Tribological and electrical properties of silica‐filled epoxy nanocomposites

The tribological and electrical properties of epoxy composites filled with nano‐sized silica particles are studied and discussed in this article. To enhance the interfacial interaction between the fillers and the matrix, nanoparticles were pretreated with silane coupling agent. Dry sliding wear tests were carried out with configuration of composite sample on a rotating steel disc. Electrical measurements such as AC breakdown voltage, at 50 Hz, high voltage‐low current arc resistance and wet tracking resistance were carried out. The results reveal the influence of nanosized silica loading on wear resistance of the epoxy. It is observed that 10 wt% loading of silica is very effective in reducing the wear loss. With further increase of silica filler loading, the nanoparticles agglomerated and resulted in increase of the specific wear rate. The influence of silica particles on the specific wear rate is more pronounced under sliding wear situation. The influence of silica particle loading on epoxy is evident in the results of electrical parameters like dielectric strength, arc resistance and tracking resistance. These parameters showed improvement with filler loading up to 15 wt% and beyond this value of filler loading noticeable deterioration was observed. The effects of electrical stresses in the morphologies of the surfaces of epoxy nanocomposites are discussed. POLYM. COMPOS., 2011. © 2011 Society of Plastics Engineers     

Sol- gel synthesis of Ga2O3 nanorods and effect of precursor chemistry on their structural and morphological properties

Synthesis of mono-crystalline Ga₂O₃ Nanorods was done by sol-gel transformation of gallium(III) isopropoxide (Ga(OPrⁱ)₃). XRD studies were done to determine the planes and crystal structure of synthesized nanorods that showed the synthesis of β-Ga₂O₃(a). TEM studies of synthesized Ga₂O₃ confirmed the synthesis of monocrystalline β-Ga₂O₃ nanorods. To study the effect of precursor chemistry and to determine role of precursor structures on the crystal structure, phase and morphology of the Ga₂O₃, a new modified precursor complex was synthesized. The reaction of Ga(OPrⁱ)₃ with N-phenylsalicylaldimine, [C₆H₄(OH)CH=N(C₆H₅)] in 1:1?M ratio yielded [{(H₅C₆)N?=?CH-C₆H₄O}Ga(OPrⁱ)₂]. The newly synthesized complex was characterized by elemental analyses, molecular weight measurement, FT-IR and NMR (¹H and ¹³C) spectral studies. Spectral studies of the modified complex suggest the presence of bi-dentate mode of attachment of Schiff's base in the solution state. Sol-gel transformations of [{(H₅C₆)N?=?CH-C₆H₄O}Ga(OPrⁱ)₂] in organic medium, yielded γ-Ga₂O₃(b), as found by XRD studies. TEM image of the sample (a) revealed the formation of nano-rods of oxide with average diameter of ~100?nm whereas the TEM image of sample (b) showed presence of nano-sized particles of oxide with average particle size of 10?nm. Morphological and compositional studies of synthesized samples (a) and (b) were carried out using SEM and EDX. The method provides a possibility of large scale synthesis of dissimilar shaped and pure Ga₂O₃ nanoparticles.     

Studies of the curing kinetics and thermal stability of epoxy resins using a mixture of amines and anhydrides

This article describes the curing and thermal behavior of diglycidyl ether of bisphenol A with phthalic anhydride (PA)/pyromellitic anhydride/diaminodiphenyl sulfone (DDS) or a mixture of anhydrides and amines in varying ratios as curing agents. The kinetics of the curing behavior was investigated with a multiple‐rate method. The activation energy of the curing reaction as determined in accordance with Ozawa's method was found dependent on the structure of the anhydride and on the ratio of amines to anhydrides. The activation energy was highest with sample DP3 (0.25 : 0.75) and DM3 (0.25 : 0.75). We evaluated the thermal stability of epoxy resin, cured isothermally, by recording thermogravimetric traces in a nitrogen atmosphere. The char yield was highest for resins cured with a mixture of DDS and PA (0.5 : 0.5) and a mixture of DDS and pyromellitic dianhydride (0.25 : 0.75). © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 100: 3919–3925, 2006     

