Microstructure and thermostability of a W–Cu nanocomposite produced via high-pressure torsion

A coarse-grained W–25% Cu alloy is subjected to high-pressure torsion (HPT) at room temperature to different strains. Evolution of the microstructure during HPT processing is studied using X-ray diffraction analysis, scanning and transmission electron microscopy. It is demonstrated that HPT processing results in fragmentation of the tungsten particles and the formation of a 5–15?nm grain size nanostructure at equivalent strains of ≥256 (saturation). It is shown that the nanostructured W–25% Cu is thermostable up to 500°C, with grain growth up to 50?nm at 720°C. During HPT processing, the lattice parameter of the copper and tungsten was found to increase and decrease, respectively, with increased level of equivalent strain. This is proposed to occur through the interdiffusion of copper atoms into tungsten grains and tungsten atoms into copper grains, as suggested by energy-dispersive X-ray analysis of the individual grains. The formation of a limited solid solution is considered and possible mechanisms for this effect discussed.     

EBSD FEG-SEM, TEM and XRD techniques applied to grain study of a commercially pure 1200 aluminum subjected to equal-channel angular-pressing

Microstructural evolution due to equal-channel angular-pressing (ECAP) with increasingly severe deformation was investigated in a commercially pure 1200 aluminum alloy. A true strain of eight produced sub-micrometer scale grains and very fine subgrains in the grain interior. The deformation process was documented and described using field-emission (FEG) gun scanning and transmission electron microscopy techniques. After eight ECAP passes, the high-angle grain boundaries accounted for approximately 70% of all boundaries. The fine spacing resolution of FEG scanning electron microscopy allowed detailed grain and subgrain statistical evaluation in the deformed microstructure; transmission electron microscopic inspection afforded appreciation of the role of very low-angle misorientation boundaries in the microstructure-refining process. ECAP results were compared with those produced by cold rolling. The material's texture evolved in a decreasing trend of Cube {001}100 intensities in favor of Cube rotated toward the normal-to-pressing direction {001}120, while Goss {110}001 and {111}110, {111}112 directions slightly increased with strain.     

Partial recrystallization in the nugget zone of friction stir welded dual-phase Cu–Zn alloy

For single and quasi-single phase metallic materials, complete dynamic recrystallization has been observed in the nugget zones (NZs) of friction stir welds (FSWs), producing fine and uniform equiaxed grains. In this study, partial dynamic recrystallization was observed in the NZ of 5 mm thick friction stir welded brass plates. Whereas the top and the advancing side of the NZ were characterized by fine completely-recrystallized grains, the remaining region consisted of coarse non-recrystallized deformed grains, annealed recrystallized grains and deformed recrystallized grains. The occurrence of partial recrystallization was attributed to the inhibiting effect of a high volume fraction of fine β′-phase particles. Increasing the FSW passes reduced the fraction and size of non-recrystallized deformed grains, but could not eliminate the partially recrystallized zone completely.     

Structure and orientation of an intermetallic phase in a W-Ni-Co alloy

The aim of this investigation is crystal structure determination of an intermetallic phase formed in a W-Ni-Co alloy during a heat-treatment carried out at a temperature of 800°C. This intermetallic phase is expected to play a critical role on the final microstructure (fine tungsten particles in an FCC matrix that is present in between large tungsten grains) and thereby, on the properties of the alloy. 92W-5.3Ni-2.7Co alloy was prepared through powder metallurgy route (liquid phase sintering) followed by heat-treatment at 800°C for 5?h. The intermetallic phase formed at this temperature was characterised using transmission and scanning electron microscopes. The intermetallic phase was found to have orthorhombic crystal structure with Pnam (62) space group as determined using automated diffraction tomography along with precession electron diffraction. Chemical analysis in TEM suggested that the intermetallic phase is based on stoichiometry (Co,Ni)₂W. Orientation imaging of the phase was also carried out in TEM and EBSD to understand its evolution. Equiaxed or lath morphology of the intermetallic phase was found to depend on the crystallographic orientation relationship of the phase with the tungsten grains and the matrix phase.     

