Synthesis of free standing nanocrystalline Cu by ball milling at cryogenic temperature

This paper reports for the first time synthesis of free standing nano-crystalline copper crystals of a similar to 30-40 nm by ball milling of copper powder at 150 K under Argon atmosphere in a specially designed cryomill. The detailed characterization of these particles using multiple techniques that includes transmission electron microscopy confirms our conclusion. Careful analysis of the chemistry of these particles indicates that these particles are essentially contamination free. Through the analysis of existing models of grain size refinements during ball milling and low temperature deformation, we argue that the suppression of thermal processes and low temperature leads to formation of free nanoparticles as the process of fracture dominates over possible cold welding at low temperatures. (C) 2012 Elsevier B.V. All rights reserved.

Texture evolution in high strain rate deformed Cu-10Zn alloy

High strain rate deformation behavior of Cu-10Zn alloy was studied. A weak texture with fine grain size was observed at high strain rate. The weak texture has been attributed to activity of higher number of slip systems under dynamic loading conditions. Twinning has minimal role on texture. (C) 2012 Elsevier B.V. All rights reserved.

Diffusion mechanism in the gold-copper system

Interdiffusion study is conducted in the Au-Cu system, which has complete solid solution in the higher temperature range and ordered phases in the lower temperature range. First experiments are conducted at higher temperatures, where atoms can diffuse randomly. Higher values of interdiffusion coefficients are found in the range of 40-50 at.% Cu. This trend is explained with the help of thermodynamic factor and possible concentration of vacancies. Following an experiment is conducted at 623 K (350 degrees C), where the ordered phases are grown. The interdiffusion coefficients at this temperature are compared after extrapolating the data calculated at higher temperatures.

Preparation and characterization chemistry of nano-crystalline Ni-Cu-Zn ferrite

In submitted research; nanocrystalline powders having elements Ni0.5Cu0.25Zn0.25Fe2 xInxO4 with varied amounts of indium ( x = 0.0, 0.1, 0.2, 0.3 and 0.4) were grown-up by modified citrate to nitrate alchemy. The realism of single phase cubic spinel creation of the synthesized ferrite samples was studied by the DTA-TGA, XRD, SEM, EDX, FT-IR, VSM and dielectric measurements. SEM was applied to inspect the morphological variations and EDX was used to determine the compositional mass ratios. The studies on the dielectric constant (epsilon'), dielectric loss (epsilon `'), loss tangent (tan delta), ac conductivity (sigma(ac)), resistive and reactive parts of the impedance analysis (Z' and Z `') at room temperature were also carried out. The saturation magnetizations (Ms) were determined using the vibrating sample magnetometer (VSM). Ms. decreased with the increase In3+ doping content, as Fe3+ of 5(mu B) ions are replaced by In3+ of 5 mu(B) ions. (C) 2012 Elsevier B. V. All rights reserved.

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.

Strategies for the Synthesis of Graphene, Graphene Nanoribbons, Nanoscrolls and Related Materials

Single-layer graphene (SLG), the 3.4 angstrom thick two-dimensional sheet of sp(2) carbon atoms, was first prepared in 2004 by mechanical exfoliation of graphite crystals using the scotch tape technique. Since then, SLG has been prepared by other physical methods such as laser irradiation or ultrasonication of graphite in liquid media. Chemical methods of synthesis of SLG are more commonly used; the most popular involves preparation of single-layer graphene oxide followed by reduction with a stable reagent, often assisted by microwave heating. This method yields single-layer reduced graphene oxide. Other methods for preparing SLG include chemical vapour deposition over surfaces of transition metals such as Ni and Cu. Large-area SLG has also been prepared by epitaxial growth over SIC. Few-layer graphene (FLG) is prepared by several methods; arc discharge of graphite in hydrogen atmosphere being the most convenient. Several other methods for preparing FLG include exfoliation of graphite oxide by rapid heating, ultrasonication or laser irradiation of graphite in liquid media, reduction of few-layer graphene oxide, alkali metal intercalation followed by exfoliation. Graphene nanoribbons, which are rectangular strips of graphene, are best prepared by the unzipping of carbon nanotubes by chemical oxidation or laser irradiation. Many graphene analogues of inorganic materials such as MoS2, MoSe2 and BN have been prepared by mechanical exfoliation, ultrasonication and by chemical methods involving high-temperature or hydrothermal reactions and intercalation of alkali metals followed by exfoliation. Scrolls of graphene are prepared by potassium intercalation in graphite or by microwave irradiation of graphite immersed in liquid nitrogen.

