Morphological, optical and electromagnetic characterization of polybutylene terephthalate/silica nanocomposites

Polybutylene terephthalate (PBT) composites containing 1 %, 3 % and 5 % silica nanoparticles were prepared by melt compounding method. The characteristics of the nanocomposites were investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM), differential scanning calorimetry (DSC), thermal gravimetric analysis (TGA), tensile strength test (TST), reflectance spectroscopy (RS), electromagnetic transition test (ETT) and atomic force microscopy (AFM). XRD method showed successful incorporation of silica into the polymer matrix. SEM and AFM results showed the presence of silica aggregates on the surface of PBT sheets. Thermal analysis results demonstrated some changes in crystallinity of PBT after addition of silica. The PBT/silica nanocomposites were found to have higher electromagnetic reflection compared with the pure PBT. Silica nanoparticle is thus suggested as a good candidate for electromagnetic shielding purposes.     

Effects of Chemical Functionalization of MWCNTs on the Structural and Physical Properties of Elastomeric Copolyetherester-based Composite Fibers

Elastomeric copolyetherester (CPEE)-based composite fibers incorporating various neat and functionalized multiwalled carbon nanotubes (MWCNTs) were prepared through a conventional wet-spinning and coagulation process. The influence of functionalized MWCNTs on the morphological features, and the thermal, mechanical properties and electrical conductivity of CPEE/MWCNT (80/20, w/w) composite fibers were investigated. FE-SEM images show that a composite fiber containing poly(ethylene glycol)-functionalized MWCNTs (MWCNT-PEG) has a relatively smooth surface owing to the good dispersion of MWCNT-PEGs within the fiber, whereas composite fibers including pristine MWCNTs (p-MWCNT), acid-functionalized MWCNTs (a-MWCNT), and ethylene glycol-modified MWCNTs (MWCNT-EG) have quite a rough surface morphology owing to the presence of MWCNT aggregates. As a result, the CPEE/MWCNT-PEG composite fiber exhibits noticeably increased thermal and tensile mechanical properties as well as a faster crystallization behavior, which stems from an enhanced interfacial interaction between the CPEE matrix and MWCNT-PEGs.     

Preparation and characterization of poly(L-lactic acid)/hollow silica nanospheres nanocomposites

This paper-reports the development of a unique nanocomposite material based on poly(L-lactic acid) and hollow silica nanospheres. The composites were produced by melt blending in a twin-screw extruder and then spun into fibers. In order to improve the compatibility between the polymer and the inorganic additive, the surface of the hollow silica nanospheres was modified by a silane coupling agent, acetoxypropyltrimethoxysilane. It was demonstrated by electron microscopy that the modified silica nanospheres were well-dispersed in the polymer matrix. The resulting nanocomposites exhibited slightly improved thermal stability, crystallinity and softness. Remarkably, the hollow spheres, which could encapsulate any active substances, remain intact after the melt processing, allowing promising applications in biomedical fields.     

Effects of nanoclay and short nylon fiber on morphology and mechanical properties of nanocomposites based on NR/SBR

Natural rubber and styrene butadiene rubber (NR/SBR) reinforced with both short nylon fibers and nanoclay (Cloisite 15A) nanocomposites were prepared in an internal and a two roll-mill mixer by a three-step mixing process. The effects of fiber loading and different loading of nanoclay (1, 3 and 5 wt. %) were studied on the microstructure and mechanical properties of the nanocomposites. The adhesion between the fiber and the matrix was improved by the addition of a dry bonding system consisting of resorcinol, hexamethylene tetramine and hydrated silica (HRH). This silicate clay layers was used in place of hydrated silica in a HRH bonding system for SBR/NR-short nylon fiber composite. Nanoclay was also used as a reinforcing filler in the matrix-short fiber hybrid composite. The cure and scorch times of the composites decreased while cure rate increased when the short fiber and nanoclay were added. The mechanical properties of the composites showed improvement in both longitudinal and transverse directions with increasing short fiber and nanoclay content. The structure of the nanocomposites was characterized with X-ray diffraction (XRD), scanning electron microscopy (SEM). X-ray diffraction results of nanocomposites indicated that the interlayer distance of silicate layers increased. The mechanical properties of nanocomposites (tensile, hardness and tear strength) are examined and the outcome of these results is discussed in this paper.     