Influence of Annealing Temperature on the Microstructure and Morphology of TiN Films Synthesized by Dual Magnetron Sputtering

TiN films synthesized on leucosapphire substrates by dual magnetron sputtering have been annealed in vacuum at 600, 700, 800, and 900°C for 2 min. The microstructure and morphology of the films have been studied by X-ray diffraction and scanning electron microscopy at different temperatures. It has been found that annealing changes the microstructure, texture, grain size, and surface roughness of the TiN films.     

The Migration of High Angle Grain Boundaries during Recrystallization

When plastically deformed metallic materials are annealed, new strain free grains emerge from the microstructure and grow by means of grain boundary migration until the deformation microstructure is eliminated. This process is called recrystallization. In this paper the various methods by which grain boundary migration rates are measured stereologically in order to characterize the growth process are described and compared using illustrations from recrystallization experiments on commercial AA1050 aluminum. It seems abundantly clear that during recrystallization of cold-deformed materials, isothermal grain boundary migration rates decrease with time and reasons for such a decrease are discussed. A new methodology whereby migration rates of the individual recrystallization texture components may be quantified by combining stereology and orientation imaging by the electron back scattered pattern analysis is outlined. By illustration, recent experiments on aluminum and copper are summarized documenting the slight growth rate advantage the cube texture component (001)[100] possesses during recrystallization of cold rolled material. The role of orientation pinning effects on grain boundary migration is described briefly. It appears that such pinning effects allow recrystallized grains emerging from the weaker deformation texture components to enjoy an average growth rate advantage over those emerging from the stronger deformation texture components.     

3D processing map and hot deformation behaviour of a new type Al–Zn–Mg alloy

ABSTRACT

The thermal compression behaviour of Al–Zn–Mg alloy was studied on a thermal simulator machine at the temperature range of 380–540°C and strain rate range of 0.01–10?s^?1. The constitutive equation and 3D processing map of the alloys were established. The microstructure characteristics of the alloy were studied by metallographic observation, electron back-scatter diffraction (EBSD) analysis and transmission electron microscopy (TEM) microstructure analysis. The results show that the peak stress of high-temperature deformation of alloy decreases with the increase of deformation temperature and increases with the increase of strain rate. The dynamic recovery of the alloy occurs at the temperature range of 380–460°C and the strain rate range of 0.01–0.1?s^?1. The dynamic recrystallization of the alloy occurs at the temperature range of 460–500°C and the strain rate range of 0.01–0.1?s^?1. The alloy maintains fine and uniform recrystallized grains at a temperature range of 460–480°C and a strain rate range of 0.01–0.1?s^?1, which is suitable for hot working.     

Effect of post-deformation ageing on the recrystallization of KCl-SrCl2 crystals

Room-temperature recrystallization of KCl single crystals, both pure and doped with 0.02 and 0.06 wt % Sr, deformed preliminarily at 250°C is studied. It is found that annealing of the original single crystals at 650°C results in the precipitation of the SrCl₂ phase from the solid solution. X-ray diffraction studies reveal that the deformed crystals undergo ageing at room temperature, which is accompanied by a change in the phase composition. In the first place, particles of the KSr₂Cl₅ phase are formed instead of the phase SrCl₂ observed in the original and deformed crystals. These particles, which are located at the boundaries of growing recrystallized grains (twins of the original single crystal) occupying not more than 8% of the volume, impede the motion of grain boundaries and hamper further recrystallization. Second, it is shown that post-deformation ageing occurring in the remaining 92% of the deformed crystal region that has not undergone recrystallization lends stability to the strain-hardened state of alkali halide crystals over a period of at least two years at room temperature.     