Synthesis, characterization and phosphotriesterase mimetic activity of some Zn(II) and Cu(II) complexes

We report here the synthesis and characterization of a few phenolate-based ligands bearing tert- amino substituent and their Zn(II) and Cu(II) metal complexes. Three mono/binuclear Zn(II) and Cu(II) complexes Zn(L1)(H2O)].CH3OH.H2O (1) (H (2) L1 = 6,6(')-(((2-dimethylamino)ethylazanediyl)bis(methylene))bis(2, 4-dimethylphenol), Zn-2(L2)(2)] (2) (H (2) L2 = 2,2(')-(((2-dimethylamino)ethyl)azanediyl)bis(methylene)bis(4- methylphenol) and Cu-2(L3)(2).CH2 Cl-2] (3) (H (2) L3 = (6,6(')-(((2-(diethylamino)ethyl)azanediyl)bis(methylene)) bis(methylene))bis(2,4-dimethylphenol) were synthesized by using three symmetrical tetradendate ligands containing N2O2 donor sites. These complexes are characterized by a variety of techniques including; elemental analysis, mass spectrometry, H-1, C-13 NMR spectroscopic and single crystal X-ray analysis. The new complexes have been tested for the phosphotriesterase (PTE) activity with the help of P-31 NMR spectroscopy. The P-31 NMR studies show that mononuclear complex Zn(L1)(H2O)].CH3OH.H2O (1) can hydrolyse the phosphotriester i.e., p-nitrophenyl diphenylphosphate (PNPDPP), more efficiently than the binuclear complexes Zn-2(L2)(2)] (2) and Cu-2(L3)(2).CH2Cl2] (3). The mononuclear Zn(II) complex (1) having one coordinated water molecule exhibits significant PTE activity which may be due to the generation of a Zn(II)-bound hydroxide ion during the hydrolysis reactions in CHES buffer at pH 9.0.

Cu-II-azide polynuclear complexes of Cu-4 building clusters with Schiff-base co-ligands: synthesis, structures, magnetic behavior and DFT studies

Three new copper-azido complexes Cu-4(N-3)(8)(L-1)(2)](n) (1), Cu-4(N-3)(6)(L-2)(2)(H2O)(2)] (2), and Cu-4(N-3)(6)(L-3)(2)](n) (3) L-1 is the imine resulting from the condensation of pyridine-2-carboxaldehyde with N-methylethylenediamine, HL2 and HL3 are the condensation products of 2-hydroxy-3-methoxybenzaldehyde with N,N-diethylethylenediamine and N-ethylethylenediamine respectively] have been synthesized by using 0.5 molar equivalents of the Schiff base ligands with Cu(NO3)(2)center dot 3H(2)O and an excess of NaN3. Single crystal X-ray structures show that the basic unit of these complexes contains very similar Cu-4(II) building blocks. While 1 and 3 have overall 1D structures, 2 forms discrete tetranuclear clusters due to blocking of two coordination sites on the tetranuclear cluster by water molecules. Magnetic susceptibility measurements over a wide range of temperatures exhibit the presence of both antiferromagnetic and ferromagnetic exchanges within the tetranuclear unit structures. Density functional theory calculations (using B3LYP functional and two different basis sets) have been performed on the complexes 1-3 to provide a qualitative theoretical interpretation of their overall magnetic behavior.

Microwave Spectroscopic and Atoms in Molecules Theoretical Investigations on the ArPropargyl Alcohol Complex: ArHO, Ar, and ArC Interactions

The structure of the Arpropargyl alcohol (ArPA) complex is determined from the rotational spectra of the parent complex and its two deuterated isotopologues, namely ArPA-D(OD) and ArPA-D(CD). The spectra confirm a geometry in which PA exists in the gauche form with Ar located in between OH and CCH groups. All a, b and c types of transitions show small splitting due to some large-amplitude motion dominated by COH torsion, as in the monomer. Splittings in a- and b-type transitions are of the order of a few kilohertz, whereas splitting in the c-type transitions is relatively larger (0.92.6 MHz) and decreases in the order ArPA>ArPA-D(CD)>ArPA-D(OD). The assignments are well supported by ab initio calculations. Atoms in molecules (AIM) and electrostatic potential calculations are used to explore the nature of the interactions in this complex. AIM calculations not only reveal the expected OHAr and Ar interactions in the Argauche-PA complex, but also novel CAr (of CH2OH group) and OHAr interactions in the Artrans-PA complex. Similar interactions are also present in the Armethanol complex.

Fine scale characterization of surface/subsurface and nanosized debris particles on worn Cu-10 % Pb nanocomposites

The identification of the damage mechanisms involved in the wear process demands the finer scale characterization of the surface, as well as the subsurface region of the wear scar region, and to this end, this article discusses the results obtained with Cu-10 wt% Pb-based metallic nanocomposites using a host of characterization techniques, including transmission electron microscopy and ion milling microscopy. Apart from finer scale characterization to understand deformation and cracking during the wear process, X-ray photoelectron spectroscopy analysis of wear debris confirms the occurrence of oxidation of Pb phase to Pb3O4. In order to understand the role of oxides on friction and wear, sliding wear tests in argon were also carried out and such tests did not result in the formation of any tribo-oxides, as confirmed using electron probe microanalysis. Conclusively, oxidative wear is attributed as the dominant wear mechanism in ambient conditions for Cu-10 wt% Pb composite.

