Flexible and rigid polyurethane (PU) foam nanocomposites were synthesized using unmodified and organically modified montmorillonite clays. X-ray diffraction and transmission electron microscopy studies showed that, while the unmodified clays were intercalated, the modified clays were exfoliated in the foams produced. The cell morphology of the foams was investigated by environmental scanning electron microscopy. The fraction of open cells (defined as the cells in which the foam lamellae are all ruptured) in the foam is an important parameter governing many properties, such as the degree of softness in the case of flexible foams and dimensional stability for both rigid and flexible foams. The open cell content in PU-clay foamed nanocomposites was investigated. It was found that clays act as efficient cell openers in both rigid and flexible foams and a greater fraction of open cells was obtained with increasing clay concentration. Modified clays were found to be more efficient cell openers than the unmodified clay. The degree of softness of flexible foam was increased and the dimensional stability of both rigid and flexible foams was improved, with clay addition. The thermal conductivity and compressive strength of the rigid foams were not significantly affected by clay addition. The kinetics of the foaming process with different clays was investigated. The polymerization and the foaming reactions were found to be affected in different ways for the modified and unmodified clays. Comparison with chemical cell openers in the case of flexible foams indicated that clays could be a good alternative.
Electromagnetic interference (EMI) shielding properties in the 1-18 GHz frequency range for multi-walled carbon nanotube (MWNT)-poly(vinylidene fluoride) (PVDF) composites are reported. A simple and gentle acid-treatment of MWNT showed a percolation threshold (PT) of 0.15 wt% in the PVDF matrix as against 0.35 wt% for unfunctionalized MWNT. Acid-treatment of MWNT significantly improves dispersion, interfacial adhesion with the matrix and the EMI shielding properties of PVDF composites. Further, the EMI shielding properties are correlated with the electrical properties. Using composite films of 0.3 mm thickness, the maximum shielding effectiveness (SET) values for 4 wt% unfunctionalized MWNT composites are found to be about 110, 45, 30, 26, and 58 dB for L (1-2 GHz), S (2-4 GHz), C (4-5.8 GHz), J (5.8-8 GHz), and X (8-12 GHz) bands, while the corresponding values for only 0.5 wt% acid functionalized MWNT composites are about 98, 45, 26, 19, and 47 dB, respectively. The electrical conductivity for both the cases is ∼10(-3) S cm(-1) and the weight contents of CNTs are higher than the PT for the respective composites. The comparable EMI SE and electrical conductivity values for both the composites at different weight fractions of CNTs suggest that there is a critical electrical conductivity above which the composites attain improved EMI shielding properties. Further, the shielding mechanism was found to be dominated by absorption loss. Therefore, the composites may also serve as a radar absorbing material.
Structural arrangements of nanoplatelets in a polymer matrix play an important role in determining their properties. In the present study, multilayered composite films of poly(vinyl alcohol) (PVA) with Laponite clay are assembled by layer-by-layer (LBL) deposition. The LBL films are found to be hydrated, flexible and transparent. A facile and solvent-free method-by depositing self-assembled monolayers (SMA) of a functional silane on substrates-is demonstrated for preparing free-standing LBL films. Evolution of nanostructures in LBL films is correlated with thermal and mechanical properties. A well-dispersed solvent-cast PVA/Laponite composite film is also studied for comparison. We found that structurally ordered LBL films with an intercalated nanoclay system exhibits tensile strength, modulus and toughness, which are significantly higher than that of the conventional nanocomposites with well-dispersed clay particles and that of pure PVA. This indicates that clay platelets are oriented in the applied stress direction, leading to efficient interfacial stress transfer. In addition, various grades of composite LBL films are prepared by chemical crosslinking and their mechanical properties are assessed. On account of these excellent properties, the LBL films may find potential use as optical and structural elements, and as humidity sensors.
Melt-mixed blends of polyamide 6 and acrylonitrile-butadiene-styrene (PA6/ABS) with multiwall carbon nanotubes (MWNTs) were prepared with the intention to develop conducting composites. A generic strategy, namely specific interactions combined with reactive coupling, was adopted to facilitate and to retain the 'network-like' structure of MWNTs during melt-mixing. This was facilitated by the sodium salt of 6-amino hexanoic acid (Na-AHA) and certain phosphonium based modifiers, where it was envisaged that these modifiers would establish specific interactions (either 'cation-π' or 'π-π' ) with the 'π-electron' clouds of MWNTs, as well as restricting them in the PA6 phase of the blends via reactive coupling. This route eventually led to a remarkable increase in the electrical conductivity and dielectric constant in the blends with MWNTs. Raman, FTIR and TEM investigations further supported these observations.
