Cyclic high-pressure torsion of nickel and Armco iron

Cyclic high-pressure torsion, a modified version of high-pressure torsion, is applied to Armco iron and nickel. The results in terms of microstructure and flow stress are compared to samples deformed by conventional high-pressure torsion. For both processes and both materials, a saturation in the decrease of the structure size and the increase in the flow stress is observed. The minimum size of the structural elements which is obtainable is smallest for the conventionally high-pressure torsion deformed samples and increases with decreasing strain per cycle in cyclic high-pressure torsion.     

High-pressure torsion applied to nickel single crystals

Nickel single crystals with different crystallographic orientations were deformed by high-pressure torsion. Special attention is devoted to examining the evolution of the micro-texture and microstructure. The initial crystal orientation was found to have a significant effect on the mechanical hardening and evolution of micro-texture at low and medium equivalent strains, whereas at very high strains no effect of the initial orientation was observed and the behaviour was very similar to a polycrystal. The evolution of micro-texture is in good qualitative agreement with the full constrained Taylor model. At very high equivalent strains the initial crystal orientation has no influence on micro-texture. At such strains, the hardening, the refinement of the structure and the texture reaches a saturation. The final micro-texture is explained by the change from one preferred crystallographic orientation to another.     

Texture of bismuth telluride-based thermoelectric semiconductors processed by high-pressure torsion

P-type Bi₂Te₃-based thermoelectric semiconductors were prepared, having a grain-refined microstructure and a preferred orientation of anisotropic crystallographic structure. Disks with a nominal composition of Bi_0.5Sb_1.5Te_3.0 were cut from an ingot grown by the vertical Bridgman method (VBM) and deformed at 473 K under a pressure of 6.0 GPa by high-pressure torsion (HPT). The crystal orientation was characterized by X-ray diffraction. The microstructures were characterized using optical microscopy and scanning electron microscopy (SEM). It was found that the HPT disks had a fine and preferentially oriented grain compared to that of the VBM disks. Further, the power factor of the HPT disks was about twice as large as that of the VBM disks. These results indicate that HPT is effective in improving the thermoelectric properties of Bi₂Te₃-based thermoelectric semiconductors.     

Microstructural evolution of tungsten oxide thin films

Tungsten oxide thin films are of great interest due to their promising applications in various optoelectronic thin film devices. We have investigated the microstructural evolution of tungsten oxide thin films grown by DC magnetron sputtering on silicon substrate. The structural characterization and surface morphology were carried out using X-ray diffraction and Scanning Electron Microscopy (SEM). The as deposited films were amorphous, where as, the films annealed above 400 °C were crystalline. In order to explain the microstructural changes due to annealing, we have proposed a “instability wheel” model for the evolution of the microstructure. This model explains the transformation of mater into various geometries within them selves, followed by external perturbation.     

液氮冷却条件下激光快速熔凝Ni-28 wt%Sn合金组织演变

研究了在液氮冷却条件下激光快速熔凝Ni-28 wt%Sn亚共晶合金的组织演化过程. 结果显示, 熔池从上至下可以分为三个区域: 表层为平行激光扫描方向的α-Ni转向枝晶区; 中部为近乎垂直于熔池底部外延生长的α-Ni柱状晶区; 底部为少量的残留α-Ni初生相和大量的枝晶间(α-Ni+Ni₃Sn) 共晶组织. 激光熔凝区组织受原始基材组织的影响很大, 熔池中的α-Ni枝晶生长方向受到了热流方向和枝晶择优取向的双重影响. 与基材中存在的层片状、棒状和少量离异(α-Ni+Ni₃Sn)共晶的混合组织相比, 熔池内的共晶组织皆为细小的规则(α-Ni+Ni₃Sn)层片状共晶, 皆垂直于熔池底部外延生长, 并且从熔池顶部至底部, 共晶层片间距逐渐增大. 分别应用描述快速枝晶生长的Kurz-Giovanola-Trivedi 模型和描述快速共晶生长的Trivedi-Magnin-Kurz模型对熔池表层凝固界面前沿的过冷度进行估算, 发现熔池表层α-Ni 枝晶和(α-Ni+Ni₃Sn)层片共晶的生长过冷度在50.4-112.5 K 之间, 远大于相应深过冷凝固(α-Ni+Ni₃Sn) 反常共晶生长的临界过冷度20 K, 这说明文献报道的临界过冷度并不是反常共晶出现的充分条件.     

