Characteristics of wet‐spun and thermally treated poly acrylonitrile fibers

The performance of carbon fibers depends on the quality of the precursor and the conditions of the thermal treatment. In detail, for a PAN precursor fiber the viscosity of a spinning dope and the draw ratio during the spinning process needs to be considered. Through wet spinning, different types of PAN precursor fibers with defined spinning parameters, including solid content, solvent content in a bath, and especially draw ratio resulting in defined cross section diameters, were fabricated and analyzed with tensile tests, density investigations, SEM, TGA‐MS, FTIR, and XRD. The results show that the mechanical properties of the fibers correlate to crystallinity. The cross section diameter is strongly related to the morphology of the fibers after thermal treatment. By extending the postdrawing of PAN fibers high tenacities were obtained at the cost of the cross section shape. In addition, TGA measurements reveal trapped residues of the wet spinning process as well as show several chemical reactions takes place at the same time at different temperatures. © 2016 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2016 , 133, 43698.     

Synthesis and characterization of electrically conducting copolymer of aniline and o‐bromoaniline using methane sulfonic acid as dopant

Polyaniline (PAN), poly(o‐bromoaniline) (POBA), and poly(aniline‐co‐o‐bromoaniline) (PABA) were synthesized by oxidative coupling. These polymers are protonated by 10–20% methane sulfonic acid (MSA) and 1M HCl. The new polymer bases have greater solubility than that of PAN in common polar organic solvents; PAN–MSA was observed to be the most thermally stable of these polymers. POBA is associated with residual quinoid diimine units as illustrated in the IR and UV‐vis spectra, after reduction with hydrazine dihydrochloride. Both the doping agents cause a downward shift of the quinoid absorption in the IR spectra. MSA‐ and HCl‐doped PAN and PABA polymers exhibit a coil‐like conformation in DMSO, whereas only MSA‐doped PAN and PABA show an “expanded coil‐like” conformation in m‐cresol with a “free carrier tail” above 800 nm in their electronic spectra. XPS spectra indicated the presence of covalent bromine in the POBA and PABA polymers. Bromine retention was greater in the homopolymer as evidenced by the IR studies after aging at 350°C. Compared to HCl, MSA is found to be a more effective dopant, enhancing the conductivity of the copolymers by 10²–10³ times in magnitude. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 86: 2662–2669, 2002     

Preparation and Use of a Boron Nitride Precursor as Binder for the Densification of Boron Nitride

A precursor of boron nitride was prepared through the partial condensation of 2,4,6-trichloroborazine and bis-(trimethylsilyl)acetylene. This reaction was conducted at 100°C and is catalyzed by AlCl₃. The condensation product pyrolyzed at 800°C, producing trimethylsilyl chloride as a volatile product and a boron nitride rich residue containing 54 wt% of the initial weight. Mixtures of the precursor and commercial boron nitride were made and hot-pressed at 800°C and 27.6 MPa. A maximum density of 1.84 g/cm³ is reached at a loading corresponding to the deposition of 13 wt% residue derived from the precursor. Examination by analytical electron microscopy, including X-ray energy dispersive spectroscopy and electron energy loss spectroscopy analyses, revealed the location of material derived from the precursor in BN-binder composites through the presence of residual aluminum, silicon, and carbon. Crystallization of boron nitride from the precursor appears to have taken place, as deduced from the morphology of the phases observed and association with residual elements present in the binder.     

Effect of heat treatment and milling on the seed, flour, rheology and baking quality of some amaranth ecotypes

Forty-five harvests corresponding to the two predominating domestic species of amaranth in Mexico were studied. The proximate analysis revealed some statistically significant differences throughout three years of observation. The Ca, P and Fe content did not vary greatly in 15 samples. No chemical differences were either manifested in the Mercado and Aztec types of A. hypochondriacus, nor in the Mexican type of A. cruentus. The latter exhibits a higher grain yield and a shorter life cycle; however, its baking quality is apparently inferior to that of the Mercado type of A. hypochondriacus. The heat treatment of the seeds (toasting, popping and cooking) affected protein and lysine contents as does in cereals and leguminous seeds although toasting in particular improves its sensory characteristics without altering digestibility and PER. Popping only improves PER. Heating at 90 or 170 degrees C for three to five minutes, at the usual seed's moisture rate of 6 to 15%, does not affect protein content and does so only slightly in the case of the fatty acids content. Amylographic and farinographic values of the starchy fractions indicate similarities to C. quinoa and differences with respect to wheat. In the case of "amaranth milk", viscosity and gelatinization temperature produced satisfactory values. The extension of amaranth cultivation in the country is hereby suggested in view of the seed's nutritional quality, and considering the behavior of whole amaranth flour and its fractions.     

