Synthesis of graft copolymers based on polyphenylene xylylene and fullerene grafted polystyrene

Graft copolymers containing poly(phenylene xylyene) (PPX) backbone and polystyrene fullerene (PSFu) grafting chains (PPX‐g‐PSFu) were prepared by using a purposed synthetic route comprising a combination of reaction mechanisms namely the modified Wessling route, an iniferter polymerization, and an atom transfer radical addition (ATRA). The monomer was first prepared by reacting dichloroxylene with tetrahydrothiophene. After that the monomer was polymerized in a sodium hydroxide solution to provide a polymer precursor. Subsequently, the polymer precursor was modified by reacting it with a dithiocarbamate (DTC) compound. The macroiniferter was obtained and then copolymerized with styrene and chloromethylstyrene via an iniferter polymerization. Finally, the graft copolymer was reacted with fullerene through an ATRA technique to attach the C60 groups onto the graft copolymer molecule. The products obtained from each of the steps were characterized by using various techniques including Fourier transform infrared spectroscopy, proton nuclear magnetic resonance spectroscopy, gel permeation chromatography, differential scanning calorimetry, UV–visible spectroscopy, and thermal gravimetric analysis. The aforementioned results suggest that the graft copolymers were prepared. The grafting yield and grafting efficiency were found to increase with the monomers concentration and the amount of DTC used. Some homopolymer contaminants also occurred but those could be minimized and subsequently removed by extraction with selective solvents. These graft copolymer products might be used for the development of a bulk heterojunction polymer solar cell. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2010     

Effect of acrylic diblock copolymer upon interfacial adhesion

The preparation and adhesion properties of poly(methyl methacrylate–butyl acrylate)[P(MMA-b-BA)] diblock copolymers have been studied. Block copolymers were analyzed by ¹H-NMR, DSC, and SEC, and confirm the synthesis of diblock copolymers, using the iniferter route. Investigation of peel strength in laminate joints, reinforced with various block copolymers, suggests that adhesion depends on both molecular weight and composition. When the copolymer contains mainly PMMA block, molecular weight has a marked effect, with adhesion being enhanced at higher copolymer molecular weight. For other PBA/PMMA compositions, no reinforcement was seen, irrespective of molecular weight. © 1996 John Wiley & Sons, Inc.     

In situ sol–gel synthesis of tungsten trioxide networks in polymer electrolyte: Dual-functional solid state chromogenic smart film

The novel electro-photochromic solid electrolyte films were successfully synthesized by in situ sol–gel synthesis of tungsten trioxide (WO₃) working electrode within gelatin/lithium cosolvent system. The transparent free-standing single-layer film with adhesiveness and flexibility, darken significantly under the UV radiation with photo-response time of 30 s and gradually reversed once the source of UV was blocked. Moreover, casted film on the indium tin oxide (ITO) glass showed electrochromic (EC) behavior as well in presence of ion storage counter electrode. X-ray diffraction analysis indicates the amorphous nature of an in situ synthesized gelatin-based film. The prepared film containing 30 wt% LiClO₄ and 10 wt% WO₃ (sample designated as GLi30W10) shows ionic conductivity value of 1.1 × 10⁻⁴ S/cm. The EC performances of the device with the following configuration; ITO/GLi30W10/NiO/ITO, was investigated by means of UV and cyclic voltammograms. Good performances and fast electro-response times (2 s/1 s) of the device were demonstrated with coloration efficiency of 51.54 cm²/C.     

