A novel low-clay translucent whiteware based on anorthite

This study was carried out to characterize the properties of a novel low-clay translucent whiteware suitable for daily use. The low-clay whiteware is produced from coarsely and finely milled prefired materials of the same composition plus a small amount of clay. It consists of anorthite (CaO·Al₂O₃·2SiO₂) and mullite (3Al₂O₃·2SiO₂) crystalline phases and a glassy phase with high crystalline to glassy phase ratio. The development of needle shaped long mullite crystals that were forming three dimensional interlocking network had significant effect on the elimination of pyroplastic deformation during glaze firing. Typical flexural strength and fracture toughness values were ∼110 MPa and ∼1.85 MPam^1/2, respectively. The low-clay whiteware had relatively low (4.6 × 10⁻⁶/°C) thermal expansion coefficient which made possible to glaze the whiteware with a typical hard porcelain glaze. A continuous interface layer was produced between the whiteware and the glaze and no crack was present through layer because of expansion mismatch.     

Electrochemical preparation and characterization of nickel and zinc-modified poly-2-aminothiazole films on mild steel surface and their corrosion inhibition performance

Poly-2-aminothiazole (pAT) was electrochemically synthesized on a mild steel (MS) specimen from 0.3 M aqueous ammonium oxalate solution containing 0.01 M 2-aminothiazole (2-AT) using cyclic voltammetry technique. The synthesized polymer film was then modified by electrodeposition of 100 μg cm⁻² Ni (MS/pAT–Ni) and Zn (MS/pAT–Zn) on top of the polymer surface. The surface morphologies of the polymer films were examined by scanning electron microscopy (SEM) and atomic force microscopy (AFM). The elemental analysis of the surface films was performed by energy dispersive X-ray spectroscopy (EDX). The effectiveness of the coatings in preventing corrosion of MS in 3.5% NaCl solution was assessed using electrochemical techniques. It was found that the obtained coatings were adherent to the steel surface. The pAT film provided a good corrosion protection against the attack of corrosive environment. Moreover, the modification of pAT film by deposition of Ni and Zn on top of the polymer surface significantly enhances the corrosion protection performance of the polymer film by exhibiting an improved barrier effect against the attack of corrosive environment. The surface morphologies and protection ability of the layers were found to be dependent on the type of deposited metal.     

Spectrophotometric and electrochemical behavior of a novel azocalix[4]arene derivative as a highly selective chromogenic chemosensor for Cr

In this study, a novel azocalix[4]arene derivative, 5,11,17-tris[(1-naphtyl)azo]-25,26,27,28-tetrahydroxy-calix[4]arene (NAC4) bearing napthyl groups on the upper rim was synthesized. Its complexation behavior for alkali, alkaline-earth and various heavy metal ions (Li⁺, Na⁺, K⁺, Rb⁺, Cs⁺, Mg²⁺, Ca²⁺, Sr²⁺, Ba²⁺, Pb²⁺, Hg²⁺, Ni²⁺, Cd²⁺, Cu²⁺, Zn²⁺, Co²⁺, Fe²⁺, Cr³⁺, Ag⁺) was investigated by spectroscopic and voltammetric methods. This chemosensor exhibits decreased absorbance in the presence of Hg²⁺ and a unique absorbance quenching effect only for Cr³⁺. In addition, a new absorption band centered at 565 nm with the formation of the 1:1 host–guest complex (Cr³⁺-NAC4) was observed in the case of Cr³⁺, leading to an obvious color change from light orange to dark lilac. In voltammetric experiments, Cr³⁺ ions decreased voltammetric peaks of NAC4, whereas no significant changes occurred in the presence of the other metal ions. The Benesi–Hildebrand method was used to determine a logarithmic value of 3.76 for the association constant of the complex between Cr³⁺ and NAC4.     

Metallo‐supramolecular materials based on terpyridine‐functionalized polyhedral silsesquioxane

In this study, novel metallo‐supramolecular materials based on terpyridine‐functionalized polyhedral silsesquioxane were synthesized from 4′‐chloro‐2,2′:6′,2″‐terpyridine and amino‐group‐functionalized polyhedral oligomeric silsesquioxane. The obtained terpyridine‐functionalized polyhedral silsesquioxanes were converted to metallo‐supramolecular hybrid materials by coordination polycondensation reaction with Co(II) or Cu(II) ions. The supramolecular polymers created were characterized by means of structure, morphology and stimuli‐responsive performance employing scanning electron microscopy, amperometric techniques and UV–visible and Fourier transform IR spectroscopy. UV?visible and cyclic voltammetry studies showed that both the optical and electrochemical properties of metallo‐supramolecular materials are affected by the substituent at the pyridine periphery. The supramolecular polymers obtained exhibited electrochromism during the oxidation processes of cyclic voltammogram studies. As a result, these terpyridine‐functionalized polyhedral silsesquioxanes are good candidates for electronic, opto‐electronic and photovoltaic applications as smart stimuli‐responsive materials. © 2013 Society of Chemical Industry     

The synthesis,characterisation and molecular structure of a new hetarylazoindole dye studied by X‐ray diffraction,spectral analysis and density functional theory calculation

1,2‐Dimethyl‐3‐(5‐methylisoxazol‐3‐yldiazenyl)‐1H‐indole was obtained by coupling 3‐amino‐5‐methylisoxazole with diazotised 1,2‐dimethylindole. It was characterised by proton and carbon nuclear magentic resonance, ultraviolet–visible, infrared and Raman spectra, and the X‐ray single crystal diffraction method. On the theoretical side, the molecular geometry, chemical shifts and the fundamental vibrational frequencies were evaluated using density functional theory. Time‐dependent density functional theory was used to evaluate the electronic excitation spectra. In addition, the scaled quantum mechanical approach was used to study the total energy distributions of the vibrational modes of the molecule. The results showed that the general agreement between experimental and calculated geometric parameters, chemical shifts and λ_max values are good. Excellent agreement was found between the calculated and experimental vibrational frequencies.     

