Texture and microstructure evolution during cold rolling of Cu-Fe laminates prepared by accumulative roll bonding

Multi-layered materials have been made from Cu-Fe with approximately equal volume fractions using the Accumulated Roll Bonding (ARB) technique with less than 1 μm thickness of the individual layers. The so-obtained multi-layers have been subjected to deformation by cold rolling to 25, 50, 75, 87 and 93% reduction in thickness. A detailed characterization has been carried out using X-ray diffraction (line profile analysis and texture measurement) and electron (scanning and transmission) microscopy. It has been found that Fe layers are disintegrated whereas Cu retains its continuity within a layer. Microstructural Characterization from X-Ray Line profile Analysis (XRDLPA) through Variance Method reveals that large amount of strain is initially carried by Cu layers during deformation. In the Cu-Fe layer, the texture is comparatively weaker in Cu layer and strong in Fe layers. Brass Component increases up to 75% reduction and then decreases, while the ratio of Cu/S and Bs/S remains almost constant through out the deformation. After 50% reduction, dynamic recovery is predominant as indicated by the increase in the amount of low angle grain boundaries and decrease in dislocation density. The presence of R component indicates continuous dynamic recovery and recrystallization (CDRR) at the advanced stage of deformation.

1-D Hydrogen bonded water in Cu(II)-picolinate coordination polymer: synthesis, crystal structure, and thermogravimetric analysis

A new Cu(II)-picolinate complex was synthesized and characterized by single crystal X-ray crystallography. The complex crystallizes in the centrosymmetric triclinic space group P (1) over bar (no. 2). Picolinate in the complex extends the neutral unit into a 1-D chain through mu(2)-bridging carboxylate. The complex has a hydrogen bonding acceptor in the second coordination sphere allowing lattice water to assemble neighboring chains. Water self-assembles to form a zig-zag 1-D chain. The adjacent chains are assembled by C-H center dot center dot center dot O interactions result in the formation 2-D hydrogen bonded network. The overall hydrogen bonding between water chain and Cu-picolinate network yields a 3-D hydrogen bonded coordination network. X-ray structural analysis, FTIR and thermal analysis have been used to characterize the reported compound in the solid state.

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.

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(In,Al)Se-2 thin films by one-step electrodeposition for photovoltaics

Chalcopyrite Cu(In,Al)Se-2 (CIAS) thin films are grown on stainless steel substrate through one-step electrodeposition at room temperature. Indium is partially replaced with aluminum to increase the band gap of CuInSe2 without creating significant change in the original structure. The deposition potential is optimized at -0.8 V (vs. SCE) and annealing of the films is performed in vacuum to remove binary phases present in the as-deposited films. In/Al ratio is varied from 1/9 to 8/2, to find the suitability for solar cell fabrication. For In/Al ratio of less than 8/2, CuAlSe2 phase is formed in the film in addition to the CIAS phase. Depth profile X-ray photoelectron spectroscopy analysis of the CIAS sample prepared with In/Al ratio of 8/2 in the precursor solution confirmed the existence of single phase CIAS throughout the film. This film showed p-type conductivity while the rest of the samples with In/Al ratio less than 8/2 showed n-type conductivity. The band gap of the film varied from 1.06 to 1.45 eV, with variation in deposition potential. Structural, optical, morphological, compositional and electrical characterizations are carried out to establish the suitability of this film for solar cell fabrication. (C) 2013 Elsevier B.V. All rights reserved.

Incorporation of Interfacial Intermetallic Morphology in Fracture Mechanism Map for Sn-Ag-Cu Solder Joints

A fracture mechanism map (FMM) is a powerful tool which correlates the fracture behavior of a material to its microstructural characteristics in an explicit and convenient way. In the FMM for solder joints, an effective thickness of the interfacial intermetallic compound (IMC) layer (t (eff)) and the solder yield strength (sigma (ys,eff)) are used as abscissa and ordinate axes, respectively, as these two predominantly affect the fracture behavior of solder joints. Earlier, a definition of t (eff), based on the uniform thickness of IMC (t (u)) and the average height of the IMC scallops (t (s)), was proposed and shown to aptly explain the fracture behavior of solder joints on Cu. This paper presents a more general definition of t (eff) that is more widely applicable to a range of metallizations, including Cu and electroless nickel immersion gold (ENIG). Using this new definition of t (eff), mode I FMM for SAC387/Cu joints has been updated and its validity was confirmed. A preliminary FMM for SAC387/Cu joints with ENIG metallization is also presented.