Methanol permeability and properties of DMFC membranes based on sulfonated PEEK/PVDF blends

Proton exchange membranes for a direct methanol fuel cell were prepared by blending poly(vinylidene fluoride) [PVDF] with sulfonated poly(etheretherketone) [SPEEK]. The effects of PVDF content on methanol permeability in the blend membranes were investigated by using a diffusion cell and gas chromatography technique. The thermal resistance and proton conductivity of the membranes were also determined by using a thermal gravimetric analysis (TGA) and an impedance analysis technique, respectively. It was found that methanol permeability in the blend membranes decreased with PVDF content at the expense of proton conductivity. The methanol permeability values of the blend membranes are much lower than that of Nafion 115, whereas proton conductivities of the membranes are comparable to that of Nafion. The thermal stability of these blend membranes are above 250°C which is sufficiently high for use in DMFC. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 102: 5941–5947, 2006     

A study on morphology and physical properties of natural–acrylic rubber blends

Morphology and physical properties of natural–acrylic rubber blends were investigated as a function of blend compositions and mixing methods. In the first method, the masticated natural rubber was cross‐blended with the acrylic rubber for 15 min, followed by a sequential addition of vulcanizing chemicals (ZnO, stearic acid, MBT, sodium stearate, and sulfur), and the mixing was terminated within 15 min. In the second method, the masticated natural rubber was premixed with its relevant vulcanizing chemicals (excepting the sulfur) for 7 min, followed by blending it with the acrylic rubber and sodium stearate for 20 min. Finally, the sulfur was added and the mixing was continued for further 3 min before termination. The resulting blends were vulcanized to their optimum cure time in a compression mold. The rubber sheet was cut into a dumbbell‐shaped specimen, and tensile properties were determined at a cross‐head speed of 500 mm/min. The morphology of the blends was examined with scanning electron microscopy (SEM). The SEM specimen was prepared by cryo‐fracturing, followed by staining with OsO₄. It was found that all of the rubber blends were immiscible, as shown by there being two separated phases in the SEM micrographs. The result was in a good agreement with that from a thermal analysis (using a differential scanning calorimeter), which showed two glass transition temperatures. Morphology of the rubber blends changed from a cocontinuous morphology to a dispersed particle morphology as the natural rubber content was increased from 20% to 80% by weight. Increasing the natural rubber content enhanced tensile properties of the rubber blends at the expense of their oil and heat resistance. Most of these properties being examined seemed to be unaffected by the mixing method, with the exception of the retention of tensile strain after aging. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 86: 1532–1539, 2002     

Effect of curing agent on interfacial adhesion in acrylic polymer-based laminates

The effect of crosslinking on interfacial adhesion between an acrylic elastomer and poly(methyl methacrylate) has been studied using a 90° peel test. Elastomers were master-batched with a 1 : 10 sulfur/sodium mixture. The compounded elastomer was then bonded with poly(methyl methacrylate) by in situ curing at various temperatures. Variations in the curing affect both the mechanism of adhesion and separation. The relationship between peel strength and crosslink density is found to be P = kM_c. Crosslinking at relatively low temperatures produced a partially crosslinked elastomer that leads to high peel strengths. When crosslinked at 180°C, the acrylic elastomer was completely cured, and the peel strength decreased by more than 80%. This is consistent with an optimum level of crosslinking required for peel strength. © 1998 John Wiley & Sons, Inc. J Appl Polym Sci 67:1277–1284, 1998     

Crystallization and thermomechanical properties of PLA composites: Effects of additive types and heat treatment

This research work has concerned a study on thermomechanical and crystallization properties of poly(lactic acid) (PLA) composites containing three different types of additives; namely: kenaf fiber (20 pph), Cloisite30B nanoclay (5 pph), and hexagonal boron nitrile (h‐BN; 5 pph). The composites were prepared using a twin screw extruder before molding. Crystallization behaviors of the various composites were also examined using a differential scanning calorimetry. By adding the additives, tensile modulus of the polymer composites increased, whereas their tensile strength and elongation values decreased as compared to those of the neat PLA. Heat distortion temperature (HDT) values of the materials slightly increased, for about 3–5°C. However, after annealing at 100°C, HDT values of the fabricated PLA composites rapidly increased with annealing time before reaching a plateau after 10 min. The HDT values of above 120°C were achieved when 20 pph kenaf fiber was used as an additive. The above results were in a good agreement with DSC thermograms of the composites, indicating that percentage crystallinity of the materials increased on annealing and crystallization rate of the PLA/kenaf system was the highest. © 2012 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013     

