Showing papers on "Grain size published in 2016"

Recent advances in grain refinement of light metals and alloys

Abstract: Grain refinement leads, in general, to a decreased tendency to hot tearing, a more dispersed and refined porosity distribution, and improved directional feeding characteristics during solidification. Reduced as-cast grain size can also lead to improved mechanical properties and wrought processing by reducing the recrystallized grain size and achieving a fully recrystallized microstructure. It is now well established that the two key factors controlling grain refinement are the nucleant particles including their potency, size distribution and particle number density, and the rate of development of growth restriction, Q, generated by the alloy chemistry which establishes the undercooling needed to trigger nucleation events and facilitates their survival. The theories underpinning our current understanding of nucleation and grain formation are presented. The application of the latest theories to the light alloys of Al, Mg and Ti is explored as well as their applicability to a range of casting and solidification environments. In addition, processing by the application of physical processes such as external fields and additive manufacturing is discussed. To conclude, the current challenges for the development of reliable grain refining technologies for difficult to refine alloy systems are presented.

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%.

Stabilized Wide Bandgap MAPbBrxI3–x Perovskite by Enhanced Grain Size and Improved Crystallinity

Abstract: The light instability of CH3NH3PbI x Br3-x is one of the biggest challenges for its application in tandem solar cells. Here we show that an improved crystallinity and grain size of CH3NH3PbI x Br3-x films could stabilize these materials under one sun illumination, improving both the efficiency and stability of the wide-bandgap perovskite solar cells.

Extreme creep resistance in a microstructurally stable nanocrystalline alloy

Abstract: A nanocrystalline copper–tantalum alloy with high strength and extremely high-temperature creep resistance is achieved via a processing method that creates clusters of atoms within the alloy that pin grain boundaries. Reducing the grain size of a metal is one way of increasing its strength, but it can often have detrimental effects on other mechanical properties. The resistance to slow irreversible deformation known as creep, for example, can be greatly diminished, owing to the relatively large volume of the material that is in the form of grain boundaries between the nanocrystalline constituents. Kristopher Darling et al. describe a family of nanostructured alloys that combine high strength with extremely high creep resistance. Key to this achievement is a processing strategy that creates tiny clusters at the grain boundaries, stabilizing the nanocrystalline grains against sliding, rotation and diffusional growth, and so greatly enhancing their resistance to creep. Nanocrystalline metals, with a mean grain size of less than 100 nanometres, have greater room-temperature strength than their coarse-grained equivalents, in part owing to a large reduction in grain size1. However, this high strength generally comes with substantial losses in other mechanical properties, such as creep resistance, which limits their practical utility; for example, creep rates in nanocrystalline copper are about four orders of magnitude higher than those in typical coarse-grained copper2,3. The degradation of creep resistance in nanocrystalline materials is in part due to an increase in the volume fraction of grain boundaries, which lack long-range crystalline order and lead to processes such as diffusional creep, sliding and rotation3. Here we show that nanocrystalline copper–tantalum alloys possess an unprecedented combination of properties: high strength combined with extremely high-temperature creep resistance, while maintaining mechanical and thermal stability. Precursory work on this family of immiscible alloys has previously highlighted their thermo-mechanical stability and strength4,5, which has motivated their study under more extreme conditions, such as creep. We find a steady-state creep rate of less than 10−6 per second—six to eight orders of magnitude lower than most nanocrystalline metals—at various temperatures between 0.5 and 0.64 times the melting temperature of the matrix (1,356 kelvin) under an applied stress ranging from 0.85 per cent to 1.2 per cent of the shear modulus. The unusual combination of properties in our nanocrystalline alloy is achieved via a processing route that creates distinct nanoclusters of atoms that pin grain boundaries within the alloy. This pinning improves the kinetic stability of the grains by increasing the energy barrier for grain-boundary sliding and rotation and by inhibiting grain coarsening, under extremely long-term creep conditions. Our processing approach should enable the development of microstructurally stable structural alloys with high strength and creep resistance for various high-temperature applications, including in the aerospace, naval, civilian infrastructure and energy sectors.

The OsmiR396c-OsGRF4-OsGIF1 regulatory module determines grain size and yield in rice

Abstract: Grain weight is the most important component of rice yield and is mainly determined by grain size, which is generally controlled by quantitative trait loci (QTLs). Although numerous QTLs that regulate grain weight have been identified, the genetic network that controls grain size remains unclear. Herein, we report the cloning and functional analysis of a dominant QTL, grain length and width 2 (GLW2), which positively regulates grain weight by simultaneously increasing grain length and width. The GLW2 locus encodes OsGRF4 (growth-regulating factor 4) and is regulated by the microRNA miR396c in vivo. The mutation in OsGRF4 perturbs the OsmiR396 target regulation of OsGRF4, generating a larger grain size and enhanced grain yield. We also demonstrate that OsGIF1 (GRF-interacting factors 1) directly interacts with OsGRF4, and increasing its expression improves grain size. Our results suggest that the miR396c-OsGRF4-OsGIF1 regulatory module plays an important role in grain size determination and holds implications for rice yield improvement.