Numerical study of the impact of inoculant and grain transport on macrosegregation and microstructure formation during solidification of an Al-22%Cu alloy

We investigate the impact of the nucleation law for nucleation on Al-Ti-B inoculant particles, of the motion of inoculant particles and of the motion of grains on the predicted macrosegregation and microstructure in a grain-refined Al-22 wt.% Cu alloy casting. We conduct the study by numerical simulations of a casting experiment in a side-cooled 76×76×254 mm sand mould. Macrosegregation and microstructure formation are studied with a volume-averaged two-phase model accounting for macroscopic heat and solute transport, melt convection, and transport of inoculant particles and equiaxed grains. On the microscopic scale it accounts for nucleation on inoculant particles with a given size distribution (and corresponding activation undercooling distribution)and for the growth of globular solid grains. The growth kinetics is described by accounting for limited solute diffusion in both liquid and solid phases and for convective effects. We show that the consideration of a size distribution of the inoculants has a strong impact on the microstructure(final grain size) prediction. The transport of inoculants significantly increases the microstructure heterogeneities and the grain motion refines the microstructure and reduces the microstructure heterogeneities.

Effects of Microstructure and Loading on Fracture of Sn-3.8Ag-0.7Cu Joints on Cu Substrates with ENIG Surface Finish

When dropped, electronic packages often undergo failure by propagation of an interfacial crack in solder joints under a combination of tensile and shear loading. Hence, it is crucial to understand and predict the fracture behavior of solder joints under mixed-mode high-rate loading conditions. In this work, the effects of the loading conditions (strain rate and loading angle) and microstructure interfacial intermetallic compound (IMC) morphology and solder yield strength] on the mixed-mode fracture toughness of Sn-3.8 wt.%Ag-0.7 wt.%Cu solder joints sandwiched between two Cu substrates with electroless nickel immersion gold (ENIG) metallization have been studied, and compared with the fracture behavior of joints attached to bare Cu. Irrespective of the surface finish, the fracture toughness of the solder joints decreased monotonically with strain rate and mode-mixity, both resulting in increased fracture proportion through the interfacial IMC layer. Furthermore, the proportion of crack propagation through the interfacial IMC layer increased with increase in the thickness and the roughness of the interfacial IMC layer and the yield strength of the solder, resulting in a decrease in the fracture toughness of the joint. However, under most conditions, solder joints with ENIG finish showed higher resistance to fracture than joints attached directly to Cu substrates without ENIG metallization. Based on the experimental observations, a fracture mechanism map is constructed correlating the yield strength of the solder, the morphology and thickness of the interfacial IMC, and the fracture mechanisms as well as the fracture toughness values for different solder joints under mode I loading.

Synthesis, X-ray structure and in vitro cytotoxicity studies of Cu(I/II) complexes of thiosemicarbazone: special emphasis on their interactions with DNA

4-(p-X-phenyl)thiosemicarbazone of napthaldehyde {where X = Cl (HL1) and X = Br (HL2)}, thiosemicarbazone of quinoline-2-carbaldehyde (HL3) and 4-(p-fluorophenyl) thiosemicarbazone of salicylaldehyde (H2L4) and their copper(I) {Cu(HL1)(PPh3)(2)Br]center dot CH3CN (1) and Cu(HL2)(PPh3)(2)Cl]center dot DMSO (2)} and copper(II) {((Cu2L2Cl)-Cl-3)(2)(mu-Cl)(2)]center dot 2H(2)O (3) and Cu(L-4)(Py)] (4)} complexes are reported herein. The synthesized ligands and their copper complexes were successfully characterized by elemental analysis, cyclic voltammetry, NMR, ESI-MS, IR and UV-Vis spectroscopy. Molecular structures of all the Cu(I) and Cu(II) complexes have been determined by X-ray crystallography. All the complexes (1-4) were tested for their ability to exhibit DNA-binding and - cleavage activity. The complexes effectively interact with CT-DNA possibly by groove binding mode, with binding constants ranging from 10(4) to 10(5) M-1. Among the complexes, 3 shows the highest chemical (60%) as well as photo-induced (80%) DNA cleavage activity against pUC19 DNA. Finally, the in vitro antiproliferative activity of all the complexes was assayed against the HeLa cell line. Some of the complexes have proved to be as active as the clinical referred drugs, and the greater potency of 3 may be correlated with its aqueous solubility and the presence of the quinonoidal group in the thiosemicarbazone ligand coordinated to the metal.

Influence of deposition time on the properties of electrodeposited Cu(In,Al)Se-2 thin films

Cu(In,Al)Se-2 films are grown using single step electrodeposition technique. The film properties are studied by varying the deposition time from 500 to 2000 s. Peaks corresponding to elemental Se and Cu2Se phase started appearing from 1200 s of deposition. The composition is changed significantly after 1500 S. Se concentration increased from 57 to 68% with the increase in the deposition time. The Cu2Se phase is dominant in the films deposited for a duration of 2000 s and the grain size increased from 1.12 to 2.15 mu m in this film. Raman analysis confirmed the presence of Se and Cu2Se phase in C1200. In C1500 and C2000 the spectra showed prominent mode corresponding to Cu2Se. The thickness of the film increased from 0.85 to 2.3 mu m with the increase in the deposition time. All the films showed p-type conductivity and resistivity reduced with increased thickness. (C) 2015 Elsevier Ltd. All rights reserved.