Structure and morphology studies of chromium film at elevated temperature in hypersonic environment

This paper presents the after shock heated structural and morphological studies of chromium film coated on hypersonic test model as a passive drag reduction element. The structural changes and the composition of phases of chromium due to shock heating (2850 K) are characterized using X-ray diffraction studies. Surface morphology changes of chromium coating have been studied using scanning electron microscopy (SEM) before and after shock heating. Significant amount of chromium ablation and sublimation from the model surface is noticed from SEM micrographs. Traces of randomly oriented chromium oxides formed along the coated surface confirm surface reaction of chromium with oxygen present behind the shock. Large traces of amorphous chromium oxide phases are also observed.

A Rare Phenoxido/Acetato/Azido Bridged Trinuclear and an Unprecedented Phenoxido/Azido Bridged One-Dimensional Polynuclear Nickel(II) Complexes: Synthesis, Crystal Structure, and Magnetic Properties with Theoretical Investigations on the Exchange Mechanism

The reaction of a tridentate Schiff base ligand HL (2-(3-dimethylaminopropylimino)-methyl]-phenol) with Ni(II) acetate or perchlorate salts in the presence of azide as coligand has led to two new Ni(II) complexes of formulas Ni3L2(OAc)(2)(mu(1,1)-N-3)(2)(H2O)(2)]center dot 2H(2)O (1) and Ni2L2(mu(1,1)-N-3) (mu(1,3)-N-3)](n)(2). Single crystal X-ray structures show that complex 1 is a linear trinuclear Ni(II) compound containing a mu(2)-phenwddo, an end-on (EO) azido and a syn-syn acetato bridge between the terminal and the central Ni(II) ions. Complex 2 can be viewed as a one-dimensional (1D) chain in which the triply bridged (di-mu(2)-phenoxido and EO azido) dimeric Ni-2 units are linked to each other in a zigzag pattern by a single end-to-end (EE) azido bridge. Variable-temperature magnetic susceptibility studies indicate the presence of moderate ferromagnetic exchange coupling in complex 1 with J value of 16.51(6) cm(-1). The magnetic behavior of 2 can be fitted in an alternating ferro- and antiferromagnetic model J(FM) = +34.2(2.8) cm(-1) and J(AF) = -21.6(1.1) cm(-1)] corresponding to the triple bridged dinuclear core and EE azido bridge respectively. Density functional theory (DFT) calculations were performed to corroborate the magnetic results of 1 and 2. The contributions of the different bridges toward magnetic interactions in both compounds have also been calculated.

Optical Properties Study of S40Se60-xSbx Bulk Alloys

Bulk samples of S40Se60-xSbx (with x=10, 20, 30, 40 at. %) were prepared from high purity S, Se and Sb by melt quenching method. XRD studies revealed that all the samples have poly-crystalline phase. The variation in optical properties with composition has been investigated by XPS and Raman spectroscopy. The intensity of XPS core level spectra changes with addition of Sb clearly interprets the optical properties change due to compositional variation. The Raman shift and new peak formation in these samples clearly shows the structural modifications due to Sb addition.

Phase relationships and magnetic properties of TbxDy1-xFe1.95 alloys

The effect of Tb/Dy ratio on the structural and magnetic properties of (Tb,Dy)Fe-2 class of alloys has been investigated using nine alloys of TbxDy1-xFe1.95 (x = 0-1) covering the entire range. Our results indicate that the three phases viz. (Tb,Dy)Fe-2 (major phase), (Tb,Dy)Fe-3 and(Tb,Dy)-solid solution (minor phases) coexist in all the alloys. The volume fraction of pro-peritectic (Tb,Dy)Fe-3 phase however, has a minimum at x = 0.4 and a maximum at x = 0.6 compositions. The volume fraction of this phase decreases upon heat treatment at 850 degrees C and 1000 degrees C. A Widmanstatten type precipitate of (Tb,Dy)Fe-3 was observed for Dy-rich compositions (0 <= x <= 0.5). The microstructural investigations indicate that the ternary phase equilibria of Tb-Dy-Fe are sensitive to Tb/Dy ratio including the expansion of (Tb,Dy)Fe-2 phase field which is in contrast to the pseudo-binary assumption that is followed in available literature to date. The lattice parameter, Curie temperature and coercivity are found to increase with Tb addition. Split of (440) peak of (Tb,Dy)Fe-2 observed in x >= 0.3 alloys indicate, a spin reorientation transition from 100] to 111] occurs with Tb addition. (C) 2012 Elsevier B. V. All rights reserved.

