High temperature deformation and extended plasticity in Mg single crystals

The high temperature deformation behavior of Mg single crystals was precisely investigated using orientation imaging microscopy. For this purpose, Mg single crystals of various orientations were tensile tested in vacuum at temperatures between 473 and 673?K. A strain rate of 4.2?×?10^?4?s^?1 was employed. The elongations to fracture depended strongly on crystal orientation, the lowest fracture strains being associated with multiple slip. Single crystals in which single slip was activated exhibited extended ductilities corresponding to more than 1.5 in true strain. The strong orientation dependence of the ductility can also be correlated with the ease of occurrence of dynamic recrystallization (DRX), which took place in the multiple-slip specimens. The role of twinning in the initiation of DRX is also discussed.     

Modelling and simulation of dynamic recrystallisation based on multi-phase-field and dislocation-based crystal plasticity models

ABSTRACT

The mechanical properties of metals used as structural materials are significantly affected by hot (or warm) plastic working. Therefore, it is industrially important to predict the microscopic behaviour of materials in the deformation process during heat treatment. In this process, a number of nuclei are generated in the vicinity of grain boundaries owing to thermal fluctuation or the coalescence of subgrains, and dynamic recrystallisation (DRX) occurs along with the deformation. In this paper, we develop a DRX model by coupling a dislocation-based crystal plasticity model and a multi-phase-field (MPF) model through the dislocation density. Then, the temperature dependence of the hardening tendency in the recrystallisation process is introduced into the DRX model. A multiphysics simulation for pure Ni is conducted, and then the validity of the DRX model is investigated by comparing the numerical results of microstructure formation and the nominal stress–strain curve during DRX with experimental results. The obtained results indicate that in the process of DRX, nucleation and grain growth occur mainly around grain boundaries with high dislocation density. As deformation progresses, new dislocations pile up and subsequent nucleation occurs in the recrystallised grains. The influence of such microstructural evolution appears as oscillation in the stress–strain curve. From the stress–strain curves, the temperature dependence in DRX is observed mainly in terms of the yield stress, the hardening ratio, and the change in the hardening tendency after nucleation occurs.     

Shear‐Enhanced Nucleation of Isotactic Polypropylene in Limited Space

The nucleation rate was measured by directly counting the number of nuclei, which were developed while an isotactic polypropylene melt was flowing under shear in a thin film. The nucleation rate was enhanced with an increased rate of shear, e.g., by a factor of 10 larger at the rate of shear of 14 s^?1 compared with the quiescent state, at 134°C. The ratio of the shear‐enhanced nucleation rate to the nucleation rate in the quiescent state was larger at a higher temperature of crystallization, i.e., about 10 times at 134°C to 590 times at 140°C. The increase of the nucleation rate under shear flow was explained by a reduction of the lateral and end (fold) surface free energies; the product σ _s ² σ _e decreased to 3.2×10^?7 for the sheared melt, from 6.0×10^?7 (J m^?2)³ for the isotropic state. The free energy reduction was caused by transition of the nucleus formation mode from three‐dimensional folded chain nuclei to two‐dimensional bundle nuclei, in which chains lie down on the glass substrate, aligning parallel to the flow direction.     

The dehydration kinetics of gypsum at high pressure and high temperature

An in situ dehydration kinetics study of gypsum under water-saturated condition was performed in the temperature and pressure ranges of 383–423?K and 343–1085?MPa by using a hydrothermal diamond anvil cell and Raman spectroscopy. Kinetic analysis shows that the dehydration rate k increases with pressure, suggesting a negative pressure dependence on dehydration rate. The elevation of temperature can contribute to the dehydration. The n values increase with pressure, indicating that the nucleation process becomes slower relative to the growth process. According to the n values of ～1.0, the dehydration of gypsum is dominated by an instantaneous nucleation and diffusion-controlled growth mechanism. The obtained average activation volume ?V is equal to 5.69?cm³/mol and the calculated activation energy E_a and the pre-exponential factor A are 66.9?kJ/mol and 4.66?×?10⁵?s^?1. The activation energy may be dependent upon grain size, shape, temperature and pressure, and surrounding water.     

