Accelerating heterogeneous nucleation to increase hardness and electrical conductivity by deformation prior to ageing for Cu-4 at.% Ti alloy

ABSTRACT

Deformation bands, especially shear bands were intentionally formed in supersaturated Cu-4 at.% Ti alloy by groove-rolling with 75% area reduction. Cold deformation prior to the ageing process changed the precipitation behaviour of the alloy. The deformed structure with shear bands was maintained, without showing recovery and recrystallisation, even after prolonged ageing at 450°C for more than one day. The thermally stable shear bands act as nucleation initiation sites and prevent the expansion of discontinuous cellular precipitates. The hardness reached a value of 305?Hv and an electrical conductivity of 15% IACS (IACS?=?International Annealed Copper Standard. 100% IACS is defined as the conductivity corresponding to a volume resistivity at 20°C of 17.241?nΩ), compared to 283?Hv and 13% IACS for conventional solid-solutioned and peak-hardened alloy. In addition, the ageing time to reach the highest hardness was shortened from 720 to 180?min at 450°C.     

Influence of heat treatment on the microstructural evolution of Al–3 wt.% Cu during high-pressure torsion

Solution-treated, peak-aged and overaged samples of the model alloy Al–3?wt.% Cu, obtained by selective heat treatments of the pre-material, have been subjected to high-pressure torsion at room temperature and at 200?°C. The mechanical behaviour of the samples was investigated with torque measurements during deformation and microhardness measurements after deformation. Irrespective of the initial material condition, in the saturation regime a comparable equilibrium microstructure was found consisting of ultrafine aluminium grains stabilized by precipitates formed at grain boundaries.     

Enhancement of hardening and thermal resistance of Mg–Sn-based alloys by addition of Cu and Al

Mg–Sn-based alloys are considered as a promising precipitation-hardening system for applications at elevated temperatures, but the hardening effect is not satisfactory owing to sluggish nucleation and rapid coarsening of the major Mg₂Sn lath precipitates. In this study, Cu and Al are added to a Mg–6Sn–1Mn base alloy. The age-hardening response and the microstructures of these modified alloys have been investigated and are compared to that of the base alloy. The additional elements are found to bring several beneficial effects to the alloys for applications at elevated temperatures. Firstly, a eutectic structure consisting of strong intermetallic phases, i.e. Mg₂Cu in the Mg–6Sn–1Mn–2Cu alloy and Al_0.93Cu_1.07Mg in the Mg–6Sn–1Mn–2Cu–2Al alloy, remains stable along the grain boundaries after solution and ageing heat treatments. Secondly, the precipitate density has been increased significantly and the precipitate size has been refined remarkably during ageing at 200?°C. Moreover, the growth of the precipitates is inhibited remarkably during the over-ageing period. Therefore, the age-hardening response and over-ageing resistance are notably improved.     

Early stage of Al3Zr precipitation in a rapidly solidified Al-Cr-Zr alloy

Abstract

Early stages of A1₃Zr precipitation have been studied in detail in the ternary Al-2.4 at.% Cr-1.1 at.% Zr alloy. A supersaturated solid solution of Zr in the asrapidly solidified state decomposes during subsequent heat treatment at 400°C. This decomposition leads to a homogeneous precipitation of very small Al₃Zr (LI₂) particles in the grain interior, but this homogeneous precipitation is not stable in the vicinity of mobile grain boundaries and is progressively consumed, giving rise to a fan-shaped precipitation of Al₃Zr (Ll₂), often coexisting with very small interlamellar particles of Al₃Zr (LI₂). All these precipitation modes are analysed in the light of the current theory of discontinuous reactions.     

Grain orientation effects on delamination during fatigue of a sensitized Al–Mg alloy

Fatigue crack growth experiments were conducted in humid air (RH~45%) at 25 °C on 29-mm-thick plate samples of an aluminium–magnesium (Al–Mg) 5083-H131 alloy in the long transverse (LT) direction. Samples were tested in both the as-received condition and after sensitization at 175 °C for 100 h. Delamination along some grain boundaries was observed in the short transverse plane after fatigue testing of the sensitized material, depending upon the level of ΔK and K_max. Orientation microscopy using electron backscattering diffraction and chemical analyses using transmission electron microscopy and energy dispersive spectroscopy of grain boundaries revealed that Mg segregation and the orientation of grains had key roles in the observed grain boundary delamination of the sensitized material.     

