A new efficient method for one‐pot conversions of aryl carboxylic acids into nitriles without solvent

A new efficient method for synthesising nitriles, important organic reagents, is reported in this paper. In an environmentally benign solvent‐free system, aryl carboxylic acids were converted into the corresponding nitriles via one‐pot reactions, by amidation with ethyl carbamate followed by dehydration with thionyl chloride, in excellent yields. The results showed that the method has the advantages of lower cost, higher yield, less pollution and greater ease of work‐up. Copyright © 2008 Society of Chemical Industry     

Synthesis,characterization and ion exchange properties of zirconium(IV) tungstoiodophosphate,a new cation exchanger

Zirconium(IV) tungstoiodophosphate has been synthesized under a variety of conditions. The most chemically and thermally stable sample is prepared by adding a mixture of aqueous solutions of 0·5 mol L⁻¹ sodium tungstate, potassium iodate and 1 mol L⁻¹ orthophosphoric acid to aqueous solution of 0·1 mol L⁻¹ zirconium(IV) oxychloride. Its ion exchange capacity for Na⁺ and K⁺ was found to be 2·20 and 2·35 meq g⁻¹ dry exchanger, respectively. The material has been characterized on the basis of chemical composition, pH titration, Fourier transform infrared spectroscopy (FTIR) and thermogravimetric analysis. The effect on the exchange capacity of drying the exchanger at different temperatures has been studied. The analytical importance of the material has been established by quantitative separation of Pb²⁺ from other metal ions.     

A One-Dimensional Nonlocal Damage-Plasticity Model for Ductile Materials

This paper presents a new 1-D non-local damage-plasticity deformation model for ductile materials. It uses the thermodynamic framework described in Houlsby and Puzrin (2000) and holds, nevertheless, some similarities with Lemaitre’s (1971) approach. A 1D finite element (FE) model of a bar fixed at one end and loaded in tension at the other end is introduced. This simple model demonstrates how the approach can be implemented within the finite element framework, and that it is capable of capturing both the pre-peak hardening and post-peak softening (generally responsible for models instability) due to damage-induced stiffness and strength reduction characteristic of ductile materials. It is also shown that the approach has further advantages of achieving some degree of mesh independence, and of being able to capture deformation size effects. Finally, it is illustrated how the model permits the calculation of essential work of rupture (EWR), i.e. the specific energy per unit cross-sectional area that is needed to cause tensile failure of a specimen.     

Effects of contact shape on biological wet adhesion

Wet adhesion is widely adopted in biological adhesion systems in nature. Wet adhesion is studied in this paper with the focus on the effect of different contact shapes (flat, concave, convex, and ring-like) on the adhesion force. The evolution of the liquid bridge between a fiber tip and substrate during the detaching process shows two transition points. The first transition from the radius-controlled to the contact-angle controlled process is critical to influence the strength and robustness of adhesion. We show that a concave shape is more effective than a flat one, while a convex shape has no advantage. A ring-like contact shape has advantages in a hydrophobic environment and on a rough surface.     

Dye-sensitized solar cell based on nanocrystalline TiO<Subscript>2</Subscript> with 3–10 nm in diameter

Nanocrystalline TiO₂ with 3–10 nm in diameter was prepared with a surfactant-template method. Dye-sensitized solar cells were assembled using the prepared nanocrystalline TiO₂ with large surface area and high crystallinity, which achieved significant higher Jsc when compared to cells fabricated with bigger particles of 25 nm in diameter. In the cells with nanocrystalline TiO₂, the sintering temperature drastically affected the conversion performance of the cells.     

Dielectric behavior of Cu–GeO<Subscript>2</Subscript> cermet thin films

Capacitance and dielectric loss measurements were carried out using an Al/Cu–GeO₂/Al sandwich structure for 0 to 10 vol% Cu films, 120–400 nm thick, deposited at 0.4–1.5 nm/s in the frequency and temperature range 1–10⁶ Hz and 90–573 K, respectively. The variation of capacitance and dielectric loss with frequency and temperature follows the Goswami and Goswami model. Capacitance decreases slowly with increasing thickness and also varies with the change in deposition rate of the cermet film.     

Efficient and stable field emission from the oxidized porous polysilicon using Pt/Ti multilayer electrode

The field emission characteristics of an oxidized porous polysilicon (OPPS) were investigated with a Pt/Ti multilayer electrode, which showed highly efficient and stable electron emission characteristics compared with those of conventional Au/NiCr electrodes. The thin Ti layer played an important role in promoting the adhesion of Pt to SiO₂ surface and the distribution of the electric field on the OPPS surface. Additionally, the Ti layer efficiently blocked the diffusion of emitter metal, which resulted in more reliable emission characteristics.     

Identification of microstructural zones and thermal cycles in a weldment of modified 9Cr-1Mo steel

This paper presents the results of a study on the microstructural and microchemical variations in a multipass Gas Tungsten Arc weld (GTAW) of modified 9Cr-1Mo steel. The changes brought about in the steel due to the heating and cooling cycles during welding and the subsequent effects due to reheating effects during multipass welding are described. Detailed analytical transmission electron microscopy has been carried to study the type and composition of the primary and secondary phases in this steel. The systematic changes in microstructural parameters such as Prior Austenite Grain Size, martensite lath size, number density, size and microchemistry of carbides, have been understood based on the different transformations that the steel undergoes during the heating and cooling process. Based on the observed microstructure, an attempt has been made to identify distinct microstructural zones and possible thermal cycles experienced by different regions of the weldment.     

Effect of preparation technique on the properties of Mo-containing Al-MCM-41

The Al-MCM-41 has been used as support to prepare Mo-containing catalysts. The 12- molybdophosphoric heteropoly acid (HPMo) is used as initial compound. The catalysts are synthesized by two different methods: incipient impregnation with aqueous solution of the acid and mechanochemical synthesis. The samples were tested in the reaction of the thiophene hydrodesulfurization after activation with mixture H₂ + H₂S. The effect of the preparation method of the catalysts on their physicochemical and catalytic properties has been studied. A partial destruction of the loaded compound is observed in mechanochemically treated sample whereas the aggregates are formed from the particles of different size in the impregnated sample. The specific surface area of the sample prepared by mechanical–chemical treatment decreases 2–3 times, while the total pore volume is about four times lower. The HDS activity is higher on the impregnated sample than on the mechanochemically treated one.     

Improved visible-light responsive photocatalytic activity of N and Si co-doped titanias

Thermal reaction of titanium tetraisopropoxide and tetraethyl orthosilicate in 1,4-butanediol afforded nanocrystalline silica-modified titanias having large surface area and superior thermal stability. In this study, the thus-obtained silica-modified titanias were treated in an NH₃ flow at high temperatures, and their physical and photocatalytic properties were investigated. Compared with NH₃-treated TiO₂ without silica modification, the NH₃-treated silica-modified titanias showed a stronger absorption in the visible region (400–500 nm) and had a larger peak at 396 eV in the N 1s XPS spectrum. These results indicate that a larger amount of nitrogen was stably doped in the silica-modified titania. The obtained products exhibited a high photocatalytic activity for degradation of Rhodamine B and decomposition of acetaldehyde under visible light irradiation. Electronic supplementary material The online version of this article (doi:) contains supplementary material, which is available to authorized users.