Spin-Selective Correlation Experiment for Measurement of Long-Range J Couplings and for Assignment of (R/S) Enantiomers from the Residual Dipolar Couplings and DFT

We report the C-HETSERF experiment for determination of long- and short-range homo- and heteronuclear scalar couplings ((n)J(HH) and (n)J(XH), n >= 1) of organic molecules with a low sensitivity dilute heteronucleus in natural abundance. The method finds significant advantage in measurement of relative signs of long-range heteronuclear total couplings in chiral organic liquid crystal. The advantage of the method is demonstrated for the measurement of residual dipolar couplings (RDCs) in enantiomers oriented in the chiral liquid crystal with a focus to unambiguously assign R/S designation in a 2D spectrum. The alignment tensor calculated from the experimental RDCs and with the computed structures of enantiomers obtained by DFT calculations provides the size of the back-calculated RDCs. Smaller root-mean-square deviations (rmsd) between experimental and calculated RDCs indicate better agreement with the input structure and its correct designation of the stereogenic center.

Measurement of Gibbs energy of formation of Ca2PbO4 using a solid-state cell with three electrodes

Phase relations in the system Ca-Pb-O at 1100 K have been determined by equilibrating 18 compositions in the ternary and identifying the phases present in quenched samples by X-ray diffraction and energy dispersive X-ray analysis (EDX). Only one ternary compound Ca2PbO4 was found to be present. The compound coexists with CaO and PbO. The intermetallic compounds Ca2Pb, Ca5Pb3 and CaPb and liquid alloys are in equilibrium with CaO. The standard Gibbs energies of formation of Ca2PbO4 (880 - 1100 K) and Pb3O4 (770 - 910 K) were determined using solid-state cells based on yttria-stabilized zirconia as the solid electrolyte. Pure oxygen gas at 0.1 MPa was used as the reference electrode. For measurements on Ca2PbO4, a novel cell design with three electrodes in series, separated by solid electrolyte membranes, was used to avoid polarization of the electrode containing three solid phases. Two three-phase electrodes were used. The first absorbs the electrochemical flux of oxygen from the reference electrode to the measuring electrode. The other three-phase electrode, which is unaffected by the oxygen flux through the solid electrolyte, is used for electromotive force (EMF) measurement. The results from EMF studies were cross-checked using thermogravimetry (TG) under controlled oxygen partial pressures. The stability of Pb3O4 was investigated using a conventional solid-state cell with RuO2 electrodes. The results can be summarized by the following equations: 2CaO + PbO +1/2O(2) --> Ca2PbO4 Delta(r)G degrees/J mol(-1) = (- 128340 + 93.21 T/K) +/- 200 3PbO + 1/2O(2) --> Pb3O4 Delta(r)G degrees/J mol(-1) = (- 70060 + 77.5 T/K) +/- 150

Method for measurement of the angles of 90-, 45-, 45-deg and 60-, 30-, 90-deg prisms

A simple technique is devised to measure the angles of 90-, 45-, 45-deg and 60-, 30-, 90-deg prisms without using expensive spectrometers, autocollimators, and angle gauges. The method can be extended to unpolished and opaque prisms made of materials other then glass. (C) 1997 Society of Photo-Optical instrumentation Engineers.

Method for measurement of the angles of an equilateral (60-deg) prism

A simple technique is devised io measure the angles of equilateral (60-deg) prisms, without using the expensive spectrometers, autocollimators, and angle gauges. The method can be extended to unpolished and opaque prisms made out of materials other than glass. (C) 1997 Society of Photo-Optical Instrumentation Engineers.

Nucleation and growth characteristics of cavities during the early stages of tensile creep deformation in a superplastic zirconia-20 wt% alumina composite

Constant-stress tensile creep experiments on a superplastic 3-mol%-yttria-stabilized tetragonal zirconia composite with 20 wt% alumina revealed that cavities nucleate relatively early during tensile deformation. The number of cavities nucleated increases with increasing imposed stress. The cavities nucleate at triple points associated largely with an alumina grain, and then grow rapidly in a cracklike manner to attain dimensions on the order of the grain facet size. It is suggested that coarser-grained superplastic ceramics exhibit lower ductility due to the ease in formation of such grain boundary facet-cracks and their interlinkage to form a macroscopic crack of critical dimensions.