Interfacial strengthening of β phase in a fully lamellar structure of TiAl alloy containing W

The strengthening of the β phase in two fully lamellar structures with different lamellar spacing of a Ti–48?at.%?Al–2?W?at.% alloy during creep deformation has been investigated. It was found that the β phase precipitates during aging treatments only within regions of α₂ lamellae following their dissolution. The strengthening of the β phase is more effective in the coarser lamellar structure, because the wider β precipitation zones, which replace the prior coarser α₂ lamellae, hinders dislocation motion stronger than the narrower ones.     

Increasing toughness by promoting discontinuous precipitation in Cu–Ni–Si alloys

The influence of precipitation morphology, including continuous precipitation (CP) and discontinuous precipitation (DP), on the mechanical behaviour of Cu–Ni–Si alloys was studied. The Cu–6Ni–1.5Si (in wt%) alloy was solution heat treated at 980 °C for 2 h and aged at 500 °C for 0.5 and 3 h to produce CP and DP structures. The DP specimen showed an abnormal increase in tensile ductility with increasing strain rate, unlike the CP counterpart. The impact toughness of the DP specimen was 1.6 times greater than that of CP specimen. The fracture mode in DP specimen was mostly dimpled rupture, while the mixed mode of cleavage fracture and dimpled rupture was noted on the CP specimen.     

Epifluorescence optical microscopy: a sensitive tool for determining the spatial distribution of europium-dihalide precipitates in KCl : KBr : Eu2+ crystals

The spatial distribution of europium-dihalide-type precipitates in KCl?:?KBr?:Eu²⁺ single crystals annealed at 200°C for long periods of time was determined by epifluorescence optical microscopy. Laue-type patterns and optical spectroscopy were used to test the degree of long-range ordering of the specimens and to monitor the precipitation during annealing, respectively. Precipitates smaller than about 0.08?µm were found (2.84?×?10¹² precipitates cm^?3) all across the host, whereas larger precipitates of about 0.17?µm were found (2.9?×?10⁴ precipitates cm^?1) along certain linear structural singularities of the matrix. These singularities, identified as crystal dislocations, were observed to terminate always either at a triple node of singularities or at the crystal surface, forming a three-dimensional network of crystal singularities (2.0?×?10⁶ singularities cm^?2), identified as the Frank network. The presence of europium exhaustive matrix zones accompanying the observed europium-decorated paths indicates that impurity segregation processes, occurring during annealing, favour the precipitation phenomena.     

Self-diffusion activation energies in α-Al2O3 below 1000°C – measurements and molecular dynamics calculation

Results from impedance spectroscopy measurements at temperatures between 400 and 1000°C, for single crystal and highly pure and dense polycrystalline α-Al₂O₃ samples with well-defined grain size, are compared with that from molecular dynamics calculation. Between 650 and 1000°C, the measured activation energy for conductivity is 1.5?eV for the single crystal, and increases from 1.6 to 2.4?eV as the grain size decreases from 15 to 0.5?µm. The molecular dynamics calculation leads to the conclusion that the self-diffusion activation energy is about 1.5?eV for O and 1.0?eV for Al in single crystal α-Al₂O₃. The much higher mobility of O ions makes the O ions responsible for the conductivity of the single crystal oxide. It seems that the grain boundary leads to an increase in the activation energy. However, the quantitative influence of grain boundary still needs to be explained. Between 400 and 650°C, the measured activation energy is about 1.0?eV and independent of the grain size.     

Effect of applied stress on precipitation of Guinier–Preston zones in a Cu–0.9 wt.% Be single crystal

A stress-oriented formation of plate-shaped Guinier–Preston (GP) zones in single crystals of a Cu–0.9?wt.%?Be alloy aged at 200°C has been found. A compressive stress applied in the [001] direction assists the formation of the GP zones perpendicular to the [001] axis, while a tensile stress results in the preferential formation of the GP zones parallel to the stress axis. The applied stress strongly affects the nucleation of the GP zones. Free ageing at 275°C after compressive-stress ageing at 200°C produces plate-shaped γ′′ precipitates perpendicular to the stress axis, indicating a continuous change in the structure of the GP zones into that of the γ′′ phase. From length-change measurements during ageing, the misfit strains of the GP zone or γ′′ precipitate in directions parallel and perpendicular to the plate plane are estimated, respectively, as ?0.01 and ?0.10 for the GP zone and ?0.01 and ?0.11 for the γ′′ precipitate.     