The effect of severe plastic deformation and annealing conditions on mechanical properties and restoration phenomena in an ultrafine-grains Fe-28.5%Ni steel

The effect of annealing condition on the microstructure evolution, together with mechanical properties of Fe-28.5Ni steel processed by one and six cycles of accumulative roll bonding (ARB), was explored. The evolution of microstructure was studied by means of Electron Backscattered Diffraction method. The ARB-processed specimens were annealed for 30 minutes between 500°C and 600°C, and the effect of these annealing processes was elaborated. Results showed a significantly reduced martensite phase during ARB process cycles. Moreover, a refined and stabilised ultrafine structure was obtained in 6-cycle ARB-processed specimen. Results also show that by annealing the 1-cycle specimen at 550°C, no significant microstructural change and mechanical properties variation are identified. As such, no significant microstructural change and mechanical properties variation were notified for annealing of 6-cycle ARB-processed specimen at 500°C. However, annealing at 600°C in both conditions led to a complete recrystallisation of the deformed structure. Annealing at 550°C in 6-cycle ARB-processed specimen showed partial recrystallisation as well as an abnormal grain growth characteristic. The abnormal grain growth was seen by annealing of 1-cycle ARB-processed specimen at 600°C. The changing features of dislocations were discussed in these specimens in terms of changing the dynamics of low- and high-angle grain boundaries. Tensile test results also showed a significant increase in the yield/ultimate tensile strengths with the application of ARB cycles. Although ARB process led to a rapid reduction of total elongation, full restoration during high-temperature annealing returned this value back to the initial, non-deformed, condition.     

Elevated temperature directional recrystallization of high-purity nickel

Electron backscattered diffraction has been used to characterise the three different kinds of boundaries that occur in grains that are generated by secondary recrystallization during directional annealing of high-purity nickel. Boundaries between columnar grains (CC boundaries) can be twin boundaries, low-angle boundaries or high-angle grain boundaries. The frequency of low-angle CC boundaries dropped from 25% to 0% while the frequency of the high-angle CC boundaries increased from 19% to 67% when the annealing temperature was increased from 1000°C to 1200°C. The misorientation angles of boundaries between columnar grains and small equiaxed grains ahead of them (CE boundaries) was random at 1200°C but had a 40° rotation relationship about ?111? at 1000°C. It was found out that the character of the CC boundaries is determined by relative mobility of the CE boundaries, which is determined by the processing temperature rather than the energy of the CC boundaries themselves. The character of the island grain boundaries sometimes found with columnar grains was not affected by the annealing temperature or the drawing velocity.     

Helium migration in palladium II. scanning electron microscopy examination of high concentration samples

Scanning electron microscopy has been used to examine bulk phenomena of palladium samples annealed at 1200°C after implantation to a dose of 10¹⁷ He atoms/cm² at 5 MeV. A 3μ deep porous layer was found at a depth of 10.9μ±0.3μ. Wide grain boundaries (microcracks) extended from this layer to the top surface of the sample.     

Sol-gel synthesis and dilute magnetism of nano MgO powder doped with Fe

Mg oxides doped with 1 % ⁵⁷Fe were prepared by a sol-gel method, and annealed at various temperatures. Nano-size Mg oxides were characterized by Mössbauer spectrometry, magnetization and XRD measurements. The crystalline size of MgO increases with increase of annealing temperature. Samples annealed at 600 °C and 800 °C gave only doublet peaks of paramagnetic Fe³⁺ in Mössbauer spectra although Fe³⁺ doping into MgO induced a distorted structure and showed weak ferromagnetism. It is considered that the magnetic property is due to defect induced magnetism by doping Fe³⁺ into MgO. For a sample heated at 1000 °C, it is found from low temperature Mössbauer spectra that Fe³⁺ species are located at the core and shell of fine MgFe₂O₄ grains and diluted in MgO matrix.     

High pressure infiltration sintering behavior of WC-Co alloys

In this paper, two average tungsten carbide particle sizes of 2, 0.5?μm are placed respectively, in contact with a WC-16Co substrate, pressed at the pressure of 4.5–5.5?GPa, and heated to temperatures ranging from 1350°C to 1500°C in a large-volume cubic press. During the process Co was forced out of the WC-16Co substrate into the compressed powder. The resulting infiltrated samples were characterized using X-ray diffraction (XRD), scanning electron microscope (SEM), Vickers hardness and cutting performance tests. The results of XRD confirmed that the sintered bulks have WC and Co phases. The scanning electron microscopy (SEM) analysis reveals that the WC grains in well-sintered alloys are round in shape and cobalt with lower content is uniformly dispersed in the WC grain boundaries. The sintered sub-micron WC-Co alloy with a cobalt content of 3.8?wt% exhibits a prominent combination of high hardness value of 23.1?GPa and a large fracture toughness value of 8.6?MPa?m^½. The high-speed cutting tests indicating its cutting performance is significantly superior to the commercial YG6X (WC-6?wt%Co with WC grain size of 0.5?μm).     