Deformation and Recrystallization texture evolution in Nano-crystalline Nickel

Deformation and recrystallization textures in nano-crystalline nickel with average grain size of 20 nm were investigated using X-ray diffraction, electron microscopy and differential scanning calorimetry. The deformation behaviour of nano-crystalline nickel is quite complicated due to intervention of other deformation mechanisms like grain boundary sliding and restoration mechanisms like grain growth and grain rotation to dislocation mediated slip. Recrystallization studies carried out on the deformed nano-crystalline nickel showed that the deformation texture was retained during low temperature annealing (300 degrees C), while at higher temperature (1000 degrees C), the texture got randomised. The exact mechanism of texture formation during deformation and recrystallization has been discussed.

Cobalt(II), Nickel(II) and Copper(II) complexes of a tetradentate Schiff base as photosensitizers: Quantum yield of O-1(2) generation and its promising role in anti-tumor activity

In the present investigation, a Schiff base N'(1),N'(3)-bis(E)-(5-bromo-2-hydroxyphenyl)methylidene]benzene-1,3-d icarbohydrazide and its metal complexes have been synthesized and characterized. The DNA-binding studies were performed using absorption spectroscopy, emission spectra, viscosity measurements and thermal denatuaration studies. The experimental evidence indicated that, the Co(II), Ni(II) and Cu(II) complexes interact with calf thymus DNA through intercalation with an intrinsic binding constant K-b of 2.6 x 10(4) M-1, 5.7 x 10(4) M-1 and 4.5 x 10(4) M-1, respectively and they exhibited potent photo-damage abilities on pUC19 DNA, through singlet oxygen generation with quantum yields of 0.32, 0.27 and 0.30 respectively. The cytotoxic activity of the complexes resulted that they act as a potent photosensitizers for photochemical reactions. (C) 2012 Elsevier B.V. All rights reserved.

Effect of co-substitution of Mn and Al on thermoelectric properties of chromium disilicide

CrSi2 was earlier reported to be an interesting thermoelectric material for high temperature applications because of its high oxidation resistance and good mechanical properties. In order to enhance its figure of merit, Mn at Cr site and Al at Si site were substituted into CrSi2. Our results indicate that Cr1-x Mn (x) Si2-x Al (x) solid solutions exhibit significantly lower thermal conductivity and a higher figure of merit than CrSi2.

Synthesis and characterization of nickel/barium hexa-aluminate composite coatings

Electrodeposition of nickel/barium hexa-aluminate (Ni/BHA) composite coatings has been carried out from a Watt's bath on mild steel substrate. BHA powders with plate habit were synthesized by solution combustion synthesis followed by heat treatment to ensure complete conversion to the hexa-aluminate phase. Heat treated material was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) combined with X-ray analysis. The dispersion behaviour and stability of BHA suspensions with cationic and anionic surfactants at room temperature were studied by dynamic light scattering under different pH. The influence of BHA concentration in the electrolytic bath, deposition temperature, pH, current density and duty cycle on particle incorporation in the coatings were studied and conditions for maximum particle incorporation were established. Coatings with a roughness of about 0 center dot 4 mu m were produced by using this technique. Effect of BHA content on microhardness was also investigated. A reasonably good thickness of the coatings was achieved in a given set of conditions.

