Dynamic mechanical analysis and thermal properties of LLDPE/EVA/modified silica nanocomposites

The effect of hexamethylene disilazane modified nanosilica on the dynamic mechanical analysis (DMA), crystallization, melting and thermal degradation behavior of linear low density polyethylene/ethylene vinyl acetate copolymer (LLDPE/EVA) blends are explored.Detailed DMA analysis is carried out in order to investigate the reinforcing behavior of nanosilica adopting Kerner–Nielson model. Oxidative degradation and thermal stabilities of samples are also studied by the thermogravimetery analysis. The high content of nanosilica particles results in significant shift of degradation temperature to higher temperatures in the oxygen atmosphere. This behavior might be attributed to the barrier properties of nanoparticles against oxygen and gaseous degradation products. However, incorporation of modified nanosilica into LLDPE/EVA blend is decreased the onset of degradation temperature of the unfilled system. In nitrogen atmosphere, no changes are observed in the thermal degradation range and only a reduction is documented in the onset of degradation temperature. Considering important role of onset of degradation temperature, activation energy of starting of degradation temperature is calculated utilizing Kissinger-Ozawa model in both oxygen and nitrogen atmospheres. Results showed that activation energy of degradation reaction is decreased by ∼ 20 kJ/mol. This decrease is owing to the release of modifiers from the nanoparticles.     

Improvement of adhesion and paint ability of EVA copolymers with different vinyl acetate contents by treatment with UV-ozone

The surface modifications produced by UV-ozone treatment of two ethylene-vinyl acetate (EVA) copolymers containing 12 and 20 wt% vinyl acetate (EVA12 and EVA20 respectively) were studied. The treatment with UV-ozone improved the wettability of both EVAs due to the creation of new carbon–oxygen moieties. The extent of these modifications increased with increasing length of the treatment and the modifications produced in EVA20 were produced for shorter lengths of treatment. The UV-ozone treatment also created roughness and heterogeneities on the EVA surfaces. Whereas roughness formation prevailed on the UV-ozone treated EVA12, important ablation was dominant on the treated EVA20. T-peel strength values in joints made with polychloroprene adhesive increased when the EVAs were treated with UV-ozone. Short length of UV-ozone treatment (1 min) produced higher T-peel strength in joints made with EVA20 whereas higher T-peel strength values in joints made with EVA12 were obtained after treatment for 5–7.5 min in which a cohesive failure into a weak boundary layer on the treated EVA surface was found. Furthermore, the adhesion of UV-ozone treated EVA20 to acrylic paint increased. Finally, the ageing resistance of the treated EVA/polychloroprene adhesive joints was good and the surface modifications on the UV-ozone treated EVAs lasted for 24 h after treatment at least.     

Ni–Fe mixed oxides prepared by calcination of layered double hydroxides: Potential pigments for the ceramic industry

Mixed Ni,Fe oxides have been prepared by calcination of precursors with the hydrotalcite-type structure which had been prepared by the reverse micelle method using different surfactants. The solids have been characterized by several physicochemical techniques: Powder X-ray diffraction, nitrogen adsorption–desorption at −196 °C for specific surface area assessment, particle size distribution, UV–vis spectroscopy, and temperature-programmed reduction. The solids are formed by NiO and NiFe₂O₄ (spinel) and their properties depend on the experimental conditions used to prepare the hydrotalcite-type precursor. The crystallite size is larger for the spinel crystallites than for the NiO crystallites and in all cases depends on the surfactant used and the pH during the synthesis. The original, uncalcined samples, show intense mainly yellow color, but on calcination almost all of them change to dark brown or even almost black; only when using a cyclic surfactant the color is markedly different from that obtained when linear surfactants are used.     

Constructing General Orthogonal Fractional Factorial Split-Plot Designs

While the orthogonal design of split-plot fractional factorial experiments has received much attention already, there are still major voids in the literature. First, designs with one or more factors acting at more than two levels have not yet been considered. Second, published work on nonregular fractional factorial split-plot designs was either based only on Plackett–Burman designs, or on small nonregular designs with limited numbers of factors. In this article, we present a novel approach to designing general orthogonal fractional factorial split-plot designs. One key feature of our approach is that it can be used to construct two-level designs as well as designs involving one or more factors with more than two levels. Moreover, the approach can be used to create two-level designs that match or outperform alternative designs in the literature, and to create two-level designs that cannot be constructed using existing methodology. Our new approach involves the use of integer linear programming and mixed integer linear programming, and, for large design problems, it combines integer linear programming with variable neighborhood search. We demonstrate the usefulness of our approach by constructing two-level split-plot designs of 16–96 runs, an 81-run three-level split-plot design, and a 48-run mixed-level split-plot design. Supplementary materials for this article are available online.     