Thermal and structure properties of biobased cellulose nanowhiskers/poly (lactic acid) nanocomposites

Cellulose nanowhiskers were used to improve the performance of poly (lactic acid) (PLA). The nanocomposites mixed with three different molecular weight of poly (ethylene glycol) (PEG) were characterized by mechanical testing, thermal gravimetry and differential scanning calorimetry. The tensile test showed an increase in tensile strength and elongation at break with the addition of PEG to PLA/CNW nanocomposites, the thermal analysis results showed an increase of crystallization temperature (T _c) and crystallization compatibility (larger crystallization and melting areas), which indicated that the cellulose nanowhiskers (CNW) and PEG or CNW alone should not be considered as nucleating agents for the PLA matrix; The CNW was homo-dispersed which contributed to decreasing mobility of polymer chain segments. The compatibility between hydrophobic PLA matrix and the hydrophilic CNW was improved by the addition of different molecular weight polymeric-PEG. The thermo gravimetric analysis indicated that the thermal stability of the different composites were reflected well in the region between 25 °C and 245 oC. The structure of the PLA/CNW/PEG composites was characterized by AFM, which showed that the CNW dispersed in the PLA matrix evenly.     

Characterization and mechanical properties of prepolymer and polyurethane block copolymer with a shape memory effect

The prepolymer and the final polyurethane (PU) block copolymer were synthesized by reacting 4,4-methylene bis(phenylisocyanate) with poly(tetramethylene glycol) and the prepolymer with 1,4-butanediol as a chain extender, respectively, to investigate the relation between phase separation and it’s resulting properties. According to FT-IR data, the phase separation of hard and soft segments in the prepolymer and the PU block copolymer grew bigger by increasing the hard segment content, and the PU showed more dominant phase separation than the prepolymer. The heat of fusion due to soft segments decreased in both the prepolymer and the PU by increasing the hard segment content, whereas the heat of fusion due to hard segments increased in the PU did not appear in the prepolymers. The breaking stress and modulus of the prepolymer increased by increasing the hard segment content, and the elongation at break decreased gradually, and the PU showed the highest breaking stress and modulus at 58 % hard segment content. However, the best shape recovery of the PU was obtained at 47 % hard segment content due to the existence of proper interaction among the hard segments for shape memory effect. Consequently, the mechanical properties and shape memory effect of the PU were influenced by the degree of phase separation, depending on the incorporation of chain extender as well as the hard segment content.     

A study of mechanical behavior and morphology of carbon nanotube reinforced UHMWPE/Nylon 6 hybrid polymer nanocomposite fiber

We report a phenomenal increase in strength, modulus, and fracture strain of ultra high molecular weight polyethylene (UHMWPE) fiber by 103 %, 219 %, and 108 %, respectively through hybridizing this fiber with Nylon 6 as a minor phase and simultaneously reinforcing it with single-walled carbon nanotubes (SWCNTs). Loading of Nylon 6 and SWCNTs into UHMWPE was 20.0 wt% and 2.0 wt%, respectively. Hybridized fibers were processed using a solution spinning method coupled with melt mixing and extrusion. We claim that the enhancement in strain-to-failure of the nanocomposites is due to induced plasticity in the hybridized Nylon 6-UHMWPE polymers. The enhancement in strength and stiffness in the nanocomposites is attributed to the load sharing of the SWCNTs during deformation. Differential scanning calorimetry (DSC), X-ray diffraction (XRD), scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FTIR) studies showed that changes in percent crystallinity, rate of crystallization, crystallite size, alignment of nanotubes, sliding of polymer interfaces and strong adhesion of CNT/polymer blends were responsible for such enhancements.     

POSS/polypropylene hybrid nanocomposite monofilaments by reactive extrusion

The Allyl-heptaisobutyl-polyhedral oligomeric silsesquioxane (AHO-POSS) grafted polypropylene (PP) was prepared by reactive extrusion and by physical blending routes. The structure and properties of physically blended and reactively blended POSS/PP nanocomposites were investigated by FTIR, wide-angle X-ray diffraction (WAXD), differential scanning calorimetry (DSC), thermogravimetric analysis, SEM, spherutlic growth and mechanical properties studies. Chemical bonding of POSS with PP in reactive extrusion was confirmed by FT-IR spectroscopy. DSC and TGA studies showed that the thermal stability of AHO-POSS/PP nanocomposite prepared by reactive extrusion improved significantly as compared to only physically blended nanocomposites. WAXD studies showed decrease in crystallinity of the AHO-POSS/PP nanocomposites prepared by reactive extrusion. SEM studies showed aggregation tendency in case of physically blended AHO-POSS/PP nanocomposites. Spherulite growth studies show reactive blending retards spherulite growth in PP polymer.     

