Effect of isothermal aging and electromigration on the microstructural evolution of solder interconnections during thermomechanical loading

The effect of different pre-aging treatments on the microstructural evolution of lead-free solder and growth of interfacial intermetallic compound layers under thermal cycling has been investigated in this work. The results show that there are distinct differences in the microstructural changes between samples with no pretreatment, samples that have experienced thermal annealing at 125A degrees C for 750 h before thermal cycling, and those that have had direct current (DC) stressing for 750 h as pretreatment. The microstructural evolution of the solder matrix is rationalized by utilizing the science of microstructures and analysis of the influence of electron flow on the precipitation phenomena. The finite-element method is utilized to understand the loading conditions imposed on the solder interconnections during cyclic stressing. The growth of intermetallic reaction layers is further analyzed by utilizing quantitative thermodynamic calculations coupled with kinetic analysis. The latter is based on the changes in the intrinsic diffusion fluxes of elements induced by current flow and alloying elements present in the system. With this concurrent approach the differences seen in thermal cycling behavior between the different pre-aging treatments can be explained.

Indentation size effect and shear transformation zone size in a bulk metallic glass in two different structural states

The existence of an indentation size effect (ISE) in the onset of yield in a Zr-based bulk metallic glass (BMG) is investigated by employing spherical-tip nanoindentation experiments. Statistically significant data on the load at which the first pop-in in the displacement occurs were obtained for three different tip radii and in two different structural states (as-cast and structurally relaxed) of the BMG. Hertzian contact mechanics were employed to convert the pop-in loads to the maximum shear stress underneath the indenter. Results establish the existence of an ISE in the BMG of both structural states, with shear yield stress increasing with decreasing tip radius. Structural relaxation was found to increase the yield stress and decrease the variability in the data, indicating ``structural homogenization'' with annealing. Statistical analysis of the data was employed to estimate the shear transformation zone (STZ) size. Results of this analysis indicate an STZ size of similar to 25 atoms, which increases to similar to 34 atoms upon annealing. These observations are discussed in terms of internal structure changes that occur during structural relaxation and their interaction with the stressed volumes in spherical indentation of a metallic glass. (C) 2012 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Influence of annealing temperature on Raman and photoluminescence spectra of electron beam evaporated TiO2 thin films

Titanium dioxide (TiO2) thin films were deposited on fused quartz substrates by electron beam evaporation method at room temperature. The films were annealed at different temperatures in ambient air. The surface morphology/roughness at different annealing temperatures were analyzed by atomic force microscopy (AFM). The crystallinity of the film has improved with the increase of annealing temperature. The effect of annealing temperature on optical, photoluminescence and Raman spectra of TiO2 films were investigated. The refractive index of TiO2 films were studied by envelope method and reflectance spectra and it is observed that the refractive index of the films was high. The photoluminescence intensity corresponding to green emission was enhanced with increase of annealing temperature. The peaks in Raman spectra depicts that the TiO2 film is of anatase phase after annealing at 300 degrees C and higher. The films show high refractive index, good optical quality and photoluminescence characteristics suggest that possible usage in opto-electronic and optical coating applications. (C) 2012 Elsevier B.V. All rights reserved.

Influence of annealing on structural, morphological, compositional and surface properties of magnetron sputtered nickel-titanium thin films

Thin films of NiTi were deposited by DC magnetron sputtering from an equiatomic alloy target (Ni/Ti: 50/50 at.%). The films were deposited without intentional heating of the substrates. The thickness of the deposited films was approximately 2 mu m. The structure and morphology of NiTi films annealed at different temperatures were analyzed in order to understand the effect of annealing on physical properties of the films. The compositional investigations of fresh and annealed films were also evaluated by energy dispersive X-ray spectroscopy (EDS) and X-ray photo-electron spectroscopy (XPS) techniques. X-ray diffraction (XRD) studies showed that as-deposited films were amorphous in nature whereas annealed films were found to poly-crystalline with the presence of Austenite phase as the dominant phase. AFM investigations showed higher grain size and surface roughness values in the annealed films. In annealed films, the grain size and film roughness values were increased from 10 to 85 nm and 2-18 nm. Film composition measured by EDS were found to 52.5 atomic percent of Ni and 47.5 atomic percent of Ti. XPS investigations, demonstrated the presence of Ni content on the surface of the films, in fresh films, whereas annealed films did not show any nickel. From HR-XPS investigations, it can be concluded that annealed NiTi films have higher tendency to form metal oxide (titanium dioxide) layer on the surface of the films than fresh NiTi films. (C) 2013 Elsevier B. V. All rights reserved.