Investigation of the photodegradation behaviors of an ethylene/vinyl acetate copolymer solar cell encapsulant and effects of antioxidants on the photostability of the material

This study concerns the photodegradation and stabilization of a solar cell encapsulating material made from ethylene/vinyl acetate copolymer (EVA). EVA was compounded with various additives in a twin‐screw extruder. After that, the extruded film was cured in a hydraulic compression mold before being exposed to ultraviolet (UV) radiation at an ambient temperature for 800 h. The thermal stability of the material was also studied through the aging of the sample at 90°C for 2000 h. The tensile strength of the unstabilized EVA decreased only slightly after the thermal aging. On the other hand, the strength of the material decreased noticeably after the UV irradiation. Fourier transform infrared spectra of various EVA films revealed that there was no deacetylation occurring after the UV irradiation. However, results from the swelling test and swollen‐state NMR suggested that the polymer degraded via a chain‐scission mechanism. After compounding with some antioxidants, most of the EVA films scarcely degraded after the UV irradiation, with the exception of the EVA compounded with a combination of the aromatic phosphate compound (0.1 phr) and hindered amine light stabilizer (0.1 phr). The results are discussed in light of an antagonism effect that occurred because of the aforementioned combination. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci, 2008     

Methanol permeability and proton conductivity of direct methanol fuel cell membranes based on sulfonated poly(vinyl alcohol)–layered silicate nanocomposites

Layered silicate nanocomposite membranes to be used as electrolyte polymeric membranes in a direct methanol fuel cell were prepared through the mixing of poly(vinyl alcohol) (PVA) with various amounts (2, 4, and 5% w/w) of sodium montmorillonite layered silicate nanoclay. The proton conductivity of the polymer was induced by the reaction of the polymer with sulfosuccinic acid. After that, a solution of the sulfonated PVA–layered silicate nanocomposite was cast into membranes. The proton conductivity and methanol permeability of the membranes were determined with a four-point probe technique and a gas chromatography technique, respectively. In addition, structures of the nanocomposite membranes were characterized with X-ray diffraction, differential scanning calorimetry, and Fourier transform infrared techniques. The mechanical properties of the nanocomposite membranes were also determined with a universal testing machine. From the results, it was found that the water uptake, proton conductivity, and methanol permeability of the membranes initially decreased after a 2% (w/w) concentration of the layered silicate was added. Above this nanoclay loading, the water uptake of the membranes increased again. The results were examined in the light of the interaction between the clay and sulfonated polymer, and the steric effect provided the exfoliation of the nanoclay. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2008     

Dynamic vulcanization of acrylic rubber‐blended PVC

Poly(vinyl chloride) was blended with an acrylic rubber at a variety of blending ratio using a twin‐screw extruder. The acrylic rubber was compounded with sulfur and sodium stearate in a two‐roll mill prior to the blending. Dynamic vulcanization was performed in a compression mould at 170°C. Mechanical properties of the blends were determined by using a tensile testing machine. Scanning electron microscope was used to examine morphology of these blends. Degree of crosslinking of acrylic rubber in the blends was evaluated by using a differential scanning calorimeter. It was found that the normal blends are miscible regardless of the blending variables. By performing dynamic vulcanization, however, the blends became immisicible, showing a typical dispersed particle morphology, which was accompanied by a remarkable improvement of tensile properties. The screw‐rotating speed was an important parameter affecting particle size and crosslink density of the rubber phase, which in turn controlled the tensile toughness of the blends. On the one hand, tensile toughness increased with the speed because of the decreasing particle size. On the other hand, the toughness decreased with the speed because of the decreasing crosslink density of the rubber. As a result, there was an optimum speed for each blend ratio, which corresponded to the maximum toughness. © 2003 Wiley Periodicals, Inc. J Appl Polym Sci 88: 2657–2663, 2003