Effective elastic properties and residual stresses in directionally solidified eutectic Al<Subscript>2</Subscript>O<Subscript>3</Subscript>/YAG/ZrO<Subscript>2</Subscript> ceramics estimated by finite element analysis

Effective elastic properties and residual stresses were assessed in directionally solidified ternary eutectic ceramic, Al₂O₃/YAG/ZrO₂, by finite element analyses. A 3D finite element model was generated from a CT scan, representative of the microstructure and with a similar volume fraction. Effective elastic properties were calculated by numerical homogenisation. They highlight a quasi-isotropic behaviour of the ternary eutectic ceramics. Despite the difficulties to measure the strain, the dispersion observed in the results and the limited reliability of the materials properties, the results constitute a step towards a better understanding of the material behaviour. Thermal residual stresses induced by the manufacturing were also evaluated. Tensile residual stresses in yttria-stabilised zirconia and compressive residual stresses in YAG and alumina were highlighted. This evaluation also shed light on the influence of the phase morphology in the microstructure. Indeed, the computed spatial distribution of the residual stresses showed that they are different from one position to another due to the variation in phase morphology and also to material properties variability. Therefore, it is important when numerically assessing the thermomechanical properties to take into account the microstructure morphology as well as the variability of material properties.     

Study of a proton exchange membrane fuel cells catalyst subjected to anodic operating conditions, by synchrotron-based scanning photoelectron microscopy (SPEM) and high lateral-resolution X-ray photoelectron spectroscopy

In this paper we report an investigation of the degradation of the Pt/C electrocatalyst of an anodic membrane-electrode assembly (MEA) after 1000 h of operation in a laboratory single-cell PEMFC, using synchrotron-based space-resolved photoelectron spectroscopy. This study is complemented by the analysis of a pristine MEA and reference materials, as well as by electrochemical measurements, SEM imaging and energy-dispersive X-ray fluorescence spectroscopy (EDX). Catalyst ageing correlates with a corrugation of morphology, as observed by SEM and scanning photoelectron microscopy (SPEM), corresponding to Pt nanoparticle agglomeration. Moreover - on the basis of high lateral resolution SPEM, X-ray photoelectron spectroscopy (XPS) and EDX analyses, - we found that, after operation, Pt is transported onto the fibres of the gas-diffusion layer (GDL). Space-resolved XPS shows a peak shift of the Pt 4f_7/2 level to higher and lower binding energies with respect to Pt(1 1 1) and pristine Pt black, respectively, corresponding to nanocrystallinity in the first case and agglomeration in the second one. No oxidised Pt was found in any location of the anodically used MEA.     

Thermoplastic Composites Reinforced with Textile Grids: Development of a Manufacturing Chain and Experimental Characterisation

A significant improvement in the properties of plastic components can be achieved by introducing flexible multiaxial textile grids as reinforcement. This reinforcing concept is based on the layerwise bonding of biaxially or multiaxially oriented, completely stretched filaments of high-performance fibers, e.g. glass or carbon, and thermoplastic components, using modified warp knitting techniques. Such pre-consolidated grid-like textiles are particularly suitable for use in injection moulding, since the grid geometry is very robust with respect to flow pressure and temperature on the one hand and possesses an adjustable spacing to enable a complete filling of the mould cavity on the other hand. The development of pre-consolidated textile grids and their further processing into composites form the basis for providing tailored parts with a large number of additional integrated functions like fibrous sensors or electroconductive fibres. Composites reinforced in that way allow new product groups for promising lightweight structures to be opened up in future. The article describes the manufacturing process of this new composite class and their variability regarding reinforcement and function integration. An experimentally based study of the mechanical properties is performed. For this purpose, quasi-static and highly dynamic tensile tests have been carried out as well as impact penetration experiments. The reinforcing potential of the multiaxial grids is demonstrated by means of evaluating drop tower experiments on automotive components. It has been shown that the load-adapted reinforcement enables a significant local or global improvement of the properties of plastic components depending on industrial requirements.     

Covalent attachment of gold nanoparticles to DNA templates

Functionalized gold nanoparticles have been covalently bound to internal, modified sites on double-stranded DNA. Gold nanoparticles coated with mercaptosuccinic acid or thioctic acid were bound to amino-modified thymine bases on double-stranded DNA. Visible absorption spectra, gel electrophoresis, and atomic force microscopy were used to analyze the products. Thiol groups were added to one end of the gold/nanoparticle product, which was then attached to a gold surface. This method has the potential to allow controlled placement of particles with subnanometer precision and to allow attachment of the product to fixed contacts for nanodevice fabrication.