Strength and plastic deformation of polycrystalline diamond composites

ABSTRACT

The use of nanopolycrystalline diamond has allowed a systematic study on deformation of polycrystalline diamond composites (PCDCs). Bulk PCDCs samples containing either Co or SiC as a binding agent were deformed under high pressure and temperature to strains up to 18% at strain rates ～10^?5?s^?1. All samples exhibit strong work hardening. The strength of PCDCs depends on the amount and type of binding agents and is consistently weaker than that of diamond single crystals. The weakening may be due to the binder materials, which play an important role in affecting grain boundary structures. In SiC-based PCDC, significant grain fragmentation occurs. Nearly all grain boundaries are wetted by SiC after large deformation, resulting in lower strength. In Co-based PCDC, the microstructure is dominated by dislocations, deformation twins, and separated grain boundaries. The density of deformation twins increases significantly with strain, with the twin domain width reaching as low as 10–20?nm at 14% strain.     

Effect of solute atoms on grain boundary sliding in magnesium alloys

The effect of solid-solution alloying on grain boundary sliding (GBS) was investigated using pure magnesium and six kinds of Mg–X (X?=?Ag, Al, Li, Pb, Y and Zn) dilute binary solid solutions with an average grain size of 10?µm. A sharp increase in damping capacity caused by GBS was observed above a certain temperature. The temperature at which a sharp increase in damping capacity occurred depended on the alloying element. The addition of Y and Ag markedly increased the onset temperature (more than 100?K) for a sharp increase in damping capacity, whereas the addition of Zn, Al and Li slightly increased the onset temperature (less than 50?K) as compared with that for pure magnesium. Tensile tests at a temperature of 423?K revealed that the higher the onset temperature, the lower the strain rate sensitivity of the flow stress. It is suggested that the former elements (Y and Ag) are more effective in suppressing GBS in magnesium alloys than the latter ones (Zn, Al and Li). The suppression of GBS was associated with low grain boundary energy, and the extent to which the energy is reduced depended on the alloying element. It was suggested that the change in the lattice parameter (the so-called c/a ratio) affects the grain boundary energy, and thus, the occurrence of GBS.     

Low-temperature fatigue behaviour and development of dislocation structure in aluminium single crystals with single-slip orientation

Al single crystals oriented for single slip were cyclically deformed under constant plastic strain amplitudes between 1?×?10^?3 and 5?×?10^?2 at 77?K. Al single crystals showed hardening to saturation at all applied shear stress amplitudes. The resultant cyclic stress–strain curve (CSSC) showed a stress plateau in a range of plastic strain amplitude from 2?×?10^?3 to 2?×?10^?2. Surface observation revealed that multiple slip systems were active even at the strain amplitude in the plateau region. At plastic strain amplitudes corresponding to the plateau of the CSSC, persistent slip bands (PSBs) were formed parallel to the primary slip plane. In the PSBs, well-developed dislocation walls parallel to the {100} planes were observed. The microstructure in the PSBs was explained by the fact of multiple activation of the primary and critical slip systems. The above results indicate that the high stacking fault energy of Al is an important factor affecting the fatigue behaviour even at 77?K.     

Hardening and thermal stability of nanocrystalline AlMg4.8 powder

Ball milled nanocrystalline AlMg4.8 powder was investigated in terms of hardening and thermal stability. The validity of the Hall–Petch relation was confirmed down to the minimum grain size of ～44 nm. Prolonged milling in the range of the minimum grain size still increased the hardness. This development is discussed in terms of contamination effects and the influence of full and partial dislocations. Concerning thermal stability, recovery processes occur in the range of 100–230°C, whereas substantial grain growth starts at a temperature of ～250°C. The enthalpy release for recovery was detected to be ～39 J mol^?1 and ～208 J mol^?1 for grain growth. Dynamic strain ageing was indicated by an activation energy for recovery of Q?～?120 kJ mol^?1. The activation energy of grain growth was calculated by means of the Kissinger theory (Q?=?200–210 kJ mol^?1) and using the results of static grain growth (Q?=?204 kJ mol^?1).     