Modulating crystal grain size and optoelectronic properties of perovskite films for solar cells by reaction temperature.

Abstract: Regulating the temperature during the direction contact and intercalation process (DCIP) for the transition from PbI2 to CH3NH3PbI3 modulated the crystallinity, crystal grain size and crystal grain orientation of the perovskite films. Higher temperatures produced perovskite films with better crystallinity, larger grain size, and better photovoltaic performance. The best cell, which had a PCE of 12.9%, was obtained on a film prepared at 200 °C. Further open circuit voltage decay and film resistance characterization revealed that the larger grain size contributed to longer carrier lifetime and smaller carrier transport resistance, both of which are beneficial for solar cell devices.

Grain-Size-Limited Mobility in Methylammonium Lead Iodide Perovskite Thin Films

Abstract: We report a systematic study of the gigahertz-frequency charge carrier mobility found in methylammonium lead iodide perovskite films as a function of average grain size using time-resolved microwave conductivity and a single processing chemistry. Our measurements are in good agreement with the Kubo formula for the AC mobility of charges confined within finite grains, suggesting (1) that the surface grains imaged via scanning electron microscopy are representative of the true electronic domain size and not substantially subdivided by twinning or other defects not visible by microscopy and (2) that the time scale of diffusive transport across grain boundaries is much slower than the period of the microwave field in this measurement (∼100 ps). The intrinsic (infinite grain size) minimum mobility extracted form the model is 29 ± 6 cm2 V–1 s–1 at the probe frequency (8.9 GHz).

Wire Arc Additive Manufacturing of AZ31 Magnesium Alloy: Grain Refinement by Adjusting Pulse Frequency

Abstract: Wire arc additive manufacturing (WAAM) offers a potential approach to fabricate large-scale magnesium alloy components with low cost and high efficiency, although this topic is yet to be reported in literature. In this study, WAAM is preliminarily applied to fabricate AZ31 magnesium. Fully dense AZ31 magnesium alloy components are successfully obtained. Meanwhile, to refine grains and obtain good mechanical properties, the effects of pulse frequency (1, 2, 5, 10, 100, and 500 Hz) on the macrostructure, microstructure and tensile properties are investigated. The results indicate that pulse frequency can result in the change of weld pool oscillations and cooling rate. This further leads to the change of the grain size, grain shape, as well as the tensile properties. Meanwhile, due to the resonance of the weld pool at 5 Hz and 10 Hz, the samples have poor geometry accuracy but contain finer equiaxed grains (21 μm) and exhibit higher ultimate tensile strength (260 MPa) and yield strength (102 MPa), which are similar to those of the forged AZ31 alloy. Moreover, the elongation of all samples is above 23%.

Effects of dilute additions of Zn and Ca on ductility of magnesium alloy sheet

Abstract: The present study seeks to clarify the mechanism by which dilute additions of zinc (Zn) and calcium (Ca) improve ductility of Mg alloy sheet. Herein, the ductility and microstructure of fully annealed pure Mg and Mg-0.1Ca, Mg-0.4Ca, Mg-0.4Zn, and Mg-0.3Zn-0.1Ca (at.%) alloy sheet were systematically investigated and compared. It is found that the ternary alloy displays better ductility than either pure Mg or binary Mg-alloys, when fully recrystallized and possessing similar grain size. In the deformed grains of the ternary alloy, traces of basal and pyramidal slip and { 10 1 2 } twins are observed, whilst only basal slip traces and { 10 1 2 } twins are observed in the pure Mg and binary alloys. Grain boundary cracks are observed in all the tensile-tested alloys. However, significantly less grain boundary cracks are observed in the ternary alloy, posited to be due to enhanced grain boundary cohesion. These observations suggest that the combination of enhanced pyramidal slip and suppressed grain boundary cracking leads to the appreciably improved ductility of the Mg-0.3Zn-0.1Ca alloy sheet.