Liquid-state interfacial reactions in Sn–Zn/Pd couples and phase equilibria of the Sn–Zn–Pd system at 260 °C

This study investigated the effects of Zn contents on the reaction products and microstructural evolution in the liquid/solid Sn–Zn/Pd interfacial reactions at 260 °C. A uniform Pd₂Zn₉ layer was formed at the Sn–9 wt.%Zn/Pd interface. The reaction phase transited from Pd₂Zn₉ to PdSn₄ when the Zn content decreased from 2 wt.% to 1 wt.%. The most striking feature is that the PdSn₄ growth was greatly suppressed with only 0.5 wt.% Zn addition in solders. Additionally, a drastic microstructural evolution was observed in the Sn–1.5 wt.%Zn/Pd reaction. The Pd₂Zn₉ layer was initially formed and then it was detached from the interface due to the decrease in the Zn content. Subsequently, the dominant phase changed to the PdSn₄ phase. Furthermore, a partial isothermal section in the Sn–Zn–Pd ternary system (less than 20 at.%Pd) at 260 °C was experimentally determined. The liquid apex of the liquid + PdSn₄ + Pd₂Zn₉ tie-triangle was located at Sn–2.7 at.%Zn–1.0 at.%Pd. The phase transition from Pd₂Zn₉ to PdSn₄ in the interfacial reactions was in good agreement with the phase equilibria relationship.     

Fracture surface evolution and apparent delamination toughness in split composite beam specimens subjected to mixed mode I–III loading

The influence of specimen twisting during global anti-plane shear loading in composite split beam specimens is studied. Tests were conducted on specimens with different thicknesses and delamination lengths to produce different amounts of specimen twisting prior to fracture. It is shown that specimen twisting causes mode I stresses to develop, thereby producing mixed mode I–III conditions along the delamination front. This causes near-tip transverse cracks to initiate, prior to delamination advance, at an orientation related to the mode mix. Unlike in homogeneous materials, transverse crack extension is accompanied by planar delamination advance, and transverse crack rotation during extension is restricted by the laminate’s fibers. The overall fracture surface evolution is therefore strongly controlled by specimen geometry. The influence of these findings on the apparent delamination toughness as obtained from composite split beam and other types of mode III tests is discussed.     

Green synthesis of polyaniline/clay/iron ternary nanocomposite by the one step solid state intercalation method

The incorporation of two or more active components into clay layered structure with uniform distribution is expected to facilitate wider applications of the material. In this study, nanocomposite composed of clay, polyaniline and iron nanoparticles was synthesized by a facile and environmentally friendly strategy for the first time. Local smectite clay from Tunisia was exchanged with Fe³⁺ then it was subjected to fine grinding with anilinium chloride using mortar grinder and the mixture has been allowed for ageing at ambient air until the change of color to dark green. Both interlayer Fe³⁺ cations and atmospheric oxygen act as oxidant for aniline polymerization. In addition, the presence of interlayer Fe³⁺ and Fe²⁺ cations (the result of the reduction of Fe³⁺) at the same time favors the formation of iron nanoparticles phase. Electrical and dielectric properties have studied using spectroscopy impedance. The ac conduction shows a regime of constant dc conductivity at low frequencies and a crossover to a frequency-dependent regime of the type Aω^S at high frequencies. The material shows high dielectric constant, resulting from the presence of iron nanoparticles, indicating its improved ability to store electric energy and to be used as capacitor.     

砷铁渣中砷酸铁的热力学分析及热分解试验

利用铁盐法处理某铅冶炼工业含砷废水,得到砷质量分数为10%的砷铁渣,物相分析表明砷与铁在渣中以砷酸铁的形态存在。据热力学分析,砷酸铁化合物在1600℃以下不会热分解,表明其热力学性质稳定;而在有添加剂碳的情况下,砷酸铁的热分解温度大大降低。试验结果表明:在1200℃条件下,静态焙烧5h,砷酸铁砷的挥发率在90%以上,铁富集10%以上。     

A novel synthesis method for manganese ferrite nanopowders: The effect of manganese salt as inorganic additive in electrosynthesis cell

Manganese ferrite nanoparticles were electro-crystallized in an electrochemical cell containing two iron electrodes, and an electrolyte solution of sodium sulfate, sodium butanoate, and manganese sulfate hydrate. The samples were characterized by X-ray diffraction, electron microscopy, magnetometry, and Mössbauer spectroscopy methods. The crystal structure of the samples was studied using X-ray diffraction. Based on obtained results we found that the manganese ferrite nanoparticles are formed in the electrochemical cell containing 0.001 M manganese sulfate hydrate. Also, the formation of a paramagnetic secondary phase in the sample without manganese is suppressed by adding manganese salt in the electrochemical cell. The nanoparticle size, shape, and morphology were characterized using electron microscopy. Magnetization curves show that all samples are magnetically soft and their specific magnetization ranges from 15 A m² kg⁻¹ to 75 A m² kg⁻¹, depending on the growth conditions. Room temperature Mössbauer spectra confirm the formation of nonstoichiometric spinel ferrite of magnetite or manganese ferrite, again depending on the growth conditions. Based on Mössbauer analysis, reduction in the population of octahedral sites provides direct evidence for the presence of the manganese ions substitution in the octahedral sites.     

Voids and their effect on the strain rate dependent material properties and fatigue behaviour of non-crimp fabric composites materials

The manufacture of composite structures is inevitably linked to the formation of voids. Several non-destructive techniques are potentially able of detecting defects, but just the exact knowledge of the effects of defects on the mechanical properties allows the definition of thresholds for the purpose of quality management. In this paper an experimental program for characterizing the effect of voids on the composite materials behaviour is presented. Therefore glass fibre non-crimp fabric reinforced epoxy composites were produced using vacuum assistant resin transfer moulding. For obtaining various void contents specially modified process parameters were used. Nominally defect free specimens are compared with flawed specimens. Tensile testing at different loading speeds and fatigue tests in tension-compression loading are performed.