An explanation for the low-temperature H evolution peak in hydrogenated amorphous silicon films deposited 'on the edge of crystallinity'

The puzzling existence of a sharp low-temperature (T = 400°C) H evolution peak in compact hydrogenated amorphous silicon (a-Si : H) films deposited 'on the edge of crystallinity' is examined. From infrared absorption and X-ray diffraction (XRD) measurements, we show that none of the standard methods used to explain the existence of this peak in a-Si : H materials is applicable to the present films. From the Si-H wag-mode peak frequency, we postulate the existence of very small Si crystallites contained within the amorphous matrix. While the crystallite volume fraction is too small to be detected by XRD in the as-grown films, crystallization is observed for this material at anneal temperatures as low as 500°C. It is proposed that these crystallites catalyse the crystallization of the remainder of the amorphous matrix upon moderate annealing, enabling H surface desorption and H₂ out-diffusion to the sample surface along newly formed grain boundaries at low anneal temperatures.     

Chemistry and morphology of β′ precipitates in an aged Mg-Nd-Y-Zr alloy

While the Mg–Y–Nd system is used for industrial applications, the details of the precipitation sequence and exact role of each alloying element during ageing have not been fully quantified. Focusing on WE43, a Mg–Y–Nd alloy containing Zr, the chemistry of β′ precipitates and matrix during isothermal ageing at 250 °C is investigated using atom probe tomography. Precipitate morphologies and compositions are compared with previous electron microscopy observations, and the roles of the alloying elements are discussed.     

New insights on tensile plasticity of ultrafine-grained metallic materials

ABSTRACT

The tensile properties of TiNi_43.5Fe_6.5 alloy samples having different grain sizes (0.16, 0.35, 1.7, 2.3, and 3.9?μm) and fabricated by severe plastic deformation and annealing were investigated. It was observed that both the strength and the elongation of the alloy increase with a decrease in the grain size until the average size reaches 1.7?μm. However, for average grain sizes smaller than 1.7?μm, the elongation decreases continuously with further grain refinement. On the other hand, the strain-hardening rate does not decrease with the decrease in plasticity but instead increases slightly. The poor ductility of the ultrafine-grained TiNi_43.5Fe_6.5 alloy is accompanied by a high degree of strain hardening. This newly observed ductility behaviour of the ultrafine-grained TiNi_43.5Fe_6.5 alloy is elucidated by characterising the intragranular and grain boundaries.     

On the role of Ag in enhanced age hardening kinetics of Mg–Gd–Ag–Zr alloys

The addition of Ag to the age hardenable Mg–Gd–Zr alloy system dramatically enhances early stage age hardening kinetics. Using atom probe tomography (APT), Ag-rich clusters were detected in a Ag-containing Mg–Gd–Zr alloy immediately after solution treatment and water quenching. During subsequent isothermal ageing at 200 °C, a high density of basal precipitates was observed during the early stages of ageing. These basal precipitates were enriched with Ag and Gd, as confirmed by APT. It is posited that Ag-rich clusters in the context of quenched-in vacancies can attract Gd atoms, increasing diffusion kinetics to facilitate the formation of the Ag + Gd-rich basal precipitates. The rapid formation of Ag + Gd-rich precipitates was responsible for accelerated ageing.     

Phase-transformation-induced hardening in Zn–22Al alloys

A phase-transformation-induced hardening effect is reported in Zn–22Al (Al: 22?wt.%) alloys. The Zn–22Al specimens were held at 300?°C for 10?h and then quenched in water. A hardening effect took place in subsequent artificial aging at 100–200?°C, which was accompanied by a phase decomposition of a soft α ₂ phase and a grain coarsening. The phase-transformation-induced hardening affects the hardness more than the grain-coarsening-induced softening, which leads to the age-hardening phenomenon.     