Grain Size Constraints on HL Tau with Polarization Signature

Abstract: The millimeter-wave polarization of the protoplanetary disk around HL Tau has been interpreted as the emission from elongated dust grains aligned with the magnetic field in the disk. However, the self-scattering of thermal dust emission may also explain the observed millimeter-wave polarization. In this paper, we report a modeling of the millimeter-wave polarization of the HL Tau disk with the self-polarization. Dust grains are assumed to be spherical and to have a power-law size distribution. We change the maximum grain size with a fixed dust composition in a fixed disk model to find the grain size to reproduce the observed signature. We find that the direction of the polarization vectors and the polarization degree can be explained with the self-scattering. Moreover, the polarization degree can be explained only if the maximum grain size is $\sim 150 {\rm~\mu m}$. The obtained grain size from the polarization is different from a size of millimeter or larger that has been previously expected from the spectral index of the dust opacity coefficient if the emission is optically thin. We discuss that porous dust aggregates may solve the inconsistency of the maximum grain size between the two constraints.

Grain size dependence of hardness and fracture toughness in pure near fully-dense boron carbide ceramics

Abstract: Room temperature fracture toughness and hardness of spark plasma sintered pure B 4 C ceramics with grain sizes ranging from 120 nm to 17 μm have been studied. Vickers indentation and single edge V-notched beam (SEVNB) techniques have been used to measure hardness and fracture toughness, respectively. A critical analysis of the results derived from these two techniques has been carried out and the conditions for proper comparison of the derived results are discussed. The results have shown that hardness follows the Hall–Petch dependence with either grain size or twin spacing when the effect of porosity is corrected for. On the contrary, fracture toughness is found to be essentially grain size independent. The value of this quantity is ∼2 MPa m 1/2 .

Pore structure characterization of Chang-7 tight sandstone using MICP combined with N 2 GA techniques and its geological control factors

Abstract: Understanding the pore networks of unconventional tight reservoirs such as tight sandstones and shales is crucial for extracting oil/gas from such reservoirs. Mercury injection capillary pressure (MICP) and N2 gas adsorption (N2GA) are performed to evaluate pore structure of Chang-7 tight sandstone. Thin section observation, scanning electron microscope, grain size analysis, mineral composition analysis, and porosity measurement are applied to investigate geological control factors of pore structure. Grain size is positively correlated with detrital mineral content and grain size standard deviation while negatively related to clay content. Detrital mineral content and grain size are positively correlated with porosity, pore throat radius and withdrawal efficiency and negatively related to capillary pressure and pore-to-throat size ratio; while interstitial material is negatively correlated with above mentioned factors. Well sorted sediments with high debris usually possess strong compaction resistance to preserve original pores. Although many inter-crystalline pores are produced in clay minerals, this type of pores is not the most important contributor to porosity. Besides this, pore shape determined by N2GA hysteresis loop is consistent with SEM observation on clay inter-crystalline pores while BJH pore volume is positively related with clay content, suggesting N2GA is suitable for describing clay inter-crystalline pores in tight sandstones.

Influence of mode of electrodeposition, current density and saccharin on the microstructure and hardness of electrodeposited nanocrystalline nickel coatings

Abstract: The main purpose of the present work is to study the influence of current density, deposition mode and the presence of saccharin as an additive on the microstructure, sulfur content, grain size and microhardness of nanocrystalline Ni coatings. Towards this purpose, nanocrystalline nickel (Ni) coatings were deposited at various current densities in Watt's bath using direct, pulse and pulse reverse current (PRC) electrodeposition and subsequently characterized for sulfur content, grain size and hardness. It was observed that, the current density has no influence on the grain size/hardness of nanocrystalline Ni coatings in direct and pulsed current electrodeposition mode. However, the grain size increased from ~ 20 to ~ 200 nm with decrease in current density in PRC mode of deposition. In addition a substantial change in microstructure and texture of PRC Ni coatings was also evident. The experimental results have been rationalized based on the adsorption–desorption type of mechanism during electrodeposition.

Crystalline Grain Interior Configuration Affects Lithium Migration Kinetics in Li-Rich Layered Oxide

Abstract: The electrode kinetics of Li-ion batteries, which are important for battery utilization in electric vehicles, are affected by the grain size, crystal orientation, and surface structure of electrode materials. However, the kinetic influences of the grain interior structure and element segregation are poorly understood, especially for Li-rich layered oxides with complex crystalline structures and unclear electrochemical phenomena. In this work, cross-sectional thin transmission electron microscopy specimens are “anatomized” from pristine Li1.2Mn0.567Ni0.167Co0.067O2 powders using a new argon ion slicer technique. Utilizing advanced microscopy techniques, the interior configuration of a single grain, multiple monocrystal-like domains, and nickel-segregated domain boundaries are clearly revealed; furthermore, a randomly distributed atomic-resolution Li2MnO3-like with an intergrown LiTMO2 (TM = transitional metals) “twin domain” is demonstrated to exist in each domain. Further theoretical calculations based on...