Microstructural Evolution and Some Unusual Effects During Thermo-Mechanical Cycling of Sn-Ag-Cu Alloys

Sn-Ag-Cu (SAC) solders are susceptible to appreciable microstructural coarsening during storage or service. This results in evolution of joint properties over time, and thereby influences the long-term reliability of microelectronic packages. Accurate prediction of this aging behavior is therefore critical for joint reliability predictions. Here, we study the precipitate coarsening behavior in two Sn-Ag-Cu (SAC) alloys, namely Sn-3.0Ag-0.5Cu and Sn-1.0Cu-0.5Cu, under different thermo-mechanical excursions, including isothermal aging at 150 degrees C for various lengths of time and thermo-mechanical cycling between -25 degrees C and 125 degrees C, with an imposed shear strain of similar to 19.6% per cycle, for different number of cycles. During isothermal aging and the thermo-mechanical cycling up to 200 cycles, Ag3Sn precipitates undergo rapid, monotonous coarsening. However, high number of thermo-mechanical cycling, usually between 200 and 600 cycles, causes dissolution and re-precipitation of precipitates, resulting in a fine and even distribution. Also, recrystallization of Sn-grains near precipitate clusters was observed during severe isothermal aging. Such responses are quite unusual for SAC solder alloys. In the regime of usual precipitate coarsening in these SAC alloys, an explicit parameter, which captures the thermo-mechanical history dependence of Ag3Sn particle size, was defined. Brief mechanistic description for the recrystallization of Sn grains during isothermal aging and reprecipitation of the Ag3Sn due to high number of thermo-mechanical cycles are also presented.

Mixed-ligand nickel(II) thiosemicarbazone complexes: Synthesis, characterization and biological evaluation

The syntheses and characterization of some new mixed-ligand nickel(II) complexes {Ni(L-1)(PPh3)] (1), Ni(L-1)(Py)] (2), Ni(L-2)(PPh3)]center dot DMSO (3), Ni(L-2)(Imz)] (4), Ni(L-3)(4-pic)] (5) and RNi(L-3))(2)(mu-4,4'-byp)]center dot 2DMSO (6)1 of three selected thiosemicarbazones the 4-(p-X-phenyl)thiosemicarbazones of salicylaldehyde) (H2L1-3) (A, Scheme 1) are described in the present study, differing in the inductive effect of the substituent X (X = F, Br and OCH3), in order to observe its influence, if any, on the redox potentials and biological activity of the complexes. All the synthesized ligands and the metal complexes were successfully characterized by elemental analysis, IR, UV-Vis, NMR spectroscopy and cyclic voltammetry. The molecular structures of four mononuclear (1-3 and 5) and one dinuclear (6) Ni(II) complex have been determined by X-ray crystallography. The complexes have been screened for their antibacterial activity against Escherichia coli and Bacillus. The minimum inhibitory concentrations of these complexes and their antibacterial activities indicate that compound 4 is the potential lead molecule for drug designing. (C) 2012 Elsevier Ltd. All rights reserved.

Synthesis, antimicrobial, DNA-binding and photonuclease studies of Cobalt(III) and Nickel(II) Schiff base complexes

New metal complexes of the type M(nih)(L)](PF6)(n)center dot xAH(2)O and M(nih)(2)](PF6)center dot xH(2)O (where M = Co(III) or Ni(II), L = 1,10-phenanthroline (phen)/or 2,2' bipyridine (bpy), nih = 2-hydroxy-1-naphthaldehyde isonicotinoyl hydrazone, n = 2 or 1 and x = 3 or 2) have been synthesized and characterized by elemental analysis, magnetic, IR and H-1 NMR spectral data. The electronic and magnetic moment 2.97-3.07 B.M. data infers octahedral geometry for all the complexes. The IR data reveals that Schiff base (nih) form coordination bond with the metal ion through azomethine-nitrogen, phenolic-oxygen and carbonyl-oxygen in a tridentate fashion. In addition, DNA-binding properties of these six metal complexes were investigated using absorption spectroscopy, viscosity measurements and thermal denaturation methods. The results indicated that the nickel(II) complex strongly bind with calf-thymus DNA with intrinsic DNA binding constant K-b value of 4.9 x 10(4) M-1 for (3), 4.2 x 10(4) M-1 for (4), presumably via an intercalation mechanism compared to cobalt(III) complex with K-b value of 4.6 x 10(4) M-1 (1) and 4.1 x 10(4) M-1 (2). The DNA Photoclevage experiment shows that, the complexes act as effective DNA cleavage agent. (C) 2012 Elsevier B.V. All rights reserved.