Polymerization of epoxides catalyzed by a mixed‐valent iron trifluoroacetate [Fe3O(O2CCF3)6(H2O)3]

The readily available mixed‐valent iron trifluoroacetate complex [Fe₂^IIIFe^II(µ₃‐O)(O₂CCF₃)₆(H₂O)₃] is an effective catalyst for the polymerization of epoxides. A very small amount of the catalyst (1.0–0.01 mol%) could initiate the polymerization of cyclohexene oxide, cyclopentene oxide and epichlorohydrin. Based on quantitative end‐group analysis by ¹⁹F NMR spectroscopy, a Lewis acid (LA^⊕) catalyzed anionic reaction mechanism is proposed. Copyright © 2012 Society of Chemical Industry     

Preparation of Gadolina Stabilized Bismuth Oxide Doped with Boron via Electrospinning Technique

In this study, boron doped and undoped poly (vinyl) alcohol/bismuth–gadolina acetate (PVA/Bi–Gd) nanofibers were prepared using electrospinning technique then calcinated at 800 °C for 2 h. The originality of this study is the addition of boron to metal acetates. The effects of boron doping were investigated in terms of solution properties, morphological changes and thermal characteristics. The characteristics of the fibers were investigated with FT-IR, XRD, SEM and BET. The addition of boron did not only increase the thermal stability of the fibers, but also their diameters, which yielded stronger fibers. XRD analyses showed that boron doping increased the peak intensities and indicated that the boron doping enhanced the crystallite size. Moreover, no shifts were noticed in diffraction angles for boron doped and undoped samples. Therefore, boron doping did not significantly alter the lattice spacing. The SEM micrograph of the fibers showed that the addition of boron resulted in the formation of cross-linked bright-surfaced fibers. The average fiber diameter for boron doped and undoped fiber mats were 204 and 123 nm, respectively. Also, grain diameters of boron doped and undoped nanocrystalline sintered powders were measured as 140 and 118 nm, respectively. The BET results showed that boron undoped and doped Bi₂O₃–La₂O₃ nanocrystalline powder ceramic structures sintered at 800 °C have surface areas of 59.72 and 39.80 m²/g, respectively.     

Lipase-Catalyzed Acidolysis of Olive Oil with Echium Oil Stearidonic Acid: Optimization by Response Surface Methodology

In this study, our aim was to enrich olive oil with stearidonic acid (SDA) together with polyunsaturated fatty acids (PUFA) by lipase-catalyzed acidolysis using olive oil (OO) and free fatty acids of Echium oil, in the presence of Lipozyme^? TL IM. The reaction conditions were optimized by using response surface methodology. A three-factor, five level central composite circumscribed designs was used to generate the design points. The factors chosen were: substrate molar ratio (S _r, 4–6?mol/mol), reaction temperature (T, 55–65?°C), and reaction time (t, 6–9?h). Targeted incorporation (5?%) of SDA into OO was achieved at substrate molar ratio of 6?mol/mol, 55?°C, and 8.4?h. Model verification performed under these conditions for mg- and g-scale production yielded SDA contents of 4.9 and 4.8?%, respectively. Moreover, it was observed that the structured lipid (SL) obtained under optimum conditions contained approximately 42?% oleic acid and 43?% PUFA including linoleic acid, α-linolenic acid, and γ-linolenic acid. Omega-6/omega-3 fatty acid ratio of SLs was 0.7. Analysis of oxidative properties resulted in lower oxidative stability of SL than unmodified OO. This type of SL containing SDA and other PUFA is believed to be beneficial for human health.     

In vacuo production of α-AlB12, C4AlB24, AlB12C2 and Al3B48C2 powders

The production of pure powder samples of boron-rich ternary Al–B–C phases was investigated in vacuum at temperatures between 1400 °C and 1600 °C, using a range of different starting powders. Compacted powder mixes of B–AlB₂–B₄C, Al–B–C, Al–B–B₄C, B–C–AlB₂, B–AlB₂ and Al–B were heated for 1–2 h under vacuum in a carbon resistance furnace and the products characterised by X-ray diffraction. It was found impossible to produce significant quantities of C₄AlB₂₄ under these conditions, but >95% pure samples of α-AlB₁₂, AlB₁₂C₂ and Al₃B₄₈C₂ were obtained. This study is a precursor to further research aimed at producing dense B₄C-type materials which might offer the advantages of easier densification and fabrication as compared with B₄C itself.     

Thermal energy storage by poly(styrene-co-p-stearoylstyrene) copolymers produced by the modification of polystyrene

A series of poly(styrene-co-p-stearoyl styrene) copolymers as novel polymeric solid–solid phase-change materials (SSPCMs) were synthesized by the modification of polystyrene with stearoyl chloride. The chemical structure and crystalline morphology of the synthesized copolymers were determined with Fourier transform infrared spectroscopy and polarized optical microscopy, respectively. The thermal energy storage properties and thermal stability of the SSPCMs were investigated with differential scanning calorimetry and thermogravimetric analysis, respectively. In addition, the thermal conductivity of the SSPCMs was measured with a thermal property analyzer. Moreover, thermal cycling tests showed that the copolymers had good thermal reliability and chemical stability after being subjected to 5000 heating/cooling cycles. The synthesized poly(styrene-co-stearoyl styrene) copolymers as novel SSPCMs have considerable potential for thermal energy storage and temperature-control applications. © 2012 Wiley Periodicals, Inc. J Appl Polym Sci, 2012