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Thermo-mechanical characterization of epoxy nanocomposites with different carbon nanotube distributions obtained by solvent aided and direct mixing
A. Martone, C. Formicola, F. Piscitelli, M. Lavorgna, M. Zarrelli, V. Antonucci, M. Giordano
Vol. 6., No.7., Pages 520-531, 2012
Vol. 6., No.7., Pages 520-531, 2012
Two different routes, namely solvent aided dispersion and direct mixing, were employed to disperse Multi-Walled Carbon Nanotubes (MWNTs) into a mono-component epoxy system used as matrix for advanced composites. In the first route, MWCNTs were diluted in three different solvents (acetone, sodium dodecyl sulfate and ethanol) and then mixed with the matrix by tip sonication. In the second case, carbonaceous nanoparticles were added directly into the hosting system and dispersion was carried out by using three different techniques (mechanical stirring, magnetic agitation and tip sonication). The effects of the solvents and agitation energy were investigated by optical microscopy at micron level, in order assess the more efficient dispersion procedure for the considered epoxy system. It was demonstrated that parameters associated with direct mixing rather than solvent solubility govern MWCNT dispersion. Optical analysis of the nanocomposite morphology evidenced a very low density of MWCNTs micron sized aggregates in the case of direct mixed tip sonicated samples if compared to those obtained by solution aided dispersion. In addition, nanocomposites obtained by sonication showed the lowest density of MWCNTs micron sized aggregates, also when compared with mechanically and magnetically stirred system. Dynamic Mechanical Analysis (DMA) and Thermo-Mechanical Analysis (TMA) results confirm the final result that among the considered direct mixing techniques, the direct tip sonication represents the most efficient route for MWCNT dispersion. Moreover, the mixing temperature of the hosting matrix system represents a fundamental feature in enhancing the MWCNT de-bundling and dispersion. Small X-ray Scattering analysis revealed that a nanosized structure of nanotubes is formed in the case of the tip sonicated samples that is heuristically correlated with both the maximum enhancement of mechanical modulus and the maximum reduction of thermal expansion coefficients.
We report the preparation, mechanisms and thermal properties of core-shell structured polymer/inorganic nanoparticle composite microspheres prepared by Pickering emulsion polymerization. Stable Pickering emulsion was firstly fabricated by using surface-modified nano-SiO2 particles as stabilizer. And then, two kinds of polystyrene/nano-SiO2 (PS/SiO2) composite microspheres with different sizes and morphologies were synthesized using hydrophobic azobisisobutyronitrile (AIBN) and hydrophilic ammonium persulfate (APS) as initiator, respectively. The possible mechanisms of Pickering emulsion polymerization initiated by different initiators were proposed according to the results of transmission electron microscope (TEM) and scanning electron microscope (SEM). The chemical structure and molecular weight of the composite microspheres were characterized by Fourier transform infrared spectroscopy (FTIR), X-ray diffractometer (XRD) and gel permeation chromatography coupled with a multi-angle laser light scattering photometer (GPC-MALLS). Thermogravimetric analysis (TGA) and differential scanning calorimeter (DSC) were used to comparatively analyze the thermal properties of nanocomposites and corresponding pure polymer. The results indicated that the decomposition temperature and glass transition temperature (Tg) of nanocomposites were elevated to a certain degree due to the existence of nano-SiO2.
A solids conveying theory called double-flight driving theory was proposed for helically channeled single screw extruders. In the extruder, screw channel rotates against static barrel channel, which behaves as cooperative embedded twin-screws for the positive conveying. They turn as two parallel arc plates, between which an arc-plate solid-plug was assumed. By analyzing the forces on the solid-plug in the barrel channel and screw channel, the boundary conditions when the solid-plug is waived of being cut off on barrel wall, were found to have the capacity of the positive conveying. Experimental data were obtained using a specially designed extruder with a helically channeled barrel in the feeding zone and a pressure-adjustable die. The effects of the barrel channel geometry and friction coefficients on the conveying mechanism were presented and compared with the experimental results. The simulations showed that the positive conveying could be achieved after optimizing extruder designs. Compared with the traditional design with the friction-drag conveying, the throughput is higher while screw torque and energy consumption are decreased. Besides, the design criteria of the barrel channel were also discussed.