The effect of minor addition of Ni on the microstructural evolution and mechanical properties of suction cast Al-0.14 at. pct Sc binary alloy

Aluminum scandium binary alloys represent a promising precipitation-hardening alloy system. However, the hardness of the binary alloys decreases with the rapid coarsening of Al3Sc precipitate during high-temperature aging. In the current study, we report a new approach to compensate for the loss of mechanical properties by combining rapid solidification with very small ternary addition of transition metal Ni. This addition yields dispersion, and at a critical concentration improves the mechanical properties. We explore additions of a maximum of 0.06 at. pct of Nickel to a binary Al-0.14 at. pct Sc alloy, which yield nickel-rich dispersions. We report two kinds of biphasic dispersions containing AlNi2Sc/Al9Ni2 and alpha-Al/Al9Ni2 phase combinations. The maximum improvement in mechanical properties occurs with the addition of 0.045 at. pct Ni with a yield strength of 239 +/- A 7 MPa for an aging treatment at 583 K (310 A degrees C) for 15 hours. DOI: 10.1007/s11661-013-1624-z (C) The Minerals, Metals & Materials Society and ASM International 2013

Isothermal transformation of beta-phase in Cu-rich Cu-Al-Sn alloys

Microstructural changes resulting from isothermal decomposition of the beta-phase have been studied in Cu-rich binary Cu-Al and ternary Cu-Al-Sn alloys containing up to 3 at.% Sn at temperatures from 873 to 673 K. Results are presented as TTT diagrams. The decomposition occurs in several stages, each of which involves the establishment of metastable equilibrium between beta and one or more of the product phases alpha, beta(1) and gamma(2). Addition of Sn has been shown to increase the stability of the ordered beta(1)-phase in relation to beta. In alloys containing more than 2 at.% Sn, the beta(1) emerges as a stable phase. At low Sn concentrations beta(1) is metastable. An important new finding is the existence of three-phase equilibrium microstructure containing alpha, beta(1) and gamma(2). Increasing addition of Sn alters the morphology of beta(1) from rosettes to dendrites and finally to Widmanstatten needles.

Carbonaceous nickel oxide nano-composites: as electrode materials in electrochemical capacitor applications

Carbonaceous nickel oxide powder samples have been synthesized from an adducted nickel beta-ketoester complex used as a ``single source precursor'' through a solution-based microwave-assisted chemical route. Comprehensive analysis of the resulting powder material has been carried out using various characterization techniques. These analysis reveal that, depending on the solvent used, either NiO/C or Ni/NiO/C composites are formed, wherein Ni and/or NiO nanocrystals are enveloped in amorphous carbon. As the components emerge from the same molecular source, the composites are homogeneous on a fine scale, making them promising electrode materials for supercapacitors. Electrochemical capacitive behavior of these oxide composites is studied in a three-electrode configuration. With a specific capacitance of 113 F g(-1), Ni/NiO/C is superior to NiO/C as capacitor electrode material, in 0.1 M Na2SO4 electrolyte. This is confirmed by impedance measurements, which show that charge-transfer resistance and equivalent series resistance are lower in Ni/NiO/C than in NiO/C, presumably because of the presence of metallic nickel in the former. The cyclic voltammograms are nearly rectangular and the electrodes display excellent cyclability in different electrolytes: Na2SO4, KOH and Ca(NO3)(2)center dot 4H(2)O. Specific capacitance as high as 143 F g(-1), is measured in Ca(NO3)(2)center dot 4H(2)O electrolyte.

Effect of thermal and thermo-mechanical cycling on the microstructure of Ni-rich NiTi shape memory alloys

Microstructural changes of Ni-rich NiTi shape memory alloy during thermal and thermo-mechanical cycling have been investigated using Electron Back Scattered Diffraction. A strong dependence of the orientation of the prior austenite grain on the misorientation development has been observed during thermal cycling and thermo-mechanical cycling. This effect is more pronounced at the grain boundaries compared to grain interior. At a larger applied strain, the volume fraction of stabilized martensite phase increases with increase in the number of cycling. Deformation within the martensite leads to stabilization of martensitic phase even at temperatures slightly above the austenite finish temperature. Modulus variation with respect to temperature has been explained on the basis of martensitic transformation.