Unique crystallization behavior of multi-walled carbon nanotube filled poly(lactic acid)

Although poly(lactic acid) (PLA) possesses many desirable properties such as miscible, reproducible, nontoxic, and biodegradable properties, extremely slow crystallization rate is a weak point in comparison with other commercial thermoplastics. Addition of nucleating agents can be a good method to increase the overall crystallization rate and multi-walled carbon nanotube (MWCNT) is generally known as a good nucleating agent as well as reinforcement. MWCNT reinforced PLA nanocomposites were prepared by melt blending and the unique nucleation and crystallization behaviors of pure PLA and MWCNT/PLA nanocomposites were investigated. Slow homogeneous nucleation and crystallization behavior of the pure PLA and fast heterogeneous crystallization behavior of MWCNT/PLA nanocomposites were observed. Crystallization behavior of MWCNT/PLA nanocomposites was irrespective of cooling rate and the peculiar behavior was due to fast heterogeneous crystallization caused by the nucleating effect of MWCNT and fast PLA chain mobility.     

Synthesis and properties of shape memory polyurethane nanocomposites reinforced with poly(ɛ-caprolactone)-grafted carbon nanotubes

Nanocomposites of polyurethane (PU) and multi-walled carbon nanotubes (MWNTs) were prepared via in-situ polymerization of poly(ɛ-caprolactone)diol (PCL)-grafted-MWNTs, 4,4′-methylene bis(phenyl isocyanate), and 1,4-butanediol. The grafting of PCL onto MWNTs was confirmed by Fourier transform infrared (FT-IR) spectroscopy and transmission electron microscopy (TEM). The nanocomposites showed more improved mechanical properties compared to conventional nanocomposites with the same MWNT loading. The thermo-responsive shape recovery as measured in a cyclic tensile test was observed to be approximately 80 % for in-situ nanocomposites, though it showed a reduced trend as the wt% of MWNTs increased. X-ray diffraction investigation also showed that the addition of MWNTs into the polyurethane increased the crystallinity. Scanning electron microscopy and TEM measurements showed better dispersion of MWNTs in the nanocomposites synthesized using in-situ method. Consequently, the presence of PCL-g-MWNTs made an important contribution to the enhancement of the mechanical and shape memory properties of polyurethane.     

Effect of CaCO3 contents on the properties of polyethylene nanocomposites sheets

Nanocomposites of high-density polyethylene/linear low-density polyethylene (HDPE/LLDPE) filled with untreated and surface treated nano-calcium carbonate (nCC) were prepared. The influence of isopropyl tri-(dioctylpyrophosphato) titanate (JN114) treatment of nCC on the morphology, mechanical, crystallization and flow properties of the nanocomposites were studied. The results of scanning electron microscopy (SEM) showed that JN114 treated nCC was better dispersion in the matrix than the untreated one. A fine dispersion of the treated nanoparticles in the nanocomposites was observed by transmission electron microscopy (TEM). The FTIR spectrum analysis revealed that the JN114 could change the surface properties of nCC, resulting in greater hydrophobicity of the surface and enhanced compatibility with nonpolar matrices. The tensile elastic modulus (E _c ) and Izod impact strength (SIC) of nanocomposites increased with the increasing of nCC content while tensile fracture strength (σ _b ) decreased. The JN114 treated nanocomposites had superior mechanical properties to those of the untreated ones. The compatibility of these nanocomposites was examined by DSC to estimate melting point (T _m ) and crystallization temperature (T _c ). Furthermore, the melt flow index (MFI) of the nanocomposite materials were measured. It was found that the MFI decreased with the addition of weight fraction of the nCC particles.     

Various nano-silica particles affecting dyeability of poly(ethylene terephthalate)/silica nanocomposite films

Poly(ethylene terephthalate) [PET] based nanocomposites containing three differently modified silica particles were prepared by melt compounding. The influence of type of nano-silica on dispersibility, thermal and dyeing properties of the resultant nanocomposite was investigated by various analytic techniques, namely, polarized optical microscopy (POM), scanning electron microscopy (SEM), differential scanning calorimetry (DSC), thermal gravimetric analysis (TGA), reflectance spectroscopy (RS), and light fastness. Optical microscopy images illustrated that nano-silica particles tended to increase the number of spherulites in the PET matrix which were dependent on nano-silica type and content. Thermal studies of the resultant nanocomposites showed a slight decrease in the melting temperature compared to a pristine PET. Silica nanocomposites were finally dyed with a disperse dye and their reflectances were determined by the aid of reflectance spectrophotometer. Such reflectances were converted to the corresponding color coordinate values which are indicative of dyeability of such nanocomposites.     

