases active to produce single wall and mainly multiwall carbon nanotubes.

Raw and purified samples of carbon nanotubes are considered as multicomponent systems with a distribution of carbonaceous, amorphous, multishell graphitic particles and nanotubes, together with the particles of metal compounds from the catalyst. With respect to the carbon nanotube fractions, a distribution of size, defect concentrations and functionalities needs to be taken into account. In order to address the problem of quantitative evaluation of purity it is necessary to measure the quality and distribution of the carbon nanotubes. In this research conventional and high resolution thermogravimetry are applied to quantify different fractions of carbonaceous and metallic materials in raw and moderately purified single walled and multiwalled carbon nanotubes. For each oxidized fraction, defined by careful line shape analysis of the derivative thermogravimetric curves (DTG), the temperature of maximum rate of oxidation, the temperature range for this oxidation, related to the degree of homogeneity, and the amount of associated material was specified The assignments of a type of carbonaceous material to each fraction in the distribution were based on several works from the literature and SEM and TEM measurements. The MWNT purified sample (1.6 wt% metal oxide) was investigated by high resolution thermogravimetry and the quantitative assessment for the carbonaceous fractions in this sample was as follow: 25 wt% of amorphous and other very defective carbonaceous including nanotubes, 54 wt% MWNT and 20 wt% multishell graphitic particles. A qualitative evaluation of these fractions was obtained from the SEM and TEM images and corroborates these results. The accuracy of the values, take into account other measurements performed for the same batch of material, should be better than ±4wt%.