NMR study of slow motions of HDA hydrocarbons chains inside lamellar structures

Measurements of H-1 and C-13 Nuclear Magnetic Resonance (NMR) for the nano-composite materials formed by the intercalation of hexadecylamine (HDA) in metal oxides (TiO2, V2O5 and MoO3), are reported. The H-1 NMR spin-lattice relaxation in the rotating frame was described by using the spectral density due to Davidson and Cole, which incorporates a distribution of correlation times characterized by a width parameter epsilon. The fitting of the data was obtained for epsilon = 0.74, indicating that the correlation times are distributed over a narrow range in this system. High-resolution C-13 NMR techniques were used to resolve the NMR lines of middle-chain methylene groups in the spectra and variable contact time cross-polarization {H-1-}C-13 experiments were employed to analyze the reorientation dynamics of the CH3 and CH2 groups in the HDA chains.

Experimental micromorphology in Tierra del Fuego (Argentina): building a reference collection for the study of shell middens in cold climates

Commonly used in archaeological contexts, micromorphology did not see a parallel advance in the field of experimental archaeology. Drawing from early work conducted in the 1990`s on ethnohistoric sites in the Beagle Channel, we analyze a set of 25 thin sections taken from control features and experimental tests. The control features include animal pathways and environmental contexts (beach samples, forest litter, soils from the proximities of archaeological sites), while the experimental samples comprise anthropic structures, such as hearths, and valves of Mytilus edulis (the most important component of shell middens in the region) heated from 200 degrees C to 800 degrees C. Their micromorphological study constitutes a modern analogue to assist archaeologists studying site formation and ethnographical settings in cold climates, with particular emphasis on shell midden contexts. (c) 2010 Elsevier Ltd. All rights reserved.

Synthesis, Spectroscopic Studies and X-ray Crystal Structures of New Pyrazoline and Pyrazole Derivatives

The synthesis and characterization of some pyrazoline compounds of 1,3-diketones with hydrazine derivatives, namely, 1-(S-benzyldithiocarbazate)-3-methyl-5-phenyl-5-hydroxypyrazoline (1); 1-(2-thiophenecarboxylic)-3-methyl-5-phenyl-5-hydroxypyrazoline (2); 1-(2-thiophenecarboxylic)-3,5-dimethyl-5-hydroxypyrazoline (3); 1-(S-benzyldithiocarbazato)-3-methyl-5-phenylpyrazole (4); 1-(2-thiophenecarboxylic)-3-methyl-5-phenylpyrazole (5) and 1-(S-benzyldithiocarbazate)-3,5-dimethylpyrazole (6) are reported. Studies by IR, ((1)H, (13)C)-NMR spectroscopies and single crystal X-ray diffraction revealed that compounds (1)(,) (2) and (3) are formed as pyrazoline, whereas (4) and (5) are formed as pyrazole derivatives only under acidic conditions. Compound (1) crystallizes in orthorhombic P2(1)2(1)2(1), a = 6.38960(10) angstrom, b = 12.9176(3) angstrom, c = 21.2552(5) angstrom, (2) crystallizes in monoclinic, P2(1)/n, a = 11.3617(2) angstrom, b = 8.4988(2) angstrom, c = 92.8900(10)angstrom and beta = 92.8900(5)degrees, (3) crystallizes in monoclinic, C2/c, a = 15.9500(5) angstrom, b = 9.3766(3) angstrom, c = 16.6910(5)angstrom and beta = 113.825(2)degrees, (4) crystallizes in monoclinic, P2(1)/c, a = 15.228(4) angstrom, b = 5.5714(13) angstrom, c = 19.956(5)angstrom and beta = 91.575(7)degrees and (6) crystallizes in orthorhombic, P2(1)2(1)2(1), a = 5.3920(2) angstrom, b = 11.2074(5) angstrom, c = 21.885(1)angstrom . The (3) derivative represents the first pyrazoline compound prepared from 2,4-pentanedione and characterized crystallographically.

Evaluation of galling resistance for some selected combinations of tool steels/stainless steel sheet materials/lubricants using pin-on-disc testing

Stainless steels are well known to be prone to cold welding and material transfer in sliding contacts and therefore difficult to cold form unless certain precautions as discussed in this paper are taken. In the present study different combinations of tool steels/stainless steels/lubricants has been evaluated with respect to their galling resistance using pin-on-disc testing. The results show that a high galling resistance is favored by a high stainless steel sheet hardness and a blasted stainless steel sheet surface topography. The effect of type of lubricant was found to be more complex. For example, the chlorinated lubricants failed to prevent metal-to-metal contact on a brushed sheet surface but succeeded on a blasted sheet surface of the same stainless steel material. This is believed to be due to a protective tribofilm which is able to form on the blasted surface, but not on the brushed surface.

