Blends of polyamide 6 and epichlorohydrin elastomers. I. Graft copolymerization in the melt blending

With the purpose of improving the mechanical properties of the polyamides, the possibility of combining polyamides with elastomers has been used. The low compatibility of the resulting blends leads to deficient mechanical properties, and therefore, it is necessary to add the compatibilizer to the mixture or to produce the compatibilizer during the melting mixture. Usually, at least one of the components must contain a reactive functional groups. In the present work, blends of polyamide 6 (PA 6) and epichlorohydrin elastomers, polyepichlorohydrin (PEPI), and the equimolar copolymer poly(epichlorohydrin‐co‐ethylene oxide), ECO, with different compositions were prepared by mechanical mixture using a Banbury‐type mixer. The blends were characterized by rheological measurements, the Molau test, elemental analysis, Infrared Spectroscopy by Diffuse Reflectance, Transmission Electron Microscopy, and X‐ray Diffractometry. The blends of PA 6 with PEPI and ECO are heterogeneous, showing a morphology of elastomer particles dispersed in the polyamide matrix. The results of rheological measurements and the Molau test indicate a graft copolymerization in the interface between the polyamide and the elastomer, PA 6‐g‐elastomer, whose concentration decreases with the elastomer content. It was found that the grafting of PEPI and PA 6 changed the diffraction pattern of PA 6. © 1999 John Wiley & Sons, Inc. J Appl Polym Sci 72: 1827–1833, 1999     

Corrosion of reinforcing steel in neutral and acid solutions simulating the electrolytic environments in the micropores of concrete in the propagation period

Steel embedded in concrete passivates due to the alkaline nature of the concrete pore solution. Reinforcement corrosion develops when the alkalinity is neutralized. Corrosion, in turn, induces acidification of the surrounding pore solution. In the present paper, corrosion rate of corrugated steel bars is studied and measured at different pH values in solutions simulating chloride environments. The media considered consists of saturated calcium hydroxide solutions containing Na and K⁺, neutralized with ferrous chloride. This latter substance is the soluble compound produced during the corrosion of steel after chloride attack. Hydrochloric acid solutions of different pHs were prepared in order to compare the steel corrosion rates in these solutions with those observed in ferrous chloride solutions of the same pH. A comparison of polarization resistance measurements (R_p) with gravimetrically weight loss determined is presented. Tafel slopes results are also included. Additionally, a comparison is made between measurements of AC impedance with those of the R_p method. The results indicate that the corrosion rate in the studied media follows the general trend found in other media of similar pH values: corrosion increases in acidic solutions, remains rather stable for pH range 3-11 and decreases significantly in highly alkaline solutions.     

Structural analysis and optimisation of press brakes

A model of the bending process in Press Brakes is established using Timoshenko beam theory. Expressions for the workpiece bending error are derived that explicitly consider the influence of shape, dimensions and initial deformation of the machine structural components on its bending accuracy. The minimization of the bending error is formulated in terms of optimisation problems that are solved numerically using a genetic algorithm. The methodology presented in this paper permits the analysis of existing Press Brake design solutions, the optimisation of their performance and the development of new solutions.     

Sulfolobus solfataricus protein disulphide oxidoreductase: insight into the roles of its redox sites

Sulfolobus solfataricus protein disulphide oxidoreductase (SsPDO)contains three disulphide bridges linking residues C⁴¹XXC⁴⁴,C¹⁵⁵XXC¹⁵⁸, C¹⁷³XXXXC¹⁷⁸. To get information on the role playedby these cross-links in determining the structural and functionalproperties of the protein, we performed site-directed mutagenesison Cys residues and investigated the changes in folding, stabilityand functional features of the mutants and analysed the resultswith computational analysis. The reductase activity of SsPDOand its mutants was evaluated by insulin and thioredoxin reductaseassays also coupled with peroxiredoxin Bcp1 of S. solfataricus.The three-dimensional model of SsPDO was constructed and correlatedwith circular dichroism data and functional results. Biochemicalanalysis indicated a key function for the redox site constitutedby Cys155 and Cys158. To discriminate between the role of thetwo cysteine residues, each cysteine was mutagenised and thebehaviour of the single mutants was investigated elucidatingthe basis of the electron-shuffling mechanism for SsPDO. Finally,cysteine pK values were calculated and the accessible surfacefor the cysteine side chains in the reduced form was measured,showing higher reactivity and solvent exposure for Cys155.     