Microstructural evolution upon annealing in Ar-implanted Si

The annealing effects of crystalline silicon (Si) implanted with argon (Ar) ions at a dose of 2 × 10¹⁶ Ar⁺/cm² at room temperature and subsequently annealed at 400-1100 °C for 30 min were investigated. The samples were analyzed by transmission electron microscopy and Raman spectroscopy. Before and after annealing up to 600 °C, an amorphous layer is formed but Ar bubbles are not observed in the damage layer. After annealing at 800 °C, argon bubbles are observed together with extended defects. The damage layer evolves into a polycrystalline structure. After annealing at 1100 °C; exfoliation occurs on the sample surface, and microtwin lamellas form in the damage layer. Raman scattering revealed that a strong recrystallization occurs from 600 °C to 800 °C. The results were compared with the case of helium implantation, with particular focus on bubble formation mechanisms.     

Microstructural evolution of pure copper during friction-stir welding

The microstructural evolution of pure copper during friction-stir welding was found to be principally influenced by welding temperature. At temperatures below ~0.5 T_m (where T_m is melting point), the microstructure was shown to be essentially determined by continuous recrystallization, leading to significant grain refinement and related material strengthening in the stir zone. In contrast, grain structure development at temperatures above ~0.5 T_m was dominated by discontinuous recrystallization producing a relatively coarse grain structure in the stir zone and giving rise to material softening.     

Microstructural evolution during containerless rapid solidification of Co-Si alloys

The Co-12%Si hypoeutectic, Co-12.52%Si eutectic and Co-13%Si hypereutectic alloys are rapidly solidified in a containerless environment in a drop tube. Undercoolings up to 207K (0.14T_E) are obtained, which play a dominant role in dendritic and eutectic growth. The coupled zone around Co-12.52%Si eutectic alloy has been calculated, which covers a composition range from 11.6 to 12.7%Si. A microstructural transition from lamellar eutectic to divorced eutectic occurs to Co-12.52%Si eutectic droplets with increasing undercooling. The lamellar eutectic structure of the Co-12.52%Si alloy consists of εCo and Co_3Si phases at small undercooling. The Co_3Si phase cannot decompose completely into εCo and αCo_2Si phases. As undercooling becomes larger, the Co_3Si phase grows very rapidly from the highly undercooled alloy melt to form a divorced eutectic. The structural morphology of the Co-12%Si alloy droplets transforms from εCo primary phase plus lamellar eutectic to anomalous eutectic, whereas the microstructure of Co-13%Si alloy droplets experiences a `dendritic to equiaxed' structural transition. No matter how large the undercooling is, the εCo solid solution is the primary nucleation phase. In the highly undercooled alloy melts, the growth of εCo and Co_3Si phases is controlled by solutal diffusion.     

First-principles investigation on high-pressure structural evolution of MnTiO3

First-principle calculations using density-functional theory with linearized augmented plane wave method and projector-augmented method have been performed for the high-pressure MnTiO₃ polymorphs and their possible dissociation products. Theoretical results demonstrate that ilmenite-type MnTiO₃ transforms into perovskite phase at 27 GPa and 0 K. The lithium niobate phase of MnTiO₃ is confirmed to be metastable according to its higher Gibbs free energy compared with that of ilmenite at ambient conditions. In ilmenite and lithium niobate phases, MnO₆ octahedra become more distorted while TiO₆ octahedra become more regular with increasing pressure. In orthorhombic perovskite phase, the structural distortion deviated from the ideal cubic perovskite is enhanced at higher pressure. Based on the non-spin-polarized calculations, perovskite phase MnTiO₃ is predicted to dissociate into Fm3?m-MnO+P2₁/c-MnTi₂O₅ at 29 GPa.     

Non-enzymatic modifications of proteins under high-pressure treatment

High-pressure treatment, e.g. used as an alternative method for food preservation, affects protein cross-linking and glycation reactions. These reactions were monitored by using mainly milk proteins in the absence and presence of different saccharides or dicarbonyl compounds. Without carbohydrates, protein cross-linking of casein is enhanced by pressure through the formation of dehydroalanine-derived lysinoalanine. A similar effect can be observed in wool, where pressure accelerates the formation of lanthionine. In contrast, saccharide or dicarbonyl compound-induced cross-linking is constrained by high pressures. Despite this, pressure is able to accelerate the degradation of sugar or carbonyl compounds, as could be seen by the measurement of their residual contents in the examined test preparations.     

Microstructural evolution in metals during helium and proton irradiations

Abstract

Recent investigations of helium-implanted and proton irradiated metals at medium temperatures (T≤100°C) have demonstrated the importance of high energy cascade effects for the microstructural evolution. They can effect the formation and the evolution of He densities in small bubbles formed by He implantation and are important also for the formation of periodic walls of defect clusters, a phenomenon observed under proton irradiations. Experimental results obtained by transmission electron microscopy and differential dilatometry for MeV irradiations of Cu and Ni are summarized and compared with observations after heavy-ion and neutron irradiations.     

