Secondary ageing in Al-Cu-Mg

Secondary ageing, that is microstructural evolution occurring at room temperature after short heating at temperatures above the metastable phase boundary of Guinier-Preston zones, has been studied for an Al-Cu-Mg alloy with a high Cu-to-Mg ratio. Combined data from positron annihilation spectroscopy, Vickers microhardness measurements and differential scanning calorimetry show that, on secondary ageing after 5 or 7min at 190°C, firstly, hardening takes place at a rate nine to 16 times slower than natural age hardening; secondly, vacancies slowly released by Cu-rich aggregates formed during the heat treatment at 190°C promote further formation of solute aggregates, with a time-dependent chemical composition; thirdly, the thermal stability of the structures formed during secondary ageing increases with increasing dwell time at room temperature; and, fourthly, solute aggregates formed at 190°C undergo a structural reorganization and possibly a change in the composition, leading to species with a different thermal stability. The slow release of vacancies from Cu-rich aggregates is proposed as one of the limiting factors of the hardening rate.     

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.     

High-angle annular dark field scanning transmission electron microscopy of the antiphase boundary in a rapidly solidified B2 type TiPd compound

High-angle annular dark field scanning transmission electron microscopy (HAADF-STEM) with Z-contrast is applied to characterize the antiphase boundary (APB) of the B2 structure in a rapidly solidified TiPd melt-spun compound. The atomic shift associated with the R ?=?(1/2) a ₀ ?111? type displacement vector is directly observed at the boundary. A microstructure modification of the melt-spun compound with the cooling rate during solidification is also described.     

ω-phase formation in a rapidly solidified Cr-40 at.% Al alloy

The diffuse ω structure has been identified by electron diffraction for the first time in a C11_b matrix of the melt-spun Cr-40 at.% Al alloy ribbon. The C11_b matrix consists of nanometre-scale ordered domains produced by a long-period chemical ordering in the precursor A2-B2 structure. Each C11 _b unit cell in the Cr-40 at.% Al alloy is based on three cubic B2 cells along the c axis and contains two antiphase boundaries. The structure of the diffuse ω is consistent with that observed by De Fontaine. The relative stability of the crystalline ω structure has been predicted with respect to bcc-type precursor phases as a function of the displacement parameter z from calculation of the cohesive energy of the ω phase using the full-potential linear muffin-tin orbital method. The results show that the three-dimensional crystalline ω structure is stable with respect to bcc-type precursor phases in the Cr-Al system and reveals the physical background as to why the ω structure in Cr-40 at% Al is diffuse in nature.     

Identification of a new tetragonal phase in the Nb-Ti-Al system

During the course of investigation of the phase equilibria in the Nb-Ti-Al system, a new phase, designated theta, was observed in three Nb-Ti-40at.%Al alloys following ageing at low temperatures (less than 1000 C). Using X-ray diffraction and transmission electron microscopy techniques, this phase was determined to have a bct structure, with lattice parameters a₀ = 5.106 A and c₀ = 28.168A, a space group of I 4₁/amd (number 141) and composition near 45at.%Nb25at.%Ti-30at.%Al. An orientation relationship between the new tetragonal phase and the gamma-TiAl phase of [101]_gamma//[120]_theta and (111)_gamma//(001)_theta was observed within the microstructure.     

Planar faults in MoSi2 single crystals deformed at high temperatures

Abstract

Dislocation structure and planar faults have been examined in MoSi₂ single crystals deformed at high temperatures. Pure stacking faults were found in a crystal deformed at 900°C. The formation of the stacking fault is closely related to the phase stability of the C11_b and C40 ordered structures. Profuse stacking faults with increasing deformation temperature assist the ductility improvement of the MoSi₂ above about 1200°C. The critical resolved shear stress for {110}(331) and {013}(331) slip is determined in the temperature range 1000 to 1500°C.     

Synthesis and characterizations of NiTiO3 nanoparticles prepared by the sol–gel process

Nanocrystalline nickel titanate (NiTiO₃) composite powders were prepared by the sol–gel process combined with a surfactant-assisted template method. The resulting powders were calcined at different temperatures ranging from 150°C to 750°C for 2 h in air. The results revealed that a pure hexagonal phase of NiTiO₃ could be obtained at the low temperature of 750°C. The phase evolution of NiTiO₃ was investigated by X-ray diffraction patterns, Fourier-transform infrared spectroscopy, and X-ray photoelectron spectroscopy. Particle size and morphology were studied by transmission electron microscopy.     