Geometric dynamic recrystallization of austenitic stainless steel through linear plane-strain machining

ABSTRACT

Type 316L austenitic stainless steel was severely plastically deformed at room temperature using linear plane-strain machining in a single pass that imparted shear strains up to 2.2 at strain rates up to 2?×?10³ s^?1. The resulting microstructures exhibited significant grain size refinement and improved mechanical strength where geometric dynamic recrystallization was identified as the primary microstructural recrystallization mechanism active at high strain rates. This mechanism is rarely observed in low to medium stacking fault energy materials. The critical stress required for twin initiation is raised by the combined effects of refined grain size and the increase in stacking fault energy due to the adiabatic heating of the chip, thus permitting geometric dynamic recrystallization. The suppression of martensite formation was observed and is correlated to the significant adiabatic heating and mechanical stabilisation of the austenitic stainless steel. A gradient of the amount of strain induced martensite formed from the surface towards the interior of the chip. As the strain rate is increased from 4?×?10² s^?1–2?×?10³ s^?1, a grain morphology change was observed from a population of grains with a high fraction of irregular shaped grains to one dominated by elongated grain shapes with a microstructure characterised by an enhanced density of intragranular sub-cell structure, serrated grain boundaries, and no observable twins. As strain rates were increased, the combination of reduction in strain induced martensite and non-uniform intragranular strain led to grain softening where a Hall-Petch relationship was observed with a negative strengthening coefficient of ?0.08?MPa m^1/2.     

Effect of alloying elements on room temperature tensile ductility in magnesium alloys

The impact of alloying elements on the room temperature tensile behaviour was investigated for a wide range of strain rates using eight types of extruded Mg-0.3 at.% X (X = Ag, Al, Li, Mn, Pb, Sn, Y and Zn) binary alloys with an average grain size of 2–3 μm. The solid solution alloying element affected not only tensile plasticity but also rate-controlling mechanism for these fine-grained magnesium alloys. Most of the alloys exhibited an elongation-to-failure of 20–50% , while the alloys with a high m-value exhibited large tensile plasticity, such as an elongation-to-failure of 140% in a strain rate of 1 × 10^?5 s^?1 for the Mg–Mn alloy. This elongation-to-failure is more than two times larger than that for pure magnesium. This is due to the major contribution of grain boundary sliding (GBS) on the deformation. Microstructural observations reveal that grain boundary segregation, which is likely to affect gain boundary energy, plays a role in the prevention or enhancement of GBS. The present results are clearly expected to open doors to the development of magnesium alloys with good secondary formability at room temperature through the control of alloying elements.     

Brittle fracture in 50Mo–50Re alloys during slow strain rate tensile testing

Tensile tests were conducted on 50 wt% Mo–50 wt% Re alloys in both fully recrystallized and recovery heat-treated conditions at a low strain rate of 10^?6 s^?1 and room temperature in air. It was found that both material conditions exhibited predominantly cleavage fracture with significant intergranular secondary cracking, compared to the predominantly ductile fracture found in the alloys at a higher strain rate. Cracks were often initiated at grain boundary triple junctions at the low strain rate. Electron backscatter diffraction (EBSD) measurements revealed significantly high misorientation gradients (i.e. highly localized change in orientation) at grain boundaries, especially in the vicinity of some grain boundary triple junctions in the deformed alloys. Transmission electron microscopy (TEM) results verified the existence of significant misorientations near grain boundaries in these alloys. Stress-assisted dynamic embrittlement, possibly due to trace interstitials, was the possible cause of brittle fracture in the 50Mo–50Re alloys at the low strain rate.     

Kinetics of high-temperature deformation of polycrystalline OFHC copper and the role of dislocation core diffusion

The mechanisms of the high-temperature deformation of oxygen-free high-conductivity (OFHC) copper have been evaluated over a wide temperature (300–950°C) and strain rate (0.001–100?s^?1) regime. The stress–strain behaviour in hot compression is typical of the occurrence of dynamic recrystallization with an initial peak in the flow stress followed by a steady state, preceded by oscillations at lower strain rates and higher temperatures. The results are analysed using the kinetic rate equation involving a hyperbolic sine relation of the steady-state flow stress with the strain rate. In the temperature and strain rate range covering 500–950°C and 0.001–10?s^?1, a stress exponent of 5 and an apparent activation energy of 145?kJ/mol were evaluated from this analysis. The power law relationship also yielded similar values (5.18 and 152?kJ/mol, respectively). On the basis of these parameters, the rate-controlling mechanism is suggested to be dislocation core diffusion. The flow stress for the OFHC copper data reported by earlier investigators for different oxygen contents is consistent with the above analysis and revealed that an oxygen content of less than about 40?ppm does not have any significant effect on the core diffusion since it is too low to ‘clog’ the dislocation pipes. At strain rates greater than 10?s^?1 and in the temperature range 750–950°C, the stress exponent is about 3.5 and the apparent activation energy is 78?kJ/mol, which suggests that the plastic flow is controlled by grain boundary diffusion.     

