Polyamide-6-based composites with pristine or functionalized multi-walled carbon nanotubes were produced using melt extrusion technique. After chemical functionalization, defect formation and attachment of carboxylic (−COOH) or amine (−NH2) groups on carbon nanotubes was confirmed from high-resolution transmission electron microscope and Fourier transform infra-red spectroscope studies. Carbon nanotubes incorporation promoted growth of α-form crystals with enhanced thermal stability through increase in crystallization temperature from 162 to 192℃. Dynamic mechanical thermal analysis (DMTA) indirectly pointed out to a homogeneous, uniform dispersion of nanotubes with reduction in free volume of the polymer, exhibiting a slight increase in glass transition temperature and a significant drop in coefficient of thermal expansion value. Composites containing 0.5 wt% NH2-carbon nanotubes show increases in elastic modulus and tensile strength by ∼60 and 76%, respectively. Uniform dispersion and high interfacial strength was manifested by drop in strain to failure and lack of evidence of carbon nanotubes debonding from the matrix.
A series of hybrid materials incorporating imide-modified silica (IM-silica) network structures into a polyimide (PI) matrix were produced with a sol-gel technique from solution mixtures of poly(amic acid) and tetraethoxysilane (TEOS) containing alkoxysilane-terminated amic acids with various degrees of polymerization. The hybrid films, obtained by solvent evaporation, were heated successively to a maximum temperature of 3008C to carry out the imidization process and silica network formation in the PI matrix. The morphology and mechanical properties of these hybrids with IM-silica networks were studied and compared with the properties of one in which reinforcement of the matrix was achieved with a pure silica network generated from TEOS. The introduction of longer imide spacer groups into the silica network led to a drastic decrease in the silica particle size. Improved tensile modulus was observed in such compatibilized hybrid systems.Comparative thermogravimetric measurements of these hybrids showed improved thermooxidative resistance. A PI hybrid with 30% IM-silica had a thermal decomposition temperature nearly 2608C higher than that of the pure PI matrix. The high surface area of the interconnected silica domains and increased interfacial interaction were believed to restrict the segmental motion of the polymer and thus slow the diffusion of oxygen in the matrix, thereby slowing the oxidative decomposition of the polymer. The reinforcement of existing and new PIs by this method offers an opportunity for improving their thermooxidative stability without degrading their mechanical strength.
The effects of temperature, time, solvent and sonication conditions under air and Argon are described for the preparation of micron and sub-micron sized vermiculite particles in a double-jacketed Rosett-type or cylindrical reactor. The resulting materials were characterized via X-ray powder diffraction (XRD), Field Emission Scanning Electron Microscopy (FE-SEM), Fourier Transform Infrared (FTIR) Spectroscopy, BET surface area analysis, chemical analysis (elemental analysis), Thermogravimetry analysis (TGA) and Laser Granulometry. The sonicated vermiculites displayed modified particle morphologies and reduced sizes (observed by scanning electron microscopy and laser granulometry). Under the conditions used in this work, sub-micron sized particles were obtained after 5h of sonication, whereas longer times promoted aggregation again. Laser granulometry data revealed also that the smallest particles were obtained at high temperature while it is generally accepted that the mechanical effects of ultrasound are optimum at low temperatures according to physical/chemical properties of the used solvent. X-ray diffraction results indicated a reduction of the crystallite size along the basal direction [001]; but structural changes were not observed. Sonication at different conditions also led to surface modifications of the vermiculite particles brought out by BET surface measurements and Infrared Spectroscopy. The results indicated clearly that the efficiency of ultrasound irradiation was significantly affected by different parameters such as temperature, solvent, type of gas and reactor type.
Pure polyamide 6 (PA6) and polyamide 6/carbon nanotube (PA6/CNT) composite samples with 0.5 weight percent loading of pristine or functionalized CNTs were made using a solution mixing technique. Modification of nanotube surface as a result of chemical functionalization was confirmed through the presence of lattice defects as examined under high-resolution transmission electron microscope and absorption bands characteristic of carboxylic, sulfonic and amine chemical groups. Microstructural examination of the cryogenically fractured surfaces revealed qualitative information regarding CNT dispersion within PA6 matrix and interfacial strength. X-ray diffraction studies indicated formation of thermodynamically more stable α-phase crystals. Thermogravimetric analysis revealed that CNT incorporation delayed onset of thermal degradation by as much as 70 °C in case of amine-functionalized CNTs, thus increasing thermal stability of the composites. Furthermore, addition of amine-functionalized CNTs caused an increase in crystallization and melting temperatures from the respective values of 177 and 213 °C (for neat PA6) to 211 and 230 °C (for composite), respectively.
In this study, the effects of functionalization and weight fraction of mutliwalled carbon nanotubes (CNTs) were investigated on mechanical and thermomechanical properties of CNT/Epoxy composite. Epoxy resin was used as matrix material with pristine-, COOH-, and NH 2 -functionalized CNTs as reinforcements in weight fractions of 0.1, 0.5, and 1.0%. Varying (increasing) the weight fraction and changing type (pristine or functionalized) of CNTs caused increment in Young's modulus and tensile strength as observed during mechanical tests. CNT reinforcement improved thermal stability of the nanocomposites as observed by thermogravimetric analysis. Thermomechanical analysis showed a slight reduction in free volume of the polymer, that is a drop in coefficient of thermal expansion, prior to glass transition temperature (T g ) beside a slight increase in T g value. Dynamic mechani-cal analysis indicated an increase in storage modulus and T g owing to the strength addition of CNT to the matrix alongside the hardener. Scanning electron microscopy analysis of the fractured surface(s) revealed that CNTs were well dispersed with no agglomeration and resulted in reinforcing the matrix. POLYMER COMPOSITES-2015 FIG. 4. Dimensional change as a function of temperature for pure epoxy and different epoxy/CNT composites. FIG. 5. DMA studies of neat epoxy and different CNT/E composites for a range of temperatures at 1.0 Hz frequency and 5 C/min heating rate: (a) storage modulus and (b) dissipation factor (tan d).FIG. 3. TGA weight loss data over a range of temperatures for neat epoxy and nanocomposite samples.
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