Microstructural characterization and high-temperature strength of hot-pressed silicon nitride ceramics with Lu2O3 additives

The microstructures of two hot-pressed Si₃N₄ ceramics, with 3.33 and 12.51 wt% Lu₂O₃ additive, have been characterized using transmission electron microscopy. The microstructures of both samples consisted of elongated β-Si₃N₄ grains and a secondary phase, contained in pockets surrounded by the grains, with a crystalline or amorphous form. In the 3.33 wt% Lu₂O₃-containing Si₃N₄ ceramic, all the multiple-grain junctions were completely crystalline while, in the 12.51 wt% Lu₂O₃-containing Si₃N₄ ceramic, approximately half the junctions were devitrified. A thin intergranular amorphous film present between the two-grain boundary was common; however, a film-free grain boundary was observed in the 12.51 wt% Lu₂O₃ sample. The film-free grain boundary was determined to be approximately 35%. Both ceramics fractured in four-point flexure between 1200 and 1600°C. Their high-temperature strength is closely associated with the nature of the grain-boundary phase formed during the sintering process.     

Positron lifetime study of an Al-1.7at.% Mg-1.1at.% Cu alloy

The behaviour of vacancies during isothermal ageing following quenching of an Al-1.7at.% Mg-1.1at.% Cu alloy has been studied by positron annihilation lifetime spectroscopy. The positron lifetime parameters vary in parallel with the Vickers hardness of the alloy, suggesting simultaneous migration of vacancies and changes in the size and concentration of vacancies containing clusters and dislocation loops. The results also explain the long hardness plateau observed previously in ageing experiments carried out between 100 and 240°C in terms of a continuous growth of Mg-Cu-vacancy clusters during ageing. The vacancy concentration of the clusters increases gradually until the setting in of the cluster Guinier-Preston-Bagaryatsky zone transformation.     

A new highly ordered Al-Ni-Ru decagonal quasicrystal with 1.6 nm periodicity

A new decagonal quasicrystal (the D phase) with a period of about 1.6 nm was found to form in conventionally solidified and heat-treated Al₇₅Ni₁₅Ru₁₀ alloys. The electron diffraction patterns of the Al-Ni-Ru D phase exhibit a large number of quite sharp diffraction spots located at precise decagonal symmetry positions, indicating a highly ordered decagonal quasicrystal with a long-range quasiperiodic correlation. The D phase is formed with a composition close to Al₇₄Ni₁₅Ru₁₁, as determined by energy-dispersive X-ray analysis. By means of high-resolution electron microscopy, the structural features of the Al-Ni-Ru D phase, which are obviously different from that of the Al-Pd D phase (a typical decagonal quasicrystal with 1.6 nm periodicity reported previously), have been revealed.     

Formation and hydrogen adsorption properties of Ti-Hf-Ni quasicrystals and crystal approximants

The formation of a high-order rational approximant (RA) phase in rapidly quenched Ti-Hf-Ni alloys and the hydrogen absorption properties of that phase are reported. Electron diffraction patterns show systematic shifts of the diffraction spots from their expected positions for the icosahedral phase (i-phase); the diffraction patterns are consistent with those expected for a 3/2 RA phase RA-(Ti-Hf-Ni). Based on differential scanning calorimetry studies, RA-(Ti-Hf-Ni) is metastable, transforming between 350 and 500°C to a quasicrystal with strong phason disorder. This crystallizes at 620°C to a Ti 2 Nitype phase. RA-(Ti-Hf-Ni) readily absorbs hydrogen, up to 1.2 hydrogen atoms per metal atom ([H][M] =1.2). Pressure-composition isotherm studies for gasphase loading show that the pressure plateau for RA-(Ti-Hf-Ni) is similar to that observed for the i-(Ti-Zr-Ni) phase, although it occurs at as lightly higher pressure and extends over a smaller range of hydrogen concentrations. Unlike i-(Ti-Zr-Ni), no irreversible hydride phase forms with hydrogen loading at 250°C, suggesting that RA-(Ti-Hf-Ni) may have superior cycling properties, of interest for hydrogen storage applications.     

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.     

On the internal structure of Guinier-Preston zones in Al-3 at.% Ag

High-angle annular dark-field scanning transmission electron microscopy has been employed to study partially decomposed Al-3 at.% Ag. After solutionizing at 550°C and quenching to room temperature, samples of an Al-3 at.% Ag single crystal were aged for short times at 105, 140 and 180°C. Independent of the ageing temperature for these early stages, Guinier-Preston zones with a diameter of about 3 nm are found. Most of these zones consist of a silver-depleted core surrounded by a silver-rich shell. The shell structure is not uniformly pronounced. Irregularly shaped Guinier-Preston zones are common, but the shell structure dominates. No indication of different structures of the Guinier-Preston zones in Al-3 at.% Ag was found after short ageing at the three different temperatures. The shell model for Guinier-Preston zones in aluminium-rich Al-Ag alloys, which was previously proposed on the basis of X-ray and neutron scattering experiments, is thus appropriate to describe the structure of the Guinier-Preston zones in the early stages of the decomposition.     