Nucleation kinetics for gold deposited onto mica substrates

The nucleation behavior of gold deposited under ultra high vacuum conditions onto cleaved mica substrates has been measured over the temperature range 270–450 °C at impingement fluxes of 6 × 10¹³ and 8 × 10¹² atoms cm^?2sec^?1. A step-kinetic technique was used wherein separate substrate areas were exposed for successively longer times to the vapor beam from a thermal source. The deposits were examined in a high resolution electron microscope. For mica cleaved in situ in UHV, the variation in number density of nuclei with time of exposure to the atom beam revealed that nucleation occurred rapidly on preferred sites which were exhausted within the first few seconds of exposure. After the initial saturation, nucleation appeared to occur randomly over the rest of the surface. The number density of preferred sites increased with decreasing temperature indicating that a spectrum of preferred sites of varying degrees of potency were active. The random nucleation rates could by analyzed satisfactorily using the atomistic model for nucleation. A critical sized nucleus consisting of one atom is consistent with the data. The characteristic energy for nucleation (2ΔG_des ?ΔG_sd), was found to be 1.1 eV. Nucleation behavior on mica substrates cleaved in air did not indicate the presence of active preferred sites, but nucleation was more rapid.     

Study of complex impedance spectroscopic properties of the KFeP2O7 compound

The KFeP₂O₇ compound was prepared by the conventional solid-state reaction. The sample was characterized by X-ray powder diffraction. The AC electrical conductivity and the dielectric relaxation properties of this compound have been investigated by means of impedance spectroscopy measurements over a wide range of frequencies and temperatures, 200 Hz–5 MHz and 553–699 K, respectively. Both impedance and modulus analysis exhibit the grain and grain boundary contribution to the electrical response of the sample. The temperature dependence of the bulk and grain boundary conductivity were found to obey the Arrhenius law with activation energies Eg?=?0.94 (3)?eV and Egb?=?0.89 (1)?eV. The grain-and-grain boundary conductivities at 573 K are 1.07?×?10^?4 and 1.16?×?10^?5 (Ω^?1 cm^?1). The scaling behavior of the imaginary part of the complex impedance suggests that the relaxation describes the same mechanism at various temperatures. The near value of the activation energies obtained from the equivalent circuit, conductivity data, and analysis of M″ confirms that the transport is through ion hopping mechanism.     

Observations of glide and decomposition of a⟨101⟩ dislocations at high temperatures in Ni-Al single crystals deformed along the hard orientation

Ni-44 at.% Al and Ni-50 at.% Al single crystals were tested in compression in the hard d001 ¢orientation. The dislocation processes and deformation behaviour were studied as a function of temperature, strain and strain rate. A slip transition in NiAl occurs from a?111? slip to non-a?111? slip at intermediate temperatures. In Ni-50 at.% Al single crystals, only a?010? dislocations are observed above the slip transition temperature. In contrast, a a?101?{101} glide has been observed to control deformation beyond the slip transition temperature in Ni-44 at.% Al. a?101? dislocations are observed primarily along both ?111? directions in the glide plane. High-resolution transmission electron microscopy observations show that the core of the a?101? dislocations along these directions is decomposed into two a?010? dislocations, separated by a distance of approximately 2 nm. The temperature window of stability for these a?101? dislocations depends upon the strain rate. At a strain rate of 1.4 210^?4 s^?1, a?101? dislocations are observed between 800 and 1000 K. Complete decomposition of a?101? dislocations into a?010? dislocations occurs beyond 1000 K, leading to a?010? climb as the deformation mode at higher temperatures. At lower strain rates, decomposition of a?101? dislocations has been observed to occur along the edge orientation at temperatures below 1000 K. Embedded-atom method calculations and experimental results indicate that a?101? dislocations have a large Peierls stress at low temperatures. Based on the present microstructural observations and a survey of the literature with respect to vacancy content and diffusion in NiAl, a model is proposed for a?101?{101} glide in Ni-44 at.% Al, and for the observed yield strength versus temperature behaviour of Ni-Al alloys at intermediate and high temperatures.     