Preparation and crystallization behavior of polylactide nanocomposites reinforced with POSS-modified montmorillonite

We herein report the preparation and crystallization behavior of polylactide (PLA) nanocomposites reinforced with polyhedral oligomeric silsesquioxane-modified montmorillonite (POSS-MMT), which is prepared by exchanging sodium cations of pristine sodium montmorillonite (Na-MMT) with protonated aminopropylisobutyl polyhedral oligomeric silsesquioxane (POSS-NH₃ ⁺). PLA nanocomposites with 1–10 wt% POSS-MMT contents are manufactured via melt-compounding, and their structures and melt-crystallization behavior are investigated. It is characterized that POSS-MMT nanoparticles in the nanocomposites have an exfoliated structure of MMT silicates with POSS-NH₃ ⁺ and partial POSS-NH₂ crystals. DSC cooling thermograms suggest that the overall melt-crystallization rates of the nanocomposite with only 3 wt% POSS-MMT are remarkably enhanced in comparison with the neat PLA. From the isothermal crystallization analysis based on the Avrami model, the overall melt-crystallization of PLA/POSS-MMT nanocomposites is found to be dominated by the heterogeneous nucleation and three-dimensional spherulite growth. Isothermal melt-crystallization experiments using a polarized optical microscope show that the spherulite nucleation density of PLA/POSS-MMT nanocomposites is much higher than that of the neat PLA, whereas the spherulite growth rates of all the nanocomposites are almost identical with the rate of the neat PLA. It is concluded that the highly enhanced melt-crystallization rates of PLA/POSS-MMT nanocomposites stem from the dominant nucleation effect of POSS-MMT nanoparticles for PLA crystals.     

Functionalized graphene nanoplatelets/poly(ethylene oxide) nanocomposites: Correlation between crystallization behavior and mechanical performance

Poly(ethylene oxide) (PEO) nanocomposites containing pristine or functionalized graphene nanoplatelets (FGnP) prepared via solution blending and thermal and mechanical properties of nanocomposites were investigated. Chemical functionalization of graphene nanoplatelets was conducted through an amidation reaction between carboxylic acid groups of acidified graphene and hydroxyl groups of polyethylene glycol (PEG). An interfacial linkage and a good dispersion of FGnP was observed via scanning electron microscope (SEM). Differential scanning calorimetry (DSC) analysis revealed that the degree of crystallinity of samples decreased by addition of graphene nanoplatelets, while the size of spherulites increased as indicated by polarized optical microscope (POM). A lower degree of crystallinity and larger spherulites were detected in the case of FGnP. Filler/matrix interfacial adhesion was also remarkably influenced the mechanical properties of PEO as an effective reinforcement of matrix obtained upon the addition of FGnP nanosheets compared to untreated graphene.     

Isothermal crystallization behavior of PAR/PBT composite prepared by island-in-a-sea fiber method

The PAR fiber reinforced PBT composite was manufactured using the PAR/PBT island-in-a-sea fiber. The isothermal crystallization kinetics of the PAR/PBT composite and the neat PBT resin were investigated in the temperature range of 187–199 °C. To calculate the Avrami parameters for analyzing the crystallization behavior, crystallization peaks were measured and analyzed in terms of the crystallization temperature and the inclusion of the PAR fiber. The crystallization rate of the PBT is faster than that of the PAR/PBT composite from the analysis of their relative crystallinity. Consequently, it is considered that the PAR fiber interrupted the crystal nucleation and growth of the PBT matrix. It can be confirmed with the crystallization half time and the crystalline morphologies at the chosen isothermal temperatures.     

Preparation and characterization of iptycene polymer/SWCNT nanocomposites

To enhance the strength while retaining the ductility of triptycene polyester, triptycene polyester/SWCNT nanocomposites were prepared. First, two different types of triptycene polyesters containing triptycenes that differ in size were synthesized and their mechanical and thermal characteristics were studied. Thermal analysis showed that the polyester containing the larger triptycene posed as a bigger hindrance factor to polymer chain-packing, resulting in lower crystallinity. Although the presence of triptycene interfered the packing of polymer chains, the increased size and amount of triptycene enhanced the thermal stability of the polymer. For the smaller sized triptycene-polyester/SWCNT composites, higher SWCNT content increased the stiffness and strength of the composite, but at the expense of the ductility. The increase in SWCNT content in the larger-sized triptycene polyester/SWCNT composites somewhat decreased the stiffness as well as the ductility of the polymer.     