Investigating thermal stability of structural defects and its effect on d(0) ferromagnetism in undoped SnO2

The effect of annealing on structural defects and d(0) ferromagnetism in SnO2 nanoparticles prepared by solution combustion method is investigated. The as-synthesized SnO2 nanoparticles were annealed at 400-800 degrees C for 2 h, in ambient conditions. The crystallinity, size, and morphology of the samples were studied using x-ray diffraction and transmission electron microscopy studies. The annealing results in grain growth due to coarsening as well as reduction in oxygen vacancies as confirmed by Raman spectroscopy, photoluminescence spectroscopy, and x-ray photoelectron spectroscopy. All the as synthesized and annealed samples exhibit room temperature ferromagnetism (RTFM) with distinct hysteresis loops and the saturation magnetization as high as similar to 0.02 emu/g in as-synthesized samples. However, the saturation magnetization is drastically reduced with increasing annealing temperature. Further the presence of singly charged oxygen vacancies (V-o(-) signal at g-value 1.99) is confirmed by electron paramagnetic resonance studies, which also diminish with increasing annealing temperature. The observed diminishing RTFM and simultaneous evidences of diminishing O vacancies clearly indicate that RTFM is driven by defects in oxide lattice and confirms primary role of oxygen vacancies in inducing ferromagnetic ordering in metal oxide semiconductors. The study also provides improved fundamental understanding regarding the ambiguity in the origin of intrinsic RTFM in semiconducting metal oxides and projects their technological application in the field of spintronics. (C) 2013 AIP Publishing LLC.

Post-deposition annealing influenced structural and electrical properties of Al/TiO2/Si gate capacitors

Titanium dioxide (TiO2) thin films are deposited on unheated p-Si (100) and quartz substrates by employing DC reactive magnetron sputtering technique. The effect of post-deposition annealing in air at temperatures in the range 673-973 K on the structural, electrical, and dielectric properties of the films was investigated. The chemical composition of the TiO2 films was analyzed with X-ray photoelectron spectroscopy. The surface morphology of the films was studied by atomic force microscope. The optical band gap of the as-deposited film was 3.50 eV, and it increased to 3.55 eV with the increase in annealing temperature to 773 K. The films annealed at higher temperature of 973 K showed the optical band gap of 3.43 eV. Thin film capacitors were fabricated with the MOS configuration of Al/TiO2/p-Si. The leakage current density of the as-deposited films was 1.2 x 10(-6) A/cm(2), and it decreased to 5.9 x 10(-9) A/cm(2) with the increase in annealing temperature to 973 K. These films showed high dielectric constant value of 36. (C) 2013 Elsevier Ltd. All rights reserved.

Effect of low oxygen pressure on structural and magnetic properties of quenched SrFe12O19 thin films

Strontium hexaferrite thin films have been grown on glass substrates at room temperature in oxygen environment by pulsed laser deposition method. The effect of oxygen pressure (p(o2)) on the structural and magnetic properties has been investigated. The as-deposited films were found to be amorphous in nature. The crystallization of these films was achieved by annealing at a temperature of 850 A degrees C in air. The thickness of the film increased with p(o2). The film grown at p(o2) = 0.455 Pa had a clear hexagonal structure. The values of coercivity for the films were found to increase with p(o2).