Microscopical study of the formation of adiabatic shear bands in 4340 steel during dynamic loading

In this study, optical microscopy, scanning electron microscopy, transmission electron microscopy, X-ray diffraction and electron probe microanalyser were used to analyse the changes in microstructure of AISI 4340 steel specimens caused by impact at high strain rates and large strains. The structures of the steel prior to dynamic deformation and after dynamic deformation were examined to understand on a microscale level, the mechanism of formation of adiabatic shear bands (ASBs). The study also includes the structural changes that occur during post-deformation annealing processes which may relate to understanding of the mechanism of formation of ASBs. Prior to deformation, the tempered steel specimens consisted of lenticular laths of α-ferrite with precipitated platelet and spherical M₃C carbides. After impact, the structure inside the shear band was characterized by refined and recrystallized grains immersed in dense dislocation structures. In addition, residual carbide particles were observed inside the shear bands due to deformation induced carbide dissolution. Regions away from the shear bands developed ‘knitted’ dislocation walls, evolving gradually into sub-boundaries and highly misoriented grain boundaries at increasing strains, leading to grain refinement of the ferrite. After impact, annealing the shear bands at 350?°C resulted in an increase in hardness regardless of the heat treatment before impact, amount of deformation and the time of annealing. This is because of the occurrence of extensive reprecipitation of dissolved carbides that existed in the steel structure prior to deformation. It is concluded that dynamic recovery/recrystallization, development of dislocation structures and carbide dissolution all contribute simultaneously to the formation of ASBs in quench-hardened steels.     

Crystallization behaviour of PZT in multilayer heterostructures

Microstructural and electrical properties of PZT (lead zirconate titanate) thin films prepared by sol-gel techniques at annealing temperatures in the range from 550°C to 900°C are studied. Perovskite (Pe) grain nucleation in PZT film starts but not completes at 550°C. Along with formation of round Pe (111) grains on the Pt (111) interface, the film contains small Pe and pyrochlore (Py) grains. Films annealed at the temperatures higher than 600°C demonstrate column structure of Pe grains, the amount of Py inclusions reduces with the annealing temperature and practically disappears at 700°C. An increase of annealing temperature leads to enhancement of (100) Pe orientation as a result of Ti diffusion on the Pt surface. Polarization decreases with the annealing temperature (maximum at 600°C), whereas permittivity increases up to the annealing temperature of 750°C.     

Effect of thermal annealing on the structure and microstructure of TiO2 thin films

Nanostructured TiO₂ thin films have been prepared through chemical route using sol-gel and spin coating techniques. The deposited films were annealed in the temperature range 400–1000°C for 1 h. The structure and microstructure of the annealed films were characterized by GAXRD, micro-Raman spectroscopy and AFM. The as-deposited TiO₂ thin films are found to be amorphous. Micro-Raman and GAXRD results confirm the presence of the anatase phase and absence of the rutile phase for films annealed up to 700°C. The diffraction pattern of the film annealed at 800 to 1000°C contains peaks of both anatase and rutile reflections. The intensity of all peaks in micro-Raman and GAXRD patterns increased and their width (FWHM) decreased with increasing annealing temperature, demonstrating the improvement in the crystallinity of the annealed films. Phase transformation at higher annealing temperature involves a competition among three events such as: grain growth of anatase phase, conversion of anatase to rutile and grain growth of rutile phase. AFM image of the asdeposited films and annealed films indicated exponential grain growth at higher temperature.      