The polyhedral oligomeric silsesquioxane (POSS) additivated polystyrene (PS) based nanocomposites were prepared by melt processing and the structure-properties relationships of the POSS-PS systems were compared to those of the neat PS. In order to investigate the effect of these structural parameters on the final properties of the polymer nanocomposites, five different kinds of POSS samples were used, in particular, POSS with different inorganic cage and with different organic pendent groups. The rheological investigation suggests clearly that the POSS acts as a plasticizer and that the processability of the PS was positively modified. The affinity between the POSS samples and the PS matrix was estimated by the calculated theoretical solubility parameters, considering the Hoy’s method and by morphology analysis. Minor difference between the solubility parameter of POSS and the matrix means better compatibility and no aggregation tendency. Furthermore, the POSS loading leads to a decrease of the rigidity, of the glass transition temperature and of the damping factor of the nanocomposite systems. The loading of different POSS molecules with open cage leads to a more pronounced effect on all the investigated properties that the loading of the POSS molecules with closed cage. Moreover, the melt properties are significantly influenced by the type of inorganic framework, by the type of the pendent organic groups and by the interaction between the POSS organic groups and the host matrix, while, the solid state properties appears to be influenced more by the kind of cage.
The aim of this research was the investigation of the effect of carbon nanotube addition on the mode I interlaminar fatigue properties of carbon fiber reinforced composites. The authors developed a localization methodology to track the interlaminar fatigue crack front using the acoustic emission (AE) technique. According to the test evaluation the carbon nanotube reinforcement decreased the crack propagation rate by 69% compared to the composite containing no nanotubes. Besides that, the fatigue life also increased significantly, the nanotube reinforced composite could withstand 3.8-times more cycles to failure than the unfilled matrix composite.
Fracture resistance of rubbers with MWCNT, organoclay, silica and carbon black fillers as assessed by the J-integral: Effects of rubber type and filler concentration
S. Agnelli, G. Ramorino, S. Passera, J. Karger-Kocsis, T. Ricco
Vol. 6., No.7., Pages 581-587, 2012
Vol. 6., No.7., Pages 581-587, 2012
The fracture resistance of different rubbers containing various nanofillers, such as multiwall carbon nanotube (MWCNT), organoclay, silica and carbon black (CB), was determined by the J-integral making use of the single edge notched tensile loaded (SEN-T) single specimen approach. The elastomeric matrices were natural (NR), ethylene propylene diene (EPDM) and hydrogenated nitrile rubbers (HNBR). Moreover, the strain softening (Payne effect) of selected rubbers with 30 part per hundred rubber (phr) filler content was also investigated by dynamic mechanical thermal analysis (DMTA) in shear mode. DMTA results indicated that the Payne effect follows the ranking: MWCNT(fibrous) > organoclay(platy) > silica(spherical). J-resistance (JR) curves were constructed by plotting the J value as a function of the crack tip opening displacement (CTOD*), monitored during loading. CTOD* = 0.1 mm was considered as crack initiation threshold and thus assigned to the critical value JIc. JIc increased with increasing filler loading, whereby MWCNT outperformed both silica and CB. On the other hand, JIc did not change with filler loading for the NR/organoclay systems that was traced to straininduced crystallization effect in NR. The tearing modulus (TJ) also increased with increasing filler loading. The related increase strongly depended on both rubber and filler types. Nonetheless, the most prominent improvement in TJ among the fillers studied was noticed for the fibrous MWCNT.
Novel blends of acrylonitrile butadiene rubber (NBR) and polyurethane-silica (PU-SiO2) hybrid networks have been prepared by melt blending. The PU-SiO2 hybrid networks were formed via the reaction of NCO groups of NCO-terminated PU prepolymer and OH groups of SiO2 in the absence of an external crosslinking agent (i.e. alcohols and amines) during the curing process of NBR. Both in the neat PU-SiO2 system and the NBR/(PU-SiO2) system, the NCO-terminated PU prepolymer could be crosslinked by SiO2 to form PU-SiO2 hybrid networks. The effects of PU-SiO2 introduction into the NBR, on the properties of the resulting blends were studied. It was found that the vulcanization was activated by the incorporation of PU-SiO2. Transmission electronic microscopy (TEM) studies indicated that the interpenetration and entanglement structures between NBR and PU-SiO2 increased with increasing PU-SiO2 content and the quasi-interpenetrating polymer networks (quasi-IPN) structures were formed when the PU-SiO2 was 50 wt% in the NBR/(PU-SiO2) systems. The microstructures formed in the blends led to good compatibility between NBR and PU-SiO2 and significantly improved the mechanical properties, abrasion resistance and flex-fatigue life of the blends.
In this work Raman spectroscopy was used for extensive characterization of multiwall carbon nanotube (MWNTs) and of MWCNTs/rubber composites. We have measured the Raman spectra of bundled and dispersed multiwall carbon nanotubes. All the Raman bands of the carbon nanotubes are seen to shift to higher wavenumbers upon debundling on account of less intertube interactions. Effects of laser irradiation were also investigated. Strong effects are observed by changing the wavelength of the laser excitation. On the other hand, at a given excitation wavelength, changes on the Raman bands are observed by changing the laser power density due to sample heating during the measurement procedure.