Ferromagnetic behaviour of ZnO: the role of grain boundaries

Abstract: The possibility to attain ferromagnetic properties in transparent semiconductor oxides such as ZnO is very promising for future spintronic applications. We demonstrate in this review that ferromagnetism is not an intrinsic property of the ZnO crystalline lattice but is that of ZnO/ZnO grain boundaries. If a ZnO polycrystal contains enough grain boundaries, it can transform into the ferromagnetic state even without doping with “magnetic atoms” such as Mn, Co, Fe or Ni. However, such doping facilitates the appearance of ferromagnetism in ZnO. It increases the saturation magnetisation and decreases the critical amount of grain boundaries needed for FM. A drastic increase of the total solubility of dopants in ZnO with decreasing grain size has been also observed. It is explained by the multilayer grain boundary segregation.

Size Effect of Porous Media on Methane Hydrate Formation and Dissociation in an Excess Gas Environment

Abstract: In this fundamental study, we examined the effect of silica sand grain size on methane hydrate formation under the excess gas formation approach method. The behavior of methane hydrate formation in four sizes of silica sands ranging from sand–silt cut off size (0.063 mm) to granular pebble (3.0 mm) was examined to capture the particle size range found in natural hydrate samples. With the exception of the smallest grain size (0.063–0.18 mm), significant gas uptake was observed in all three sand sizes within the given experimental time of 70 h, and some unexpected formation behavior was seen in the coarse sands (0.56–1.3 mm) and granular samples (1.5–3.0 mm), where significant amounts of methane hydrate were observed to form on top of the porous media instead of dispersed within the porous media. This observation highlights the importance in selecting an appropriate porous medium and experimental approach to synthesize artificial methane hydrate in the laboratory for production tests, especially for reactor...

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.

Ductilisation of tungsten (W): On the shift of the brittle-to-ductile transition (BDT) to lower temperatures through cold rolling

Abstract: Here we show that cold rolling decreased the brittle-to-ductile transitions (BDT) temperature of tungsten (W). Furthermore, we show that the BDT temperature correlates with the grain size (the smaller the grain size, the lower the BDT temperature) following a Hall–Petch-like equation. This relation between the grain size and the BDT temperature is well known from ferrous materials and is generally accepted in the steel community. Our ductilisation approach is the modification of the microstructure through cold rolling. In this work, we assess three different microstructures obtained from (i) hot-rolled, (ii) cold-rolled, and (iii) hot-rolled and annealed (1 h/2000 °C, annealed in H2) tungsten plates. From these plates, Charpy impact test samples with dimensions of 1 × 3 × 27 mm3, without notch, were cut and tested in the L-S and T-S directions. The results show the following BDT temperatures: 675 °C/948 K (L-S, “annealed”), 375 °C/648 K (L-S, “hot-rolled”) and 125 °C/398 K (L-S, “cold-rolled”). The microstructure of the plates is analysed by means of SEM (EBSD: grain size, subgrains, texture, KAM), FIB (channelling contrast) and TEM analyses (bright field imaging). The question of how cold rolling decreases the BDT temperature is discussed against the background of (i) microcracking, crack branching, and crack bridging effects; (ii) texture effects; (iii) the role of dislocations; and (iv) the impact of impurities, micropores, and sinter pores. Our results suggest that the availability of dislocation sources (dislocation boundaries, grain boundaries; in particular, IDBs and HAGBs) is the most important parameter responsible for the increase of the cleavage resistance stress, σF, or the decrease of the BDT temperature, respectively.

Influence of Friction Stir Processed Parameters on Superplasticity of Al-Zn-Mg-Cu Alloy

Abstract: Friction stir processing (FSP) is a novel technique for refining the microstructure. In this study, the effect of FSP process parameters such as tool rotation, traverse speed and tool tilt on resulting grain size, microstructure and superplastic behavior of high-strength thick Al-Zn-Mg-Cu alloy is reported. The microstructure examination of the stir zone (SZ) was performed by optical as well as scanning electron microscope. Microstructure variation attributed to different process parameters is reflected in the SZ. It is observed that grain size increases with increasing tool rotation speed, and decreases with increasing traverse speed. However, tool tilt has no significant effect on grain size. Moreover, at higher tool tilt distorted grains were observed in microscopic images. The highest average value of hardness in the SZ is obtained for low heat input value corresponding to higher tool rotation and traverse speed. In this study, hardness has shown no dependency on the grain size of the SZ due to the st...