Methacrylate/acrylate terminated derivatives of diglycidyl hexahydrophthalate: Synthesis,structural, and thermal characterization

Mono‐ or di(meth)acrylate‐terminated derivatives of diglycidyl hexahydrophthalate (ER) were prepared by reacting 1 : 1 or 1 : 2M ratio of ER and methacrylic acid or acrylic acid. These vinyl ester (VE) resins were characterized by determining epoxy equivalent weight, acid number, and molecular weight by gel permeation chromatography. Structural characterization was done by FTIR and ¹H NMR spectroscopy. In the ¹H NMR spectra of acrylate‐terminated VE resins, three proton resonance signals were observed in the region 5.8–6.4 ppm due to vinyl group while in methacrylate‐terminated VE resins only two proton resonance signals due to vinylidene protons were observed at 5.6–6.1 ppm. The Brookfield viscosity (room temperature (25 ± 2)°C) of these resins diluted with varying amounts of MMA was determined at 20 rpm. Curing behavior was monitored by determination of gel time and differential scanning calorimetry. An exothermic transition was observed in the DSC scans in the temperature range of (81–150)°C. Isothermal curing of MMA‐diluted VE resins containing AIBN as an initiator was done at 60°C for 2 h in N₂ atmosphere, and then heating for another 2 h in static air atmosphere. Thermal stability of isothermally cured resins in N₂ atmosphere was evaluated by thermogravimetric analysis. All cured resins decomposed above 310°C in single step. Thermal stability of the cured resins having acrylate end caps was marginally higher than the resins having methacrylate end groups. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci, 2006     

Studies with inorganic precipitate membrane: evolution of thermodynamically effective fixed charge density and test of the most recently developed theory of membrane potential based on the principles of non-equilibrium thermodynamics

Electrical potentials developed across nickel, manganese chromate and cupric iodide membranes using various 1:1 electrolytes are reported. Thermodynamically effective fixed charge density, which is an important parameter governing the membrane phenomena, has been evaluated by the recently developed theory of Nagasawa et al. Most recently developed theories of Toyoshima and Nozaki based on the principles of the irreversible thermodynamics has been examined to predict the bi-ionic potentials developed across the membranes. Theoretical predictions were borne out quite satisfactorily by our experimental results.     

Fabrication of poly (vinyl alcohol)/ovalbumin/cellulose nanocrystals/nanohydroxyapatite based biocomposite scaffolds

Biocomposite scaffolds composed of PVA, ovalbumin, cellulose nanocrystals, and nanohydroxyapatite were fabricated by freeze-drying method. The results revealed that the different fractions of nanohydroxyapatite and cellulose nanocrystals provide the mechanical strength and stiffness to the desired biocomposite scaffolds. In vitro biomineralization showed the formation of apatite onto the surface of obtained biocomposite scaffolds and increased as amount of nanohydroxyapatite increased. The obtained results suggest that the different combinations of these four biomaterials can be used to fabricate highly porous scaffolds with desired mechanical performance and degradation rate by adjusting ratio for potential use in low load-bearing applications.     

Electrical and mechanical properties of PMMA/reduced graphene oxide nanocomposites prepared via in situ polymerization

We report the effect of filler incorporation techniques on the electrical and mechanical properties of reduced graphene oxide (RGO)-filled poly(methyl methacrylate) (PMMA) nanocomposites. Composites were prepared by three different techniques, viz. in situ polymerisation of MMA monomer in presence of RGO, bulk polymerization of MMA in presence of PMMA beads/RGO and by in situ polymerization of MMA in presence of RGO followed by sheet casting. In particular, the effect of incorporation of varying amounts (i.e. ranging from 0.1 to 2 % w/w) of RGO on the electrical, thermal, morphological and mechanical properties of PMMA was investigated. The electrical conductivity was found to be critically dependent on the amount of RGO as well as on the method of its incorporation. The electrical conductivity of 2 wt% RGO-loaded PMMA composite was increased by factor of 10⁷, when composites were prepared by in situ polymerization of MMA in the presence of RGO and PMMA beads, whereas, 10⁸ times increase in conductivity was observed at the same RGO content when composites were prepared by casting method. FTIR and Raman spectra suggested the presence of chemical interactions between RGO and PMMA matrix, whereas XRD patterns, SEM and HRTEM studies show that among three methods, the sheet-casting method gives better exfoliation and dispersion of RGO sheets within PMMA matrix. The superior thermal, mechanical and electrical properties of composites prepared by sheet-casting method provided a facile and logical route towards ultimate target of utilizing maximum fraction of intrinsic properties of graphene sheets.     