The effect of multisubstitution on the thermoelectric properties of chalcogenide-based Cu2.1Zn0.9Sn1-xInxSe4 (0 <= x <= 0.1)

Quinary chalcogenide compounds Cu2.1Zn0.9Sn1-xInxSe4 (0 <= x <= 0.1) were prepared by melting (1170K) followed by annealing (773 K) for 172 h. Powder X-ray diffraction (XRD) data accompanied by electron probe microanalysis (EPMA) and Raman spectra of all the samples confirmed the formation of a tetragonal kesterite structure with Cu2FeSnS4-type. The thermoelectric properties of all the samples were measured as a function of temperature in the range of 300-780K. The electrical resistivity of all the samples exhibits metallic-like behavior. The positive values of the Seebeck coefficient and the Hall coefficient reveal that holes are the majority charge carriers. The codoping of copper and indium leads to a significant increase of the electrical resistivity and the Seebeck coefficient as a function of temperature above 650 K. The thermal conductivity of all the samples decreases with increasing temperature. Lattice thermal conductivity is not significantly modified as the doping content may infer negligible mass fluctuation scattering for copper/zinc and indium/tin substitution. Even though, the power factors (S-2/rho) of indium-doped samples Cu2.1Zn0.9Sn1-xInxSe4 (x = 0.05, 0.075) are almost the same, the maximum zT = 0.45 at 773K was obtained for Cu2.1Zn0.9Sn0.925In0.075Se4 due to its smaller value of thermal conductivity. (C) 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim

Process induced electroactive beta-polymorph in PVDF: effect on dielectric and ferroelectric properties

The effects of various processing conditions, like annealing, poling, mechanical rolling and their combinations, on the dielectric and ferroelectric properties of PVDF poly(vinylidene fluoride)] were systematically studied in this work. Further, the effect of processing sequence on the structure and properties was investigated. While all the processing conditions adopted here resulted in phase transformation of the alpha- to electroactive beta-polymorph in PVDF, the fraction of beta-phase developed was observed to be strongly contingent on the adopted process. The transformation of alpha- to electroactive beta-polymorph was determined by X-ray diffraction and FTIR. The neat PVDF showed only beta-phase, whereas mechanically rolled samples exhibited the highest ca. 85% beta-phase in PVDF. Both the permittivity and the loss tangent decreased in the samples which had undergone different processing conditions. The polarization-electric field (P-E) loops for all the samples were evaluated. Interestingly, the energy density, estimated from the electrical displacement-electric field (D-E) loops, was observed to be highest for the poled samples which were initially rolled. The results indicate that various processing conditions can influence the dielectric and the ferroelectric properties differently.

Effect of High-Pressure Torsion on Texture, Microstructure, and Raman Spectroscopy: Case Study of Fe- and Te-Substituted CoSb3

Fe0.05Co0.95Sb2.875Te0.125, a double-element-substituted skutterudite, was prepared by induction melting, annealing, and hot pressing (HP). The hot-pressed sample was subjected to high-pressure torsion (HPT) with 4 GPa pressure at 673 K. X-ray diffraction was performed before and after HPT processing of the sample; the skutterudite phase was observed as a main phase, but an additional impurity phase (CoSb2) was observed in the HPT-processed sample. Surface morphology was determined by high-resolution scanning electron microscopy. In the HP sample, coarse grains with sizes in the range of approximately 100 nm to 300 nm were obtained. They changed to fine grains with a reduction in grain size to 75 nm to 125 nm after HPT due to severe plastic deformation. Crystallographic texture, as measured by x-ray diffraction, indicated strengthening of (112), (102) poles and weakening of the (123) pole of the HPT-processed sample. Raman-active vibrational modes showed a peak position shift towards the lower energy side, indicating softening of the modes after HPT. The distortion of the rectangular Sb-Sb rings leads to broadening of Sb-Sb vibrational modes due to local strain fluctuation. In the HPT process, a significant effect on the shorter Sb-Sb bond was observed as compared with the longer Sb-Sb bond.

Effect of radio frequency power and thickness on the electrochemical properties of Li2-x MnO3-y thin films

In the present work, Li2-x MnO3-y (LMO) thin films have been deposited by radio frequency (RF) reactive magnetron sputtering using acid-treated Li2MnO3 powder target. Systematic investigations have been carried out to study the effect of RF power on the physicochemical properties of LMO thin films deposited on platinized silicon substrates. X-ray diffraction, electron microscopy, surface chemical analysis and electrochemical studies were carried out for the LMO films after post deposition annealing treatment at 500 A degrees C for 1 h in air ambience. Galvanostatic charge discharge studies carried out using the LMO thin film electrodes, delivered a highest discharge capacity of 139 mu Ah mu m(-1) cm(-2) in the potential window 2.0-3.5 V vs. Li/Li+ at 100 W RF power and lowest discharge capacity of 80 mu Ah mu m(-1) cm(-2) at 75 W RF power. Thereafter, the physicochemical properties of LMO films deposited using optimized RF power 100 W on stainless steel substrates has been studied in the thickness range of 70 to 300 nm as a case study. From the galvanostatic charge discharge experiments, a stable discharge capacity of 68 mu Ah mu m(-1) cm(-2) was achieved in the potential window 2.0-4.2 V vs. Li/Li+ tested up to 30 cycles. As the thickness increased, the specific discharge capacity started reducing with higher magnitude of capacity fading.