Friction stir welding of duplex stainless steels

Duplex stainless steels are successful in a variety of applications such as the food industry, petrochemicals and plants for desalination of seawater, where high corrosion resistance and high mechanical strength are required. However, the beneficial microstructure may change during fusion welding steps, and it can compromise the performance of these materials. Friction stir welding is a solid-state process avoiding typical problems concerning solidification such as solidification cracks, liquation and segregation of alloying elements. Superduplex stainless steels can avoid unbalanced proportions of ferrite and austenite, formation of secondary deleterious phases and grain growth of ferrite in the heat-affected zone. Consolidated friction stir welded joints with full penetration 6 mm thick were obtained for UNS S32101 and S32205 duplex and S32750 and S32760 superduplex stainless steels. The friction stir welds were submitted to tensile tests indicating an improvement of strength in welded joints, showing increased yield and tensile strength for all studied cases. Regarding the microstructural characterization, an outstanding grain refinement was observed in the welded joint, achieving grain sizes as small as 1 μm. This refinement was associated with the combination of microstructural restoration mechanisms in the dual-phase microstructure promoted by severe deformation associated with a high temperature during the welding process.     

Characterization of Mechanical Properties and Residual Stress in API 5L X80 Steel Welded Joints

The use of high-strength and low-alloy steels, high design factors and increasingly stringent safety requirements have increased the operating pressure levels and, consequently, the need for further studies to avoid and prevent premature pipe failure. To evaluate the possibility of improving productivity in manual arc welding of this type of steel, this work characterizes the mechanical properties and residual stresses in API 5L X80 steel welded joints using the SMAW and FCAW processes. The residual stresses were analyzed using x-ray diffraction with the sin² ψ method at the top and root of the welded joints in the longitudinal and transverse directions of the weld bead. The mechanical properties of the welded joints by both processes were characterized in terms of tensile strength, impact toughness and Vickers microhardness in the welded and shot peening conditions. A predominantly compressive residual stress was found, and shot peening increased the tensile strength and impact toughness in both welded joints.     

Condensation of alkoxysilanes in alcoholic media: II. Oligomerization of aminopropylmethyldiethoxysilane and co‐oligomerization with dimethyldiethoxysilane

In the context of the preservation of cultural heritage, the treatment of paper by an aminoalkylalkoxysilane, or its mixture with dimethyldiethoxysilane (DMDES), gave encouraging results. The condensation experiments presented here, carried out in alcohol medium using aminopropylmethyldiethoxysilane (AMDES) alone or with DMDES, were followed using ¹H NMR, ²⁹Si NMR and matrix‐assisted laser desorption ionization time‐of‐flight (MALDI TOF) spectroscopies. The aim was to determine whether DMDES and AMDES could copolymerize under the conditions used. An exchange reaction was observed for AMDES in ethanol in the absence of water, under conditions where no exchange took place for DMDES. In methanol, this reaction proceeded much more rapidly and the reactivity of methoxysilyl groups was higher than that of ethoxysilyl groups. In the same solvent, in the presence of water, hydrolysis, cyclization and oligomerization were observed using NMR and MALDI TOF spectroscopies. In ethanol, a kinetic study of a mixture of DMDES and AMDES showed that the condensation of the two monomers proceeded at comparables rates and MALDI‐TOF analysis gave evidence that mixed oligomers were produced, containing from one to four AMDES units. It was concluded that the co‐oligomerization did not lead to a mixture of homo‐oligomers, which would be due to different hydrolysis and condensation kinetics, but induced the formation of co‐oligomers. Copyright © 2010 Society of Chemical Industry     

A cathodoluminescence study of boron doped {111}-homoepitaxial diamond films

In this work we use cathodoluminescence (CL) at liquid helium temperature to investigate the boron incorporation in {111}-homoepitaxial diamond films, grown outside the visible plasma ball by the Microwave plasma-assisted chemical vapor deposition (MPCVD) technique. The boron concentration of this set of films covers the whole possible doping range divided into four parts: Low doping (5 × 10¹⁶ < [B] < 1.5 × 10¹⁹ cm^? 3), high doping (1.5 × 10¹⁹ < [B] < 3 × 10²⁰ cm^? 3), heavy doping (3 × 10²⁰ < [B] < 2 × 10²¹ cm^? 3), and phase separation range ([B] > 2 × 10²¹ cm^? 3). The phase separation occurs for very high boron concentrations, between the diamond phase (sp³ carbon) and the other components of the layer, namely sp² carbon and boron. A part of them is accumulated outside the diamond lattice.This detailed cathodoluminescence investigation of {111}-homoepitaxial diamond films has led to determining the doping range of the films and following the evolution of their crystalline quality when the boron concentration increases. In addition, a comparison between {111} and {100} films in the same doping ranges has been undertaken.     

Hydrogen passivation of boron acceptors in as-grown boron-doped CVD diamond epilayers

A homoepitaxial boron-doped diamond single layer is investigated by means of Fourier transformed infrared spectroscopy (FTIR) and cathodoluminescence (CL). Both techniques are shown to be complementary. µ-FTIR mapping allows to determine the location of active boron while CL allows discernability between passivation and compensation. Hydrogen incorporation during chemical vapour deposition (CVD) growth is revealed to passivate boron acceptors. The obtained results highlight that plasma etching can induce a dissociation of B–H centres.