Annealing behaviour of nanocrystalline NiTi (50 at% Ni) alloy produced by high-pressure torsion

An equiatomic nanocrystalline NiTi alloy, deformed by high-pressure torsion (HPT), was investigated. The as-prepared bulk NiTi alloy consisted of both amorphous and nanocrystalline phases. Crystallization and structural changes during annealing were investigated by differential scanning calorimetry (DSC), X-ray diffraction (XRD) and transmission electron microscopy (TEM). DSC thermograms and X-ray analyses revealed stress relaxation and partial crystallization below 500?K, while grain growth of the nanocrystals occurred predominantly after heating to temperatures above 573?K. Along with the amorphous phase crystallization, a continuous growth of pre-existing nanocrystals that are retained after HPT was observed. The DSC signals observed during continuous heating experiments indicate an unusually large separation between the crystallization and growth stages. A detailed analysis of the evolution of the enthalpy release upon annealing revealed reproducibly non-monotonous trends with annealing temperature that cannot be explained solely by nucleation and growth of crystalline volume fractions. Instead, the results can be rationalized by assuming a reverse amorphization process occuring during annealing at 523?K. This behavior, which also caused a large variation in nanocrystal size after annealing at higher temperatures, is discussed with respect to the nanoscale microstructural heterogeneity after initial deformation processing.     

Evidence for a transition in deformation mechanism in nanocrystalline pure titanium processed by high-pressure torsion

Nanocrystalline titanium with an average grain size of about 60–70 nm was prepared by high-pressure torsion. The results of hardness and structural evolutions indicate that a strain-induced hardening–softening–hardening–softening behaviour occurs. For coarse-grained titanium, 〈a〉-type dislocation multiplication, twinning and a high pressure-induced α-to-ω phase transformation play major roles to accommodate deformation, leading to a significant strain hardening. As deformation proceeds, dynamic recrystallisation leads to a decrease in dislocation density, especially for 〈a〉-type dislocations, leading to a slight strain softening. The 〈c〉-component dislocation multiplication dominates the deformation when the grain size decreases to 100 nm and 〈c〉-component dislocation multiplication, grain refinement and the α-to-ω phase transformation contribute to the second strain hardening. The following strain softening is attributed to dynamic recovery.     

Effect of temperature on solid-state formation of bulk nanograined intermetallic Al3Ni during high-pressure torsion

A bulk form of nanograined intermetallic Al₃Ni was produced by severe plastic deformation using high-pressure torsion (HPT). Powder mixtures of 75?mol% Al and 25?mol% Ni were processed by HPT at a selected temperature in the range of room temperature (RT) to 573?K under a pressure of 6?GPa. X-ray diffraction analysis revealed that the Al₃Ni intermetallic formed after processing for 50 revolutions at RT but, as the processing temperature increased, less revolutions (i.e. lower imposed strain) were required for the formation of Al₃Ni. Observations by transmission electron microscopy showed that the microstructure consists of ultrafine grains having a size of 300–2000?nm after 3 and 10 revolutions. Once the Al₃Ni formed after a higher number of revolutions, equiaxed nanograins with a size of ~30?nm prevailed with a significant increase in hardness. The increase in hardness was more significant when processed at higher temperatures because of increasing the fraction of Al₃Ni. It was shown that the solid-state formation of Al₃Ni occurred due to enhanced diffusion (i.e. decreased activation energy for diffusion) through the presence of high density of lattice defects.     

Superplasticity of a microcrystalline aluminum-lithium alloy under torsion

The deformation of an aluminum-lithium alloy under torsion in the temperature range 523–673 K at angular velocities of 0.322 and 0.0322 rad/s is studied. The shear strain γ prior to failure is found to increase with decreasing strain rate, and its temperature dependence has a maximum at 553 K (γ≈30). The initial loading-induced jump in the dependence of the torque on the angle of rotation (stress-strain curve) is followed by a softening stage, which changes into a hardening stage or a stage with a constant torque at all temperatures except those near 673 K. The stress distribution over a cross section is analyzed, and the dependence of the shear-strain rate \(\dot \gamma \) on the stress τ and temperature T is found to be \(\dot \gamma \sim \tau ^n \exp ( - {U \mathord{\left/ {\vphantom {U {kT}}} \right. \kern-\nulldelimiterspace} {kT}})\). The results are compared with those obtained earlier from tensile tests of this alloy.