Magnetic orientation of carbon nanotubes at temperatures of 231 K and 314 K

Carbon nanotubes were placed in magnetic fields of  80.0 kOe at temperatures of 231 K and 314 K. Scanning electron microscopy showed that nanotubes were oriented with the tube axis parallel to the fields. It was also observed that the probability of the orientation became higher, when the temperature was raised from 231 K to 314 K. The anisotropy in the susceptibilities parallel X∥ and perpendicular X _⊥ to the tube axis is suggested to increase with rise in temperature: X∥ ? X⊥ = (4 ± 2) × 10^?6 emu mol^?1 (per mol of carbon atoms) at 231 K and X∥ ? X⊥ = (45 ± 27) × 10^?6 emu mol^?1 at 314 K.     

Effects of damage rate on Cu precipitation in Fe–Cu model alloys under neutron irradiation

The formation of Cu precipitates and point defect clusters was investigated in two Fe–Cu binary model alloys, Fe–0.3Cu and Fe–0.6Cu, irradiated at 573?K at three different damage rates, namely 3.8?×?10^?10, 1.5?×?10^?8 and 5?×?10^?8?dpa (displacements per atom)/s, up to about 1.6?×?10^?2?dpa. Results of positron annihilation experiments indicated that Cu precipitates were formed in these irradiations with different damage rates. The growth of Cu precipitates does not increase monotonously with increasing irradiation dose, but it rather depends on the nucleation and growth of microvoids. It is also clear that the nucleation and growth of microvoids are influenced by the irradiation dose rate.     

The measurement of solid–liquid interfacial energy in colloidal suspensions using grain boundary grooves

Interfacial energy is a fundamental physiochemical property of any multi-phase system. Among the most direct approaches for determining solid–liquid interfacial energy is a technique based on measuring the shape of grain boundary grooves in specimens subjected to a linear temperature gradient. This technique was adapted to crystallizing colloids in a gravitational field. Such colloids exhibit a freezing–melting phase transition and are important not only as self-assembling precursors to photonic crystals, but also as physical models of atomic and molecular systems. The grain boundary groove technique was tested using suspensions of sterically stabilized poly(methyl methacrylate) spheres, which have been shown to closely approximate the hard sphere potential. Whereas isotropic models did not fit grain boundary groove data well, the capillary vector model, which is suitable for both isotropic and anisotropic surface energies, produced γ₁₁₀?=?0.58?±?0.05 k _B T/σ². This value of interfacial energy is in agreement with many of the published values for hard spheres, supporting the validity of our grain boundary groove technique adaptations to colloidal systems in a gravitational field. Finally, kinks observed in groove profiles suggest a minimum anisotropy parameter of ε?=?0.029 for hard spheres.     

A study of the α ↔ γ transformation in pure iron: rate variations revealed by means of thermal analysis

The α???γ transformation in nominally high purity Fe is shown to occur with a stepped peak in differential thermal analysis on both heating and cooling at rates between 0.5?K?min^?1 and 10?K?min^?1. The composite peaks mark changes in the transformation rate. To endorse the findings, the instrumental output has been thoroughly analyzed providing evaluations of time lags, suggestions for calibration and for the use of the derivative of the peak. The change in rate occurred in all samples irrespective of their grain size (average values from 91?µm to 1100?µm). The rate of movement of the interface in the α???γ transformation is estimated between 4?×?10^?5?m?s^?1 and 3?×?10^?6?m?s^?1. The present results extend previous dilatometric work in which the rate variation was detected only for large grain size and low undercooling. Possible reasons for the variation in rate are outlined: local development of strain in the austenite due to lattice misfit with respect of the growing ferrite, formation of a ragged microstructure and pinning of the boundaries by impurity.