Structural details, electrical properties, and electromagnetic interference shielding response of processable copolymers of aniline

Processable copolymers of aniline with 2-alkylanilines were prepared by in situ chemical oxidative polymerization route. Formation of copolymers was confirmed by X-ray diffractometer (XRD), UV–Vis, and solubility measurements. XRD revealed that copolymerization leads to increase in inter-chain spacing and reduction of doping levels. UV–vis results showed that incorporation of substituted anilines in copolymeric backbone leads to decrease in conjugation, the extent of which is directly related to size of alkyl substituent. The electrical conductivities of these copolymers were slightly less than pure polyaniline, but noticeable improvement in the solution processability was observed. In addition, these copolymers also provided shielding against electromagnetic interference (EMI) with ~99 % attenuation of incident energy. Among various copolymers, 95:5 copolymer of aniline with 2-isopropyl aniline (CP95Ip) gave best performance in terms of electrical conductivity (12.8 S/cm), solubility (4.9 g/L in N-methyl pyrrolidone), and EMI shielding effectiveness (?23.2 dB) values.     

Rheological characterization of raw and roasted green gram pastes

Rheological properties of raw and roasted green gram pastes have been determined at different moisture contents (52–56 g/100 g) and temperatures (10–40 °C). These pastes exhibit shear-thinning behavior and possess yield stress. Cross model is suitable (0.986 ≤ r ≤ 0.999, p ≤ 0.01) to explain the flow characteristics of the pastes. The Cross model parameters such as zero-shear viscosity and relaxation time are sensitive to concentration of solids in the paste as well as temperature of measurement, and vary widely between raw and roasted samples. The effect of temperature on the apparent viscosity follows the Arrhenius type relationship (r ≥ 0.961, p ≤ 0.01). The viscoamylographic indices and trypsin inhibitor content are also different for raw and roasted samples. The roasted pastes show a smooth and cohesive microstructure. The optimized sample of roasted flour having a moisture content of 55 g/100 g is suitable as bread spread with appropriate stickiness and spreadability.     

Non-fluorinated hybrid composite membranes based on polyethylene glycol functionalized polyhedral oligomeric silsesquioxane [PPOSS] and sulfonated poly(ether ether ketone) [SPEEK] for fuel cell applications

Novel hybrid composite membranes were prepared by blending poly(ethylene glycol) functionalized polyhedral oligomeric silsesquioxane [PPOSS] as nanofiller in varying concentration ranging from 1 to 5% (w/w) into sulfonated poly(ether ether ketone) [SPEEK] with degree of sulfonation ～55% for proton exchange membrane fuel cells [PEMFCs]. The effect of incorporation of PPOSS into SPEEK matrix was investigated in terms of thermomechanical and morphological properties, water uptake and proton conductivity of SPEEK. All the composite membranes were thermally and mechanically stable up to 250 °C. Transmission electron microscopy (TEM) revealed that the smallest particle size (～100 nm) of PPOSS was found for SPEEK membranes containing 2% (w/w) PPOSS where as agglomeration (～300 nm) was observed at higher loadings of PPOSS. The proton conductivity was found to be dependent on the morphology and was independent of the amount of water present in the membranes. At 100 °C and 100% RH, the highest proton conductivity (47 mS/cm compared 34 mS/cm for neat SPEEK i.e. an increase of ～51%) was recorded at 2% (w/w) PPOSS contents followed by a decrease on further addition of PPOSS.The water uptake of composite membranes increased with concentration of PPOSS while maintaining their hydrolytic stability at 100 °C for more than 24 h.