Effect of sputtering parameters on the structure, microstructure and magnetic properties of Tb-Fe films

The effect of sputtering parameters such as gas pressure and power on the structure, microstructure and magnetic properties of sputtered Tb-Fe thin films was investigated. X-ray diffraction and transmission electron microscopy studies showed that all the films were amorphous in nature irrespective of the sputtering parameters. A fine island kind of morphology was observed at low sputtering power whereas large clusters were seen at higher sputtering power. While the composition of Tb-Fe films remained constant with increasing sputtering power, the magnetic behaviour was found to change from superparamagnetic to ferromagnetic. On the other hand, the increase in argon gas pressure was found to deplete the iron concentration in Tb-Fe thin films, which in turn reduced the anisotropy and Curie temperature. Annealing of the films at 773 K did not result in any crystallization and the magnetic properties were also found to remain unchanged. (C) 2015 Elsevier B.V. All rights reserved.

Effect of processing route on phase stability in equiatomic multicomponent Ti20Fe20Ni20Co20Cu20 high entropy alloy

The evolution of microstructure and phase formation in equiatomic Ti20Fe20Ni20Co20Cu20 high entropy alloy synthesised by conventional arc melting followed with suction casting and ball milling with spark plasma sintering route is distinctly different. The cast microstructure exhibits one body centre cubic and two face centre cubic high entropy phases based on titanium, cobalt and copper respectively along with a eutectic containing Ti2Ni type Laves phase. On the contrary, spinodal decomposed microstructure consisting of cobalt and copper solid solution is obtained in the sintered sample. However, long term annealing of cast sample at 950 degrees C reveals a eutectoid transformation with different phases than the cast sample. The aforementioned observations are discussed using CALPHAD thermodynamical approach and available literature.

Evolution of annealing texture in cryo-rolled copper

The present study addresses the evolution of texture and microstructure during annealing in a cryorolled copper. Transition from copper to brass texture during the cryo-rolling has been illustrated. Twinning and interaction between twins and shear bands have been found to play the important role in grain refinement and strengthening. The low temperature vacancy clustering and its effect on the recrystallization have been experimentally demonstrated. Fine scale twinning, and grain refinement have been attributed to the higher yield strength found in the case of samples subjected to cryo-rolling. (C) 2015 Elsevier B.V. All rights reserved.

Effect of semi-solid heat treatment on elevated temperature plasticity of 304L stainless steel

The present work explores the potential of semi-solid heat treatment technique by elucidating its effect on the plastic behavior of 304L SS in hot working domain. To accomplish this objective, hot isothermal compression tests on 304L SS specimens with semi-solid heat treatment and conventional annealing heat treatment have been carried out within a temperature range of 1273-1473 K and strain rates ranging from 0.01 to 1 s(-1). The dynamic flow behavior of this steel in its conventional heat-treated condition and semi-solid heat-treated condition has been characterized in terms of strain hardening, temperature softening, strain rate hardening, and dynamic flow softening. Extensive microstructural investigation has been carried out to corroborate the results obtained from the analysis of flow behavior. Detailed analysis of the results demonstrates that semi-solid heat treatment moderates work hardening, strain rate hardening, and temperature sensitivity of 304L SS, which is favorable for hot deformation. The post-deformation hardness values of semi-solid heat-treated steel and conventionally heat-treated steel were found to remain similar despite the pre-deformation heat treatment conditions. The results obtained demonstrate the potential of semi-solid heat treatment as a pre-deformation heat treatment step to effectively reduce the strength of the material to facilitate easier deformation without affecting the post-deformation properties of the steel.