Interfacial precipitation of the M5B3-type boride in Ni-based superalloys

Microstructural characteristics of an experimental Ni-based superalloy with boron addition subjected to a long-term ageing treatment were systematically investigated by various kinds of transmission electron microscopy technique. Based on detailed electron diffraction analyses, we found that there are many nanosized M₅B₃ precipitates in our long-term ageing alloys, which keeps a good orientation relationship with the γ/γ′ matrix. Furthermore, the precipitation characteristics of M₅B₃ phase were clarified. It is found that the M₅B₃-type boride prefers to precipitate at the γ/γ′ interfaces and low-angle grain boundaries. These interfacial nanosized precipitates can play the role of pinning effect and are expected to be advantageous for postponing the γ′ rafting and low-angle grain boundary migration to some extent at high temperature.     

Discontinuous precipitation initiated at interphase boundaries in a Zn-rich Zn-6.3 at.% Ag alloy

Discontinuous precipitation in a two-phase Zn-rich Zn-6.3at.%Ag alloy has been studied. It has been shown that the eta/epsilon interphase boundaries have the ability to initiate discontinuous precipitation as do the eta/eta grain boundaries. The back-polishing method is used to show the interconnection between a discontinuous precipitate colony and the eta/epsilon interphase boundary. The reaction front velocity of discontinuous precipitation initiated at the eta/eta grain boundary is 12-90% higher than that of discontinuous precipitation initiated at the eta/epsilon interphase boundary under various ageing temperatures.     

Room temperature ferromagnetism and photoluminescence of nanocrystalline Zn1 − xCoxO thin films prepared by sol–gel MOD

Zn_1???xCo_xO (ZC) [x?=?0, 1, 3, 5, 7 and 9?mol%] thin films were prepared by sol–gel combined metallo-organic decomposition method. The films were deposited on the Si substrate with spin-coating technique and annealed at 600?°C for 3?h. X-ray diffraction pattern shows the formation hexagonal wurtzite phase and distortion (c/a) decreases with increasing Co concentration in ZnO. The average grain size is measured using Scherer relation. Atomic force microscopy is used to confirm the formation of nanograins resulted by the use of polyethylene glycol as surfactant. The photoluminescence was recorded by using He-Cd laser of excitation wavelength 325?nm in wavelength region of 350–650?nm which exhibits some influence of Co doping on the multiplication of defects such as O vacancies, Zn interstitials and grain boundary defects. All thin films show room temperature ferromagnetism except pure ZnO which is diamagnetic and 9?mol% of Co shows paramagnetism. This behaviour is interpreted as due to fluctuations in the magnetic ordering, depending on grain size and site location in grain boundaries or oxygen vacancies.     

Aluminium precipitates in the primary silicon of as-sprayformed hypereutectic aluminium-silicon alloys

Precipitates have been observed in the primary silicon of as-spray-formed hypereutectic aluminium-silicon alloys with and without various alloy additions. The precipitates have been investigated using transmission electron microscopy and high-resolution transmission electron microscopy. They are aluminium based and generally adopt a spheroidal morphology, with diameters in the range of approximately 5-10nm, unless located on a stacking fault or grain boundary. Spray forming is a rapid solidification process and precipitation occurs because of the low solid solubility of aluminium in silicon (maximum of 0.016 +/- 0.003at.% at 1190 C). The morphology of the precipitates suggests that they form from aluminium or aluminium-rich liquid. The orientation relationships of several precipitates in one of the primary silicon grains have been determined.     

Dynamic precipitation at elevated temperatures in a dual-phase AlCoCrFeNi high-entropy alloy: an in situ study

ABSTRACT

The effect of a possible phase transformation or precipitation of the face-centred cubic (FCC) phase on intermediate-temperature deformation of a dual-phase AlCoCrFeNi high-entropy alloy has been studied using in situ tensile testing at 550°C. Electron backscatter diffraction (EBSD) results showed localised precipitation of the FCC phase during the intermediate-temperature deformation. The overall fracture behaviour and crack propagation of the material was not altered much compared to the room-temperature behaviour, namely brittle trans-granular fracture. Deformation at higher temperatures (above 750°C) is suggested as a way to enhance the dynamic FCC phase precipitation, in order to improve the ductility or deformability of the alloy.