Regarding the effect of aging heat treatment on the failure behaviour of a SiC reinforced Al based metal matrix composite

In the present study, 6061 Al metallic matrix was reinforced by 12.2 wt% df SiC particulates using liquid metallurgy route. The composite material thus obtained was extruded and characterized in the as-solutionized and peak aged conditions in order to delineate the effect of aging associated precipitation of secondary phases on the tensile fracture behavior of the composite samples. The results' of microstructural characterization studies carried out using scanning electron microscope revealed the increased presence of precipitated secondary phases in the metallic matrix and a more pronounced interfacial segregation of alloying elements in case of peak aged samples when compared to the as-solutionized samples. The results of the fractographic studies conducted on the as-solutionized samples revealed that the failure was dominated by the SiC particulates cracking while for the peak aged samples the fracture surface revealed a comparatively more pronounced SiC/6061 Al debonding and reduced SiC particulates cracking. This change in the failure behavior was rationalized in terms of embrittlement of the interfacial region brought about by the aging heat treatment and is correlated, in addition, with the mechanical properties of the composite samples in as-solutionized and peak aged conditions.

Microstructure and properties of squeeze cast Cu-carbon fibre metal matrix composite

There have been reported attempts of producing Cu based MMCs employing solid phase routes. In this work, copper was reinforced with short carbon fibres by pressure infiltration (squeeze casting) of molten metal through dry-separated carbon fibres. The resulting MMC's microstructure revealed uniform distribution of fibres with minimum amount of clustering. Hardness values are considerably higher than that for the unreinforced matrix. Addition of carbon fibres has brought in strain in the crystal lattice of the matrix, resulting in higher microhardness of MMCs and improved wear resistance. Tensile strength values of MMCs at elevated temperatures are considerably higher than that of the unreinforced matrix processed under identical conditions. (C) 1999 Kluwer Academic Publishers.

Residual strength and fatigue life assessment of composite patch repaired specimens

Design, analysis and technology for the integrity enhancement of damaged or underdesigned structures continues to be an engineering challenge. Bonded composite patch repairs to metallic structures is receiving increased attention in the recent years. It offers various advantages over rivetted doubler, particularly for airframe repairs. This paper presents an experimental investigation of residual strength and fatigue crack-growth life of an edge-cracked aluminium specimen repaired using glass epoxy composite patch. The investigation begins with the evaluation of three different surface treatments from bond strength viewpoint. A simple thumb rule formula is employed to estimate the patch size. Cracked and repaired specimens are tested under static and fatigue loading. The patch appears to restore the original strength of the undamaged specimen and enhance the fatigue crack growth life by an order of magnitude. (C) 1999 Elsevier Science Ltd. All rights reserved.

Sensing of delaminations in composite laminates using embedded magnetostrictive particle layers

This is an exploratory study to illustrate the feasibility of detecting delamination type of damage in polymeric laminates with one layer of magnetostrictive particles. One such beam encircled with excitation and sensing coils is used for this study. The change in stress gradient of the magnetostrictive layer in the vicinity of delamination shows up as a change in induced voltage in the sensing coil, and therefore provides a means to sense the presence of delamination. Recognizing the constitutive behavior of the Terfenol-D material is highly nonlinear, analytical expressions for the constitutive relations are developed by using curve fitting techniques to the experimental data. Analytical expressions that relate the applied excitation field with the stress and magnetic flux densities induced in the magnetostrictive layer are developed. Numerical methods are used to find the relative change in the induced voltage in the sensing coil due to the presence of delamination. A typical example of unidirectional laminate, with embedded delaminations, is used for the simulation purposes. This exploratory study illustrates that the open-circuit voltage induced in the sensing coil changes significantly (as large of 68 millivolts) with the occurrence of delamination. This feature can be exploited for device off-line inspection techniques and/or linking monitoring procedures for practical applications.