Effect of cooling rate on properties of plasma nitrided AISI 1010 steel

In this work, AISI 1010 steel samples were plasma nitrided into 20% N 2 100 Pa and 400 Pa for N 2 and H 2 , respectively), temperatures of 500 and 580 °C, during 2 h. Three different procedures for cooling were accomplished after nitriding. In the first procedure the cooling occurred naturally, that is, the sample was kept on substrate holder. In the second one the sample was pulled off and cooling in a cold surface. Finally, in the third cooling process the sample was pulled off the substrate holder down into special reservoir filled with oil held at ambient temperature. The properties of the AISI 1010 steel samples were characterized by optical and electron microscopy, X-ray diffraction, Mössbauer spectroscopy and microhardness tests. Thermal gradient inside the sample kept on substrate holder during cooling process was measured by three inserted thermocouples at different depths. When samples were cooled rapidly the transformation of ϵ-Fe 2 − 3 N to γ′-Fe 4 N was inhibited. Such effect is indicated by the high concentration of ϵ-Fe compound zone. To get solid state solution of nitrogen in the diffusion zone, instead of precipitates of nitride phases, the cooling rate should be higher than a critical value of about 0.95 °C/s. When this value is reached at any depth of the diffusion zone, two distinct diffusion zones will appear. Temperature gradients were measured inside the samples as a consequence of the plasma treatment. It's suggested the need for standardization of the term “treatment temperature” for plasma treatment because different nitrided layer properties could be reported for the same “treatment temperature”.

Desenvolvimento e caracterização de um compósito matriz metálica (CMM): aço EUROFER97 reforçado com Carbeto de Tântalo - TaC

Steel is an alloy EUROFER promising for use in nuclear reactors, or in applications where the material is subjected to temperatures up to 550 ° C due to their lower creep resistance under. One way to increase this property, so that the steel work at higher temperatures it is necessary to prevent sliding of its grain boundaries. Factors that influence this slip contours are the morphology of the grains, the angle and speed of the grain boundaries. This speed can be decreased in the presence of a dispersed phase in the material, provided it is fine and homogeneously distributed. In this context, this paper presents the development of a new material metal matrix composite (MMC) which has as starting materials as stainless steel EUROFER 97, and two different kinds of tantalum carbide - TaC, one with average crystallite sizes 13.78 nm synthesized in UFRN and another with 40.66 nm supplied by Aldrich. In order to improve the mechanical properties of metal matrix was added by powder metallurgy, nano-sized particles of the two types of TaC. This paper discusses the effect of dispersion of carbides in the microstructure of sintered parts. Pure steel powders with the addition of 3% TaC UFRN and 3% TaC commercial respectively, were ground in grinding times following: a) 5 hours in the planetary mill for all post b) 8 hours of grinding in the mill Planetary only for steel TaC powders of commercial and c) 24 hours in the conventional ball mill mixing the pure steel milled for 5 hours in the planetary mill with 3% TaC commercial. Each of the resulting particulate samples were cold compacted under a uniaxial pressure of 600MPa, on a cylindrical matrix of 5 mm diameter. Subsequently, the compressed were sintered in a vacuum furnace at temperatures of 1150 to 1250 ° C with an increment of 20 ° C and 10 ° C per minute and maintained at these isotherms for 30, 60 and 120 minutes and cooled to room temperature. The distribution, size and dispersion of steel and composite particles were determined by x-ray diffraction, scanning electron microscopy followed by chemical analysis (EDS). The structures of the sintered bodies were observed by optical microscopy and scanning electron accompanied by EDS beyond the x-ray diffraction. Initial studies sintering the obtained steel EUROFER 97 a positive reply in relation to improvement of the mechanical properties independent of the processing, because it is obtained with sintered microhardness values close to and even greater than 100% of the value obtained for the HV 333.2 pure steel as received in the form of a bar

Nest Digging by Leaf-Cutting Ants: Effect of Group Size and Functional Structures.

Leaf-cutting ant workers dig underground chambers, for housing their symbiotic fungus, interconnected by a vast quantity of tunnels whose function is to permit the entrance of food (leaves), gaseous exchanges, andmovement of workers, offspring, and the queen. Digging is a task executed by a group of workers, but little is known about the group effect and group-constructed functional structures. Thus, we analyzed the structures formed by worker groups (5, 10, 20, and 40 individuals) of the leaf-cutting ant, Atta sexdens rubropilosa, for 2 days of excavation. The digging arena was the same for the 4 groups, with each group corresponding to a different density. Our results verified a pattern of tunneling by the workers, but no chamber was constructed. The group effect is well known, since the 40-worker group dug significantly more than the groups of 5, 10, and 20. These groups did not differ statistically from each other. Analysis of load/worker verified that workers of the smallest group carried the greatest load. Our paper demonstrates the group effect on the digging of nests, namely, that excavation is proportional to group size, but without emergence of a functional structure such as a chamber.