Effects of thermally induced anatase-to-rutile phase transition in MOCVD-grown TiO2 films on structural and optical properties

Titanium dioxide (TiO₂) films with a thickness of 550 nm were deposited on quartz glass at 300 °C by metalorganic chemical vapor deposition. The effects of post-annealing between 600 °C and 1000 °C were investigated on the structural and optical properties of the films. X-ray diffraction patterns revealed that the anatase phase of as-grown TiO₂ films began to be transformed into rutile at the annealing temperature of 900 °C. The TiO₂ films were entirely changed to the rutile phase at 1000 °C. From scanning electron spectroscopy and atomic force microscopy images, it was confirmed that the microstructure of as-deposited films changed from narrow columnar grains into wide columnar ones. The surface composition of the TiO₂ films, which was analyzed by X-ray photoelectron spectroscopy data, was nearly constant although the films were annealed at different temperatures. When the annealing temperature increased, the transmittance of the films decreased, whereas the refractive index and the extinction coefficient calculated by the envelope method increased at high temperature. The values of optical band gap decreased from 3.5 eV to 3.25 eV at 900 °C. This abrupt decrease was consistent with the anatase-to-rutile phase transition. Received: 4 October 2000 / Accepted: 4 December 2000 / Published online: 23 May 2001     

Surface morphology of ZnO buffer layer and its effects on the growth of GaN films on Si substrates by magnetron sputtering

ZnO thin films were first prepared on Si(111) substrates using a radio frequency magnetron sputtering system. Then the as-grown ZnO films were annealed in oxygen ambient at temperatures of 700, 800, 900, and 1000°C , respectively. The morphologies of ZnO films were studied by an atom force microscope (AFM). Subsequently, GaN epilayers about 500 nm thick were deposited on the ZnO buffer layers. The GaN/ZnO films were annealed in NH₃ ambient at 900°C. The microstructure, morphology and optical properties of GaN films were studied by x-ray diffraction (XRD), AFM, scanning electron microscopy (SEM) and photoluminescence (PL). The results are shown, their properties having been investigated particularly as a function of the ZnO layers. For better growth of the GaN films, the optimal annealing temperature of the ZnO buffer layers was 900°C.     

Effects of annealing temperature on YAG:Ce synthesized by spray-drying method

In this report, YAG:Ce phosphors were synthesized by spray-drying method. The effects of annealing temperature on crystal structure, morphology and photoluminescence property (PL) of as-prepared samples were investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM) and spectrofluorometer, respectively. The XRD patterns showed all the samples are in consistence with a single garnet phase, and the location of strongest peak shifts to smaller angle with increasing the annealing temperature. The SEM micrographs revealed the sample annealed at 1200 °C appears to be a spherical polycrystalline aggregate; as the samples were annealed at 1300?1400 °C, spherical grains obviously grow up; but the sample annealed at over 1400 °C forms an irregular bulk. The emission spectra of samples indicated the PL of samples annealed at 1200?1400 °C improve with increasing the annealing temperature because of the diffusion of Si⁴⁺ ions; whereas the PL of sample annealed at the temperature over 1400 °C decreases likely resulting from inflection effects of multiangular shape of grains. Therefore, the samples annealed at 1400 °C are suitable for gaining phosphor with high brightness and good morphology.     

Microstructure changes in two phase β+ γ Co-Ni-Al ferromagnetic shape memory alloys in relation to Al/Co ratio

The microstructure of Co_{35 + x}-Ni_{40 - x}-Al₂₅ (x = 0, 2.5, 5.0) ferromagnetic shape memory alloys annealed at 1200 °C and water quenched has been investigated by optical (OM) and analytical transmission electron microscopy (TEM). The microstructure consists of elongated grains of martensite and γ phase. Annealing twins were found frequently in the γ phase. The volume fraction of γ phase has been determined to be about 40%. TEM observations show twinned L1₀ martensite with {111}-type twinning plane and tetragonality c/a = 0.85 in all investigated alloys. Determination of the composition of β phase, allows to calculate Al/Co and e/a ratio in the range 7.68–8.40 in correlation with its Ms temperatures between 66 and 167 °C, respectively. An increase in the Al/Co ratio together with a decrease of Ni content in β phase causes a decrease of the e/a ratio, which promotes a decrease of martensitic transformation temperatures.