Nanocomposites of rigid polyurethane foam with unmodified vermiculite clay are synthesized. The clay is dispersed either in polyol or isocyanate before blending. The viscosity of the polyol is found to increase slightly on the addition of clay up to 5 pphp (parts per hundred parts of polyol by weight). The gel time and rise time are significantly reduced by the addition of clay, indicating that the clay acts as a heterogeneous catalyst for the foaming and polymerization reactions. X-ray diffraction and transmission electron microscopy of the polyurethane composite foams indicate that the clay is partially exfoliated in the polymer matrix. The clay is found to induce gas bubble nucleation resulting in smaller cells with a narrower size distribution in the cured foam. The closed cell content of the clay nanocomposite foams increases slightly with clay concentration. The mechanical properties are found to be the best at 2.3 wt% of clay when the clay is dispersed in the isocyanate; the compressive strength and modulus normalized to a density of 40 kg/m 3 are 40% and 34% higher than the foam without clay, respectively. The thermal conductivity is found to be 10% lower than the foam without clay.
The composite processing technique and nanofiller concentration and its functionalization significantly alter the properties of polymer nanocomposites. To realize this, multi-walled carbon nanotubes (CNT) were dispersed in a poly(vinylidene fluoride) (PVDF) matrix at carefully selected CNT concentrations by two illustrious methods, such as solution-cast and melt-mixing. Notwithstanding the processing method, CNTs induced predominantly the γ-phase in PVDF, instead of the commonly obtained β-phase upon nanofiller incorporation, and imparted significant improvements in dielectric properties. Acid-treatment of CNT improved its dispersion and interfacial adhesion significantly with PVDF, and induced a higher γ-phase content and better dielectric properties in PVDF as compared to pristine CNT. Further, the γ-phase content was found to be higher in solution-cast composites than that in melt-mixed counterparts, most likely due to solvent-induced crystallization in a controlled environment and slow solvent evaporation in the former case. However, interestingly, the melt-mixed composites showed a significantly higher dielectric constant at the onset of the CNT networked-structure as compared to the solution-cast composites. This suggests the possible role of CNT breakage during melt-mixing, which might lead to higher space-charge polarization at the polymer-CNT interface, and in turn an increased number of pseudo-microcapacitors in these composites than the solution-cast counterparts. Notably, PVDF with 0.13 vol% (volume fraction, f c = 0.0013) of acid-treated CNTs, prepared by melt-mixing, displayed the relative permittivity of ∼217 and capacitance of ∼5430 pF, loss tangent of ∼0.4 at 1 kHz and an unprecedented figure of merit of ∼10(5). We suggest a simple hypothesis for the γ-phase formation and evolution of the high dielectric constant in these composites. Further, the high-dielectric composite film showed marked improvements in mechanical and thermal properties over the neat PVDF film. These composites with exceptional dielectric properties and concomitant improvement in mechanical and thermal properties offer a great promise for use in flexible and mechanically robust charge storage devices.
PET-clay nanocomposites were prepared using alkyl quaternary ammonium and phosphonium modified clays by melt-mixing at 280 C using a micro twin screw extruder. The latter clays were prepared by synthesizing phosphonium surfactants using a simple onestep method followed by a cation exchange reaction. The onset temperature of decomposition (T onset ) for phosphonium clays (>300 C) was found to be significantly higher than that of ammonium clays (around 240 C). The clay modified with a lower concentration (0.8 meq) of phosphonium surfactant showed a higher T onset as compared to the clay modified with a higher concentration (1.5 meq) of surfactants. Nanocomposites prepared with octadecyltriphenyl phosphonium (C18P) modified clay showed a higher extent of polymer intercalation as compared with benzyltriphenylphosphonium (BTP) and dodecyltriphenylphosphonium (C12P) modified clays. The nanocomposites prepared with ammonium clays showed a significant decrease in the molecular weight of PET during processing due to thermal degradation of ammonium surfactants. This resulted in a substantial decrease in the mechanical properties. The molecular weight of PET was not considerably reduced during processing upon addition of phosphonium clay. The nanocomposites prepared using phosphonium clays showed an improvement in thermal properties as compared with ammonium clay-based nanocomposites. T onset increased significantly in the phosphonium clay-based nanocomposites and was higher for nanocomposites which contained clay modified with lower amount of surfactant. The tensile strength decreased slightly; however, the modulus showed a significant improvement upon addition of phosphonium clays, as compared with PET. Elongation at break decreased sharply with clay.
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