Light emission from ferroelectric barium titanate nanocrystals

Thin laminates (thickness δ = 20–45 nm) of barium titanate, BaTiO₃ (BT), have been synthesised by the sol–gel method followed by heating of the amorphous precursor powder in air. An orthorhombic BT polymorph forms along with a tetragonal phase (t-BT) after 2 h of heating the precursor at 600°C, as evidenced by a well-defined X-ray diffraction pattern. The average crystallite size D ～ 21 nm compares the δ-value obtained from the scanning electron micrograph. On heating at temperatures as high as 750°C, the structure remains mostly t-BT (D ? 44 nm), which emits violet–blue–green light at a wavelength of 380–580 nm with a maximum at around 422 nm. The emission extends to wavelengths shorter than ～300 nm owing to a quantum-size effect in smaller crystals processed at lower temperatures. Electron paramagnetic resonance (EPR), which occurs at a g-value of 1.995 (linewidth ΔH = 1.12 mT) in a sample heated at 400°C, shows an order of magnitude of lower intensity at g = 1.993 (ΔH = 3.69 mT) on annealing out the paramagnetic defects at 600°C in air. No EPR signal arises in t-BT free from such defects in larger crystals.     

Tuning the structure of MoO3 nanoplates via MoS2 oxidation

Orthorhombic phase MoO₃ (α-MoO₃) nanoplates were synthesized by oxidizing MoS₂ nanoplates in air at 300?°C, while α-MoO₃ microplates were achieved by directly evaporating MoO₃ powders at 800?°C. Much thinner α-MoO₃ nanoplates were characterized by scanning electron microscopy, X-ray diffraction, X-ray photoelectron spectroscopy and micro Raman spectroscopy. This experiment may provide a pathway to the formation of α-MoO₃ nanoplates.     

Structure images of unaged martensite containing a high carbon content

Abstract

A highly tetragonal (large c/a ratio) martensite in a Fe-4 wt% Al-1·6 wt% Mn-2 wt% Calloy, which is not aged and considered to be as ‘fresh’ as possible, has been observed by high-resolution electron microscope. From the arrangement of atom rows in the [010] structure image and the corresponding electron diffraction pattern, it is concluded that carbon atoms are clustered on the (305) plane. The unit structure of these carbon-clustered regions is similar to that of the modulated structure observed in Fe-C alloys, although a periodic layer distribution of carbon atoms is not observed.     

Pressure-Induced transitions in amorphous TlxSe100−x alloys

Abstract

The electrical resistivity of bulk semiconducting amorphous Tl_xSe_100?x alloys with 0 ≤ x ≤ 25 has been investigated up to a pressure of 14 GPa and down to liquidnitrogen temperature by use of a Bridgman anvil device. All the glasses undergo a discontinuous pressure-induced semiconducting-to-metal transition. X-ray diffraction studies on the pressure-recovered samples show that the high-pressure phase is the crystalline phase. The pressure-induced crystalline products are identified to be a mixture of Se having a hexagonal structure with a = 4·37 Å and c = 4·95 Å and TlSe having a tetragonal structure with a = 8·0 Å and c = 7·0 Å     

Structural characteristics of a high-quality Al?Ni?Ru decagonal quasicrystal with 1.6nm periodicity,studied by atomic-scale electron microscopy observations

We report the structural characteristics of a high-quality stable decagonal quasicrystal (D phase) with 1.6nm periodicity, formed in Al₇₅Ni₁₅Ru₁₀ alloy annealed at 890°C for 24h. The tiling structure and the arrangement of transition-metal atoms (Ru and Ni) in this Al-Ni-Ru D phase have been clearly revealed by high-resolution electron microscopy (HREM) and by highangle annular detector dark-field (HAADF) scanning transmission electron microscopy (STM) respectively. On the basis of the HREM and HAADF STM observations, the relationship between the arrangement of local structural units and the formation of the long-range quasiperiodic tiling structure is discussed.     

Plastic deformation behaviour of decagonal Al70Ni15Co15 single quasicrystals

High-temperature deformation experiments have been performed on decagonal Al₇₀Ni₁₅Co₁₅ single quasicrystals at a constant strain rate of 10^-5s^-1 in the temperature range between 700 and 860°C. The samples were deformed in compression with the compression axis in different orientations, parallel to, inclined by 45° and perpendicular to the tenfold symmetry axis. Stress relaxation tests and temperature changes were carried out to determine thermodynamic activation parameters. The flow stress and the activation enthalpy were found to depend on the sample orientation whereas dependences of the activation volume and the stress exponent on the orientation were not observed. Additionally, deformation tests were performed on samples of the basic Co-rich modification of the decagonal phase at the temperature of 860°C in the same three orientations. The deformation behaviours of the two different modifications of the decagonal phase are discussed.     

The crystallographic structure of λ transition-alumina compared with the periodic antiphase boundary structure of a Ga2O3-rich Mg gallate

One of the high-temperature metastable phases found in the MgGa₂O₄–Ga₂O₃ system is the ε_Mg non-stoichiometric Mg gallate. It has a one-dimensional periodic antiphