Showing papers on "Grain growth published in 2016"

Electron beam melted Ti–6Al–4V: Microstructure, texture and mechanical behavior of the as-built and heat-treated material

Abstract: Electron Beam Melting (EBM), a powder bed additive layer manufacturing process, was used to produce Ti–6Al–4V specimens, whose microstructure, texture, and tensile properties were fully characterized. The microstructure, analyzed by optical microscopy, SEM/EBSD and X-ray diffraction, consists in fine α lamellae. Numerical reconstruction of the parent β phase highlighted the columnar morphology of the prior β grains, growing along the build direction upon solidification of the melt pool. The presence of grain boundary αGB along the boundaries of these prior β grains is indicative of the diffusive nature of the β→α phase transformation. Texture analysis of the reconstructed high temperature β phase revealed a strong pole in the build direction. For mechanical characterization, tensile specimens were produced using two different build themes and along several build orientations, revealing that vertically built specimens exhibit a lower yield strength than those built horizontally. The effect of post processing, either mechanical or thermal, was extensively investigated. The influence of surface finish on tensile properties was clearly highlighted. Indeed, mechanical polishing induced an increase in ductility – due to the removal of critical surface defects – as well as a significant increase of the apparent yield strength – caused by the removal of a ~150 µm rough surface layer that can be considered as mechanically inefficient and not supporting any tensile load. Thermal post-treatments were performed on electron beam melted specimens, revealing that subtransus treatments induce very moderate microstructural changes, whereas supertransus treatments generate a considerably different type of microstructure, due to the fast β grain growth occurring above the transus. The heat treatments investigated in this work had a relatively moderate impact on the mechanical properties of the parts.

Tailoring nanostructures and mechanical properties of AlCoCrFeNi2.1 eutectic high entropy alloy using thermo-mechanical processing

Abstract: The effect of thermo-mechanical processing on the evolution of microstructure and mechanical properties was investigated in an AlCoCrFeNi2.1 high entropy alloy. For this purpose, the alloy was cold-rolled to 90% reduction in thickness and annealed at temperatures ranging from 800 °C to 1200 °C. The as-cast alloy revealed eutectic lamellar mixture of (Ni, Al) rich but Cr depleted B2 phase and Al-depleted L12 phases, having volume fractions of ~35% and 65%, respectively. Nanosized precipitates enriched in Cr and having disordered BCC structure were found dispersed inside the B2 phase. Cold-rolling resulted in progressive disordering of the L12 phase but the B2 phase maintained the ordered structure. The disordering of the L12 phase was accompanied by the evolution of ultrafine lamellar structure and profuse shear band formation. Annealing of the 90% cold-rolled material at 800 °C resulted in the formation of a duplex microstructure composed of two different phases with equiaxed morphologies, having significant resistance to grain growth up to 1200 °C. The annealed materials showed disordered FCC and precipitate-free B2 phases. This indicated that quenching of the annealed specimens to room temperature was sufficient to prevent the ordering of the L12 phase and the formation of the Cr-rich nano-precipitates which were dissolved in the B2 phase during annealing. Significant improvement in tensile properties compared to the as-cast alloy could be achieved by thermo-mechanical processing. All the specimens annealed at 800 °C to 1200 °C were having good tensile ductility over 10% as well as high tensile strength greater than 1000 MPa. These indicated that the properties of the EHEA could be successfully tailored using thermo-mechanical processing for a wide range of engineering applications.

Effect of annealing on mechanical properties of a nanocrystalline CoCrFeNiMn high-entropy alloy processed by high-pressure torsion

Abstract: A CoCrFeNiMn high-entropy alloy (HEA) was processed by high-pressure torsion (HPT) under 6.0 GPa pressure up to 10 turns at room temperature. It is shown that there is a gradual evolution in hardness with increasing numbers of turns but full homogeneity is not achieved even after 10 turns. Microhardness measurements reveal that the material reaches a saturation hardness value of ~4.41 GPa and in this condition the microstructure shows exceptional grain refinement with a grain size of ~10 nm. An ultimate strength value of ~1.75 GPa and an elongation to fracture of ~4% were obtained in a sample processed for 5 turns. The nanostructured HEA was subjected to post-deformation annealing (PDA) at 473–1173 K and it is shown that the hardness increases slightly to 773 K due to precipitation and then decreases up to 1173 K due to a combination of recrystallization, grain growth and a dissolution of the precipitates. The formation of brittle precipitates, especially σ-phase, at 873 and 973 K significantly reduces the ductility. Short-term annealing for 10 min at 1073 K prevents grain growth and leads to a combination of high strength and good ductility including an ultimate tensile strength of ~830 MPa and an elongation to failure of ~65%.

Ferroelectricity in undoped-HfO2 thin films induced by deposition temperature control during atomic layer deposition

Abstract: HfO2 thin films, extensively studied as high-k gate dielectric layers in metal-oxide-semiconductor field effect transistors, have attracted interest of late due to their newly discovered ferroelectricity in doped HfO2. The appearance of the ferroelectric orthorhombic phase of HfO2 was previously examined in variously doped and undoped systems, but the effects of process-variable changes on the physical and chemical characteristics of a thin film and the resulting ferroelectricity have not been studied systematically. Here, the evolution of ferroelectricity in HfO2 thin films through deposition temperature control during atomic layer deposition was systematically examined without the intentional doping of metallic elements other than Hf. The lower-temperature-deposited HfO2 showed an increased impurity concentration, which was mainly carbon, and the involvement of these impurities suppressed the lateral grain growth during the crystallization thermal treatment. The grain size reduction could stabilize the metastable orthorhombic phase, whose surface and grain boundary energies are lower than those of the room-temperature-stable monoclinic phase, by increasing the grain boundary areas. The 9 nm-thick HfO2 thin film deposited at 220 °C exhibited a remanent polarization value of 10.4 μC cm−2 and endured up to 108 switching cycles, which is a 102-fold improvement compared to the previously reported undoped 6 nm-thick HfO2. This can be ascribed to the decrease in the relative portion of defective interfacial layers by increasing the total film thickness. The strategy of using deposition temperature control is a feasible method for the fabrication of these new lead-free binary ferroelectric thin films.

Large Perovskite Grain Growth in Low-Temperature Solution-Processed Planar p-i-n Solar Cells by Sodium Addition.

Abstract: Thin-film p-i-n type planar heterojunction perovskite solar cells have the advantage of full low temperature solution processability and can, therefore, be adopted in roll-to-roll production and flexible devices. One of the main challenges with these devices, however, is the ability to finely control the film morphology during the deposition and crystallization of the perovskite layer. Processes suitable for optimization of the perovskite layer film morphology with large grains are highly desirable for reduced recombination of charge carriers. Here, we show how uniform thin films with micron size perovskite grains can be made through the use of a controlled amount of sodium ions in the precursor solution. Large micrometer-size CH3NH3PbI3 perovskite grains are formed during low-temperature thin-film growth by adding sodium ions to the PbI2 precursor solution in a two-step interdiffusion process. By adjusting additive concentration, film morphologies were optimized and the fabricated p-i-n planar perovskite...

Electrode Effects on Microstructure Formation During FLASH Sintering of Yttrium‐Stabilized Zirconia

Abstract: Systematic microstructural statistics for 3 mol% yttria-stabilized zirconia synthesized by both conventional sintering and flash sintering with AC and DC current were obtained. Within the gage section, flash sintered microstructures were indistinguishable from those synthesized by conventional sintering procedures. With both techniques, full densification was obtained. However, from both AC and DC flash sintered specimens, heterogeneous grain size distributions and residual porosity were observed in the proximity of the electrodes. After DC sintering, an almost 400 times increased average grain size was observed near cathode compared to the gage section, unlike areas close to the anode. Concepts of Joule heating alone were not sufficient to explain the experimental observations. Instead, the activation energy for grain growth close to the cathode is lowered considerably during flash sintering, hence suggesting that electrode effects can cause significant heterogeneities in microstructure evolution during flash sintering. Microstructural characterization further indicated that microfracturing during green-pressing and variations in contact resistance between the electrodes and the ceramic may also contribute to grain size gradients and hence local variations of physical properties.

Chemical Expansion of Yttrium-Doped Barium Zirconate and Correlation with Proton Concentration and Conductivity

Abstract: Y-doped BaZrO3 (BZY) is a promising candidate as an electrolyte in fuel cells, and attracts increasing attention. In this work, a systematic investigation was performed on microstructure, proton concentration, proton conductivity, and hydration induced chemical expansion in Y-doped BaZrO3. The results revealed that the bimodal microstructure in BaZr0.85Y0.15O3−δ was composed of large grains with composition close to the nominal value, and fine grains with large compositional discrepancy. This property is considered to be one of the evidences of phase separation at lower temperature than sintering temperature (1600°C), which hinders the grain growth. Thermal expansion coefficient of BZY was measured for various dopant level, and was determined to be around 10−5 K−1 in wet and dry argon atmosphere. In addition, chemical expansion effect due to hydration was confirmed by HT-XRD in dry and wet Ar atmospheres, and suggests an interesting relationship between the lattice change ratio and proton concentration, in the BZY system with different Y content. The change ratio of lattice constant due to hydration increased obviously with the proton concentration for the sample containing the Y content of 0.02 and 0.05, but only changed slightly when the Y content was increased to 0.1 and 0.15. However, when the Y content was further increased over 0.2, the change ratio of lattice constant due to hydration starts to increase obviously again. Such results indicate a high possibility that the stable sites of protons in BZY changed with the variation in Y content.

Microstructural Evolutions During Annealing of Plastically Deformed AISI 304 Austenitic Stainless Steel: Martensite Reversion, Grain Refinement, Recrystallization, and Grain Growth

Abstract: Microstructural evolutions during annealing of a plastically deformed AISI 304 stainless steel were investigated. Three distinct stages were identified for the reversion of strain-induced martensite to austenite, which were followed by the recrystallization of the retained austenite phase and overall grain growth. It was shown that the primary recrystallization of the retained austenite postpones the formation of an equiaxed microstructure, which coincides with the coarsening of the very fine reversed grains. The latter can effectively impair the usefulness of this thermomechanical treatment for grain refinement at both high and low annealing temperatures. The final grain growth stage, however, was found to be significant at high annealing temperatures, which makes it difficult to control the reversion annealing process for enhancement of mechanical properties. Conclusively, this work unravels the important microstructural evolution stages during reversion annealing and can shed light on the requirements and limitations of this efficient grain refining approach.

High-speed extrusion of dilute Mg-Zn-Ca-Mn alloys and its effect on microstructure, texture and mechanical properties

Abstract: Three dilute Mg-Zn-Ca-Mn alloys were successfully extruded at 24 m/min and the alloy with lowest Zn content (0.21 wt%) can even be extruded at 60 m/min without any surface defects, which was ascribed to the thermally stable Mg2Ca phase and high solidus temperature (∼620 °C). The alloys extruded at die-exit speed ≥6 m/min showed a fully dynamically recrystallized (DRXed) microstructure and weak rare earth (RE) texture at the position between [2 1 1 4] and [2 1 1 2] parallel to the extrusion direction. Besides, fine Mg2Ca and α-Mn particles dynamically precipitated during extrusion, acting as effective pinning obstacles against the DRXed grain growth via Zener drag effect. Due to the deformation temperature rise with increasing extrusion speeds, the grain size increased gradually, which can be understood from the relationship between DRXed grain size and Zener-Hollomon parameter. The RE texture contributed to high uniform elongation of ∼23%, but the increased grain size (>30 µm) deteriorated post-uniform elongation due to the prevalence of {10 1 1} contraction and {10 1 1}-{10 1 2} double twins during post-uniform deformation.

Evolution of twins and substructures during low strain rate hot deformation and contribution to dynamic recrystallization in alloy 617B

Abstract: Substructure and twin boundary evolution of alloy 617B during dynamic recrystallization (DRX) was investigated by optical microscope, electron backscatter diffraction (EBSD) and transmission electron microscope (TEM) technique. Simulated compression tests were carried out at different true strains in the temperature range of 1120–1210 °C with a strain rate of 0.001 s −1 . The results show that discontinuous dynamic recrystallization (DDRX) featured by original grain boundary bulging is the dominant nucleation mechanism for alloy 617B. The progressive subgrain rotation, which is a characterization of continuous dynamic recrystallization (CDRX) can be detected at the early stage of hot deformation at lower temperature, which can just be considered as an assistant mechanism. The evolution of substructure and twin boundaries have a significant effect on DRX process of alloy 617B. Twinning formation can active the DRX process by accelerating original grain boundary bulging and separation of bulging grain boundaries. The formation of twin steps resulting from twin slipping provide additional DRX nucleation locations. The effort of twins gets weaker with the increase of temperature as the DRX grain growth process associated with grain boundary area reduction gradually becomes a preferential mechanism for energy minimization. Different from previous study, the fraction of twin boundaries decrease with the increase of temperature, which can be attributed to the twin boundary accelerated prior grain growth process. Such process also results in the serious bulging of grain boundaries into adjacent grains.

Controlled Grain Growth for High Performance Nanoparticle-Based Kesterite Solar Cells

Abstract: Large-grain absorber formation through selenization techniques is a promising route for high performance chalcogenide solar cells. Understanding and subsequently controlling such grain growth is essential in improving absorber quality and developing absorbers with unique optoelectronic and morphological properties. We explain the essential role of liquid selenium in the grain growth of Cu2ZnSnSe4 (CZTSe) absorbers from Cu2ZnSnS4 nanoparticles by proposing a liquid-assisted grain growth mechanism. Through the use of a multizone rapid-thermal-processing furnace, control of liquid Se delivery to the film and the Se(g) atmosphere during processing is shown to result in novel absorbers with tunable properties. Additionally, the processing parameters necessary for high quality CZTSe absorbers, the role of nanoparticle properties, and the role of alkali metal dopants in the liquid-assisted growth mechanism are shown. Ultimately, record nanoparticle-based device performance of 9.3% is achieved for selenized CZTSe...

Prediction of machining-induced phase transformation and grain growth of Ti-6Al-4 V alloy

Abstract: The high-speed machining process can significantly influence the microstructure of the machined surface in titanium alloy. A physics-based finite element method is proposed for the modeling of machining-induced phase transformation and grain size growth of Ti-6Al-4 V material. Prediction of the grain growth and phase transformation are obtained with the Johnson-Mehl-Avrami-Kolmogorov (JMAK) dynamic recrystallization model and Avrami model, respectively. A modified Johnson Cook flow stress model is embedded into the method to account for the phase transformation. The accuracy of the proposed method is validated with experimental data. Parametric studies are conducted to investigate the effects of the cutting speed and the feed rate on the microstructure change in machining.

Influence of growth temperature on bulk and surface defects in hybrid lead halide perovskite films.

Abstract: The rapid development of perovskite solar cells has focused its attention on defects in perovskites, which are gradually realized to strongly control the device performance. A fundamental understanding is therefore needed for further improvement in this field. Recent efforts have mainly focused on minimizing the surface defects and grain boundaries in thin films. Using time-resolved photoluminescence spectroscopy, we show that bulk defects in perovskite samples prepared using vapor assisted solution process (VASP) play a key role in addition to surface and grain boundary defects. The defect state density of samples prepared at 150 °C (∼1017 cm−3) increases by 5 fold at 175 °C even though the average grains size increases slightly, ruling out grain boundary defects as the main mechanism for the observed differences in PL properties upon annealing. Upon surface passivation using water molecules, the PL intensity and lifetime of samples prepared at 200 °C are only partially improved, remaining significantly lower than those prepared at 150 °C. Thus, the present study indicates that the majority of these defect states observed at elevated growth temperatures originates from bulk defects and underscores the importance to control the formation of bulk defects together with grain boundary and surface defects to further improve the optoelectronic properties of perovskites.

The significance of self-annealing at room temperature in high purity copper processed by high-pressure torsion

Abstract: High purity copper was processed by high-pressure torsion (HPT) at room temperature and then stored at room temperature for periods of up to 6 weeks to investigate the effect of self-annealing. Hardness measurements were recorded both at 48 h after HPT processing and after various storage times. The results show the occurrence of recovery near the edges of the discs after processing through 1/2 and 1 turn and this leads to a significant drop in the measured hardness values which is accompanied by microstructural evidence for abnormal grain growth. Conversely, there was no recovery, and therefore no hardness drops, after processing through 5 and 10 turns. X-ray line profile analysis was used to determine the crystallite sizes and dislocation densities at 1 h after HPT and after storage for different times. The results show a good thermal stability in high purity Cu after processing through more than 1 turn of HPT but care must be exercised in recording hardness measurements when processing through only fractional or very small numbers of turns.