Vanadium complexes with thiosemicarbazones: Synthesis, characterization, crystal structures and anti-Mycobacterium tuberculosis activity

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

FeNbP in ultra-low carbon Nb-added steel containing high P

Precipitation of FeTiP is reported to occur in Ti-added IF steels containing high P during thermomechanical processing. An ultra-low carbon (ULC) Nb-added steel ingot containing a higher P content (< 0.8 wt-%) was produced via aluminothermic reduction of Fe2O3 followed by double electron beam melting (EBM). FeNbP coarse precipitates were observed in the as-cast microstructure. After soaking at 1050C for 1 h, the plate was hot rolled from 31 mm down to 7 mm in thickness (total reduction of 77%). During cold rolling of these hot bands we observed embrittlement. We believe that this embrittlement can be attributed to the presence of the FeNbP precipitates. Light optical and scanning electron microscopy (SEM/EDS) were used to characterize the microstructure of this ULC steel. (C) 2000 Elsevier B.V. All rights reserved.

Residual stress influence on fatigue lifetimes of electroplated AISI 4340 high strength steel

Residual stresses play an important role in the fatigue lives of structural engineering components. In the case of near surface tensile residual stresses, the initiation and propagation phases of fatigue process are accelerated; on the other hand, compressive residual stresses close to the surface may increase fatigue life. In both decorative and functional applications, chromium electroplating results in excellent wear and corrosion resistance. However, it is well known that it reduces the fatigue strength of a component. This is due to high tensile internal stresses and microcrack density. Efforts to improve hard chromium properties have increased in recent years. In this study, the effect of a nickel layer sulphamate process, as simple layer and interlayer, on fatigue strength of hard chromium electroplated AISI 4340 steel hardness - HRc 53, was analysed. The analysis was performed by rotating bending fatigue tests on AISI 4340 steel specimens with the following experimental groups: base material, hard chromium electroplated, sulphamate nickel electroplated, sulphamate nickel interlayer on hard chromium electroplated and electroless nickel interlayer on hard chromium electroplated. Results showed a decrease in fatigue strength in coated specimens and that both nickel plating interlayers were responsible for the increase in fatigue life of AISI 4340 chromium electroplated steel. The shot peening pre-treatment was efficient in reducing fatigue loss in the alternatives studied.

Improvement in the fatigue strength of chromium electroplated AISI 4340 steel by shot peening

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Repair Welding Effects on the Bending Fatigue Strength of AISI 4130 Aeronautical Steel used in a Critical to the Flight-Safety Structure

The aim of this study was to analyze the effect of successive TIG (tungsten inert gas) welding repairs on the reverse bending fatigue strength of AISI 4130 steel, which is widely used in components critical to the flight-safety. In order to simulate the abrupt maneuvers, wind bursts, motor vibration and helixes efforts, which generate cyclic bending loadings at the welded joints of a specific aircraft component called motor cradle, experimental reverse bending fatigue tests were carried out on specimens made from hot-rolled steel plate, 1.10 mm (0.043 in) thick, by mean of a SCHENK PWS equipment, with load ratio R = -1, under constant amplitude, at 30 Hz frequency and room temperature. It was observed that the bending fatigue strength decreases after the TIG (Tungsten Inert Gas) welding process application on AISI 4130 steel, with subsequent decrease due to re-welding sequence as well. Microstructural analyses and microhardness measurements on the base material, heat-affected zone (HAZ) and weld metal, as well as the effects of the weld bead geometry on the obtained results, have complemented this study.

Effects of several TIG weld repairs on the axial fatigue strength of AISI 4130 aeronautical steel-welded joints

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Fatigue strength of tungsten inert gas-repaired weld joints in airplane critical structures

In this work the effect of Gas Tungsten Arc Welding (GTAW) repairs on the axial fatigue strength of an AISI 4130 steel welded joint used in airframe critical to the flight-safety was investigated. Fatigue tests were performed at room temperature on 0.89 mm thick hot-rolled plates with constant amplitude and load ratio of R = 0.1, at 20 Hz frequency. Monotonic tensile tests, optical metallography and microhardness, residual stress and weld geometric factors measurements were also performed. The fatigue strength decreased with the number of GTAW repairs, and was related to microstructural and microhardness changes, as well as residual stress field and weld profile geometry factors, which gave origin to high stress concentration at the weld toe. (C) 2011 Elsevier B.V. All rights reserved.

Orientation dependence of stored energy of cold work in semi-processed electrical steels after temper rolling

Microhardness measurements were carried out in a low carbon lamination steel after 6% of temper rolling, in order to evaluate local variations of work hardening as a function of crystallographic orientation. EBSD (electron back scattered diffraction) was used to determine grain orientations with respect to individual rolling planes and rolling directions. Hardness was shown to increase with the local Taylor factor. TEM observations and a well-known dislocation hardening model were used to confirm the equivalence between hardness values and the stored energy of cold work. A definite correlation between stored energy and Taylor factors could therefore be established, being more consistent than previous data reported in the literature. The improvement was thought to be related to the rather small plastic deformation, during which Taylor factors could be considered to remain constant. (c) 2006 Elsevier B.V. All rights reserved.