Compressive viscoelastic properties of softwood kraft lignin-based flexible polyurethane foams

Softwood kraft lignin (SKL)-based water-blown flexible polyurethane foams were prepared using SKL as a crosslinking agent and a hard segment polyol. Polyethylene glycol (PEG) as a soft segment diol and 2,4-toluene diisocyanate (TDI) were used. While increasing hard segment content caused the increase in crosslink density in foams, the foams became more and more viscous with increasing hard segment content due to the distinctive phase heterogeneity in foams. In this case, the contributiveness of the filler-like behaviors of separated hard segments always overtook the crosslinking effects derived from SKL in terms of overall viscoelasticity, thus the resultant viscometric properties such as tanδ _max and hysteresis loss increased as hard segment content increased. Furthermore, increasing M _n,PEG caused the severer microphase separation and intensified the filler effects in foams, thus the foams became more viscous with increasing M _n,PEG. The 25 % and 65 % CFD values and Young’s moduli of foams increased with increasing hard segment content due to the increase in crosslink density for foams, and the properties also increased with increasing foam density. Most of foams showed the support factors in the range of 2–3, which are suitable values for cushioning use. Even though the microscopic deformation behaviors in foams are irrelevant to foam density, the cyclic compressive tests showed that the higher foam density possess the better shape recovery performances.     

Incorporation of surface modified graphene nanoplatelets for development of shape memory PLA nanocomposite

In this study, a temperature sensitive shape memory polymer (SMP) system based on polylactic acid (PLA) has been developed and the effect of graphene nanoplatelets (GNPs) on the shape memory properties was evaluated. Dispersion of GNPs in PLA was improved with the aid of a zwitterionic surfactant. X-ray diffraction (XRD) and transmission electron microscopy (TEM) showed that the surface modified graphene nanoplatelets (SMGNPs) were exfoliated and homogenously dispersed in the PLA matrix due to enhancement of the polymer-graphene interaction. Mechanical properties of the samples namely stiffness and elasticity were increased upon incorporation of graphene nanoplatelets accompanied by their good dispersion in the PLA matrix. Furthermore, differential scanning calorimetry (DSC) revealed that the nucleation effect of graphene promote the crystallization and noticeably enhanced the degree of crystallinity. Finally, prominent mechanical properties along with high degree of crystallization due to fine dispersion of surface modified graphenes, resulted in drastic improvement in shape memory performance.     

Effects of heat treatment on the properties of bamboo fiber/polypropylene composites

In this paper, the effects of heat treated parameters on the properties of bamboo fiber (BF) / polypropylene (PP) composites were investigated. The crystallization properties of BF/PP composites after heat treatment were characterized by differential scanning calorimetry (DSC), and the mechanical properties were measured. The results showed that the crystallinities of the heat treated composite were enhanced compared with that of the untreated. When the heat treated time was 30 mins, the crystallinities became almost unchanged. However, the crystallinity decreased after 12 h heat treatment. In addition, when the heat treated temperature was above 90 °C, the higher the temperature was, the higher the crystallinities became. Moreover, the tensile strengths of BF/PP composites increased and then decreased with increasing heat treated time, while the impact strengths had a decreasing trend. In the meanwhile, the tensile strengths increased but the impact strengths decreased as the heat temperature increased.     

Crystallization of poly(vinylidene fluoride)-SiO2 hybrid composites prepared by a Sol-gel process

Organic-inorganic hybrid composites consisting of poly(vinylidene fluoride) (PVDF) and SiO₂ were prepared through a sol-gel process and the crystallization behavior of PVDF in the presence of SiO₂ networks was investigated by spectroscopic, thermal and x-ray diffraction measurements. The hybrid composites obtained were relatively transparent, and brittleness increased with increasing content of tetraethoxysilane (TEOS). It was regarded from FT-IR and DSC thermal analyses that at least a certain interaction existed between PVDF molecules and the SiO₂ networks. X-ray diffraction measurements showed that all of the hybrid samples had a crystal structure of PVDFγ-phase. Fresh gel prepared from the sol-gel reaction showed a very weak x-ray diffraction peak near 2θ=21° due to PVDF crystallization, and intensity increased gradually with time after gelation. The crystallization behavior of PVDF was strongly affected by the amount of SiO₂ networks. That is, SiO₂ content directly influenced preference and disturbance for crystallization. In polymer-rich hybrids, SiO₂ networks had a favorable effect on the extent of PVDF crystallization. In particular, the maximum percent crystallinity of PVDF occurred at the content of 3.7 wt% SiO₂ and was higher than that of pure PVDF. However, beyond about 10 wt% SiO₂, the crystallization of PVDF was strongly confined.