Densification kinetics, phase assemblage and hardness of spark plasma sintered Cu-10 wt% TiB2 and Cu-10 wt% TiB2-10 wt% Pb composites

The present work demonstrates the synthesis of Cu-10 wt% TiB2 composites with a theoretical density of more than 90% by tailoring the spark plasma sintering (SPS) conditions in the temperature range of 400-700 degrees C. Interestingly, 10 wt% Pb addition to Cu-10 wt% TiB2 lowers the sinter density and the difference in the densification behavior of the investigated compositions was discussed in reference to the current profile recorded during a SPS cycle. The sintering kinetics and phase assemblage were also discussed in reference to surface melting of the constituents prior to bulk melting temperature, temperature dependent wettability of Pb on Cu, diffusion kinetics of Cu as well as the formation of various oxides. An important result is that a high hardness of around 2 GPa and relative density close to 92% qtheoretical was achieved for the Cu-10 wt% TiB2-10 wt% Pb composite, and such a combination has never been achieved before using any conventional processing route.

Exploring the color of transition metal ions in irregular coordination geometries: new colored inorganic oxides based on the spiroffite structure, Zn2-xMxTe3O8 (M = Co, Ni, Cu)

We describe the synthesis, crystal structures, and optical absorption spectra of transition metal substituted spiroffite derivatives, Zn2-xMxTe3O8 (M-II = Co, Ni, Cu; 0 < x <= 1.0). The oxides are readily synthesized by solid state reaction of stoichiometric mixtures of the constituent binaries at 620 degrees C. Reitveld refinement of the crystal structures from powder X-ray diffraction (XRD) data shows that the Zn/MO6 octahedra are strongly distorted, as in the parent Zn2Te3O8 structure, consisting of five relatively short Zn/M-II-O bonds (1.898-2.236 angstrom) and one longer Zn/M-II-O bond (2.356-2.519 angstrom). We have interpreted the unique colors and the optical absorption/diffuse reflectance spectra of Zn2-xMxTe3O8 in the visible, in terms of the observed/irregular coordination geometry of the Zn/M-II-O chromophores. We could not however prepare the fully substituted M2Te3O8 (M-II = Co, Ni, Cu) by the direct solid state reaction method. Density Functional Theory (DFT) modeling of the electronic structure of both the parent and the transition metal substituted derivatives provides new insights into the bonding and the role of transition metals toward the origin of color in these materials. We believe that transition metal substituted spiroffites Zn2-xMxTe3O8 reported here suggest new directions for the development of colored inorganic materials/pigments featuring irregular/distorted oxygen coordination polyhedra around transition metal ions.

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.

Room-temperature anelasticity and viscoplasticity of Cu-Zr bulk metallic glasses evaluated using nanoindentation

Anelastic and viscoplastic characteristics of Cu50Zr50 and Cu65Zr35 binary bulk metallic glasses at room temperature were examined through nanoindentation creep experiments. Results show that both the deformations are relatively more pronounced in Cu50Zr50 than in Cu65Zr35, and their amount increases with the loading rate. The results are analyzed in terms of the influences of structural defects and loading rate on the room temperature indentation creep.

Experimental study of phase equilibria in the system Cu-Al-Sn

Phase equilibria in the Cu-rich corner of the ternary system Cu-Al-Sn have been re-investigated. Final equilibrium microstructures of 20 ternary alloy compositions near Cu3Al were used to refine the ternary phase diagram. The microstructures were characterized using optical microscopy (OM), x-ray diffraction (XRD), electron probe microanalysis and transmission electron microscopy. Isothermal sections at 853, 845, 833, 818, 808, 803 and 773 K have been composed. Vertical sections have been drawn at 2 and 3 at% Sn, showing beta(1) as a stable phase. Three-phase fields (alpha + beta + beta(1)) and (beta + beta(1) + gamma(1)) result from beta -> alpha + beta(1) eutectoid and beta + gamma(1) -> beta(1) peritectoid reactions forming metastable beta(1) in the binary Cu-Al. With the lowering of temperature from 853 to 818 K, these three-phase fields are shifted to lower Sn concentrations, with simultaneous shrinkage and shifting of (beta + beta(1)) two-phase field. The three-phase field (alpha + beta + gamma(1)) resulting from the binary reaction beta -> alpha + gamma(1) shifts to higher Sn contents, with associated shrinkage of the beta field, with decreasing temperature. With further reduction of temperature, a new ternary invariant reaction beta + beta(1) -> alpha + gamma(1) is observed at similar to 813 K. The beta disappears completely at 803 K, giving rise to the three-phase field (alpha + beta(1) + gamma(1)). Some general guidelines on the role of ternary additions (M) on the stability of the ordered beta(1) phase are obtained by comparing the results of this study with data in the literature on other systems in the systems group Cu-Al-M.