Studies on indentation fracture toughness on ceramic and ceramic composite using acoustic emission technique

This paper is aimed at investigating the acoustic emission activities during indentation toughness tests on an alumina based wear resistant ceramic and 25 wt% silicon carbide whisker (SIC,) reinforced alumina composite. It has been shown that the emitted acoustic emission signals characterize the crack growth during loading. and unloading cycles in an indentation test. The acoustic emission results indicate that in the case of the composite the amount of crack growth during unloading is higher than that of loading, while the reverse is true in case of the wear resistant ceramics. Acoustic emission activity observed in wear resistant ceramic is less than that in the case of composite. An attempt has been made to correlate the acoustic emission signals with crack growth during indentation test.

The studies on micro-structural defects in deformed composite matrix of Al-Si-Mg and SiC

Detailed Fourier line shape analysis has been performed on three different compositions of the composite matrix of Al-Si-Mg and SiC. The alloy composition in wt% is Al-7%Si, 0.35%Mg, 0.14%Fe and traces of copper and titanium (similar to 0.01%) with SiC varying from 0 to 30wt% in three steps i.e., 0, 10 and 30wt%. The line shift analysis has been performed by considering 111, 200, 220, 311 and 222 reflections after estimating their relative shift. Peak asymmetry analysis has been performed considering neighbouring 111 and 200 reflections and Fourier line shape analysis has been performed after considering the multiple orders 111 and 222, 200 and 400 reflections. Combining all these three analyses it has been found that the deformation stacking faults both intrinsic alpha' and extrinsic alpha " are absent in this alloy system whereas the deformation twin beta has been found to be positive and increases with the increase of SiC concentration. So, like other Al-base alloys this ternary alloy also shows high stacking fault energy, and the addition of SiC introduces deformation twin which increases with its concentration in the deformed lattices.

Non-resonant perturbation formula for interaction impedance measurement for a folded-waveguide SWS

The non-resonant perturbation formula for the measurement of interaction impedance of a folded-waveguide slow-wave structure was derived for the relevant electromagnetic field configuration at the axis of the beam-hole of the structure. Efficacy of the theory was benchmarked through virtual measurement using 3D electromagnetic modeling in CST-studio.

Bubble size measurement in a gas-liquid ejector for a sodium chloride-air system

A high speed photographic technique has been employed to measure the Sauter mean diameter of bubbles experimentally in a gas liquid ejector using a sodium chloride-air system. The measured values are compared with the theoretically predicted maximum bubble size diameter using Sprow's correlation. Bubble size as a function of the liquid flow rate and also of its distance from the throat of the ejector has been reported in this paper. The results obtained for this non-reactive system are also compared with those obtained earlier for the air-water system.

Enhanced lithium-ion transport in PEG-based composite polymer electrolyte with Mn0.03Zn0.97Al2O4 nanoparticles

The ion conduction and thermal properties of composite solid polymer electrolyte (SPE) comprising Poly(ethylene) Glycol (PEG, mol wt. 2000), lithium perchlorate (LiClO4) and insulating Mn0.03Zn0.97Al2O4 nanoparticle fillers were studied by complex impedance analysis and DSC techniques. The average size of the nanoparticles was determined by powder X-ray diffraction (XRD) using Scherrer's equation and was found to be similar to 8 nm. The same was also determined by TEM imaging and found to be similar to 12 nm. The glass transition temperature T, as measured by differential scanning calorimeter (DSC), showed a minimum at 5 mol% of narroparticles. Fractional crystallinity was determined using DSC. NMR was used to deter-mine crystallinity of a pure PEG sample, which was then used as the standard. Fractional crystallinity X. was the lowest for 5 mol% and beyond. The ionic conductivity of the composite polymer electrolyte containing 5 mol% Mn0.03Zn0.97Al2O4 nanoparticles was found to be 1.82 x 10(-5) S/cm, while for the pristine one, it was 7.27 x 10(-7) S/cm at room temperature. As a function of nanoparticle content, conductivity was observed to go through two maxima, one at around 5 mol% and another shallower one at around 12 mol%. The temperature dependence of conductivity could be divided into two regions, one consistent with Arrhenius behaviour and the other with VTF. We conclude that the enhancement of ionic conductivity on the addition of Mn0.03Zn0.97Al2O4 nanoparticles is a result of reduction in both the T, and the crystallinity. (C) 2002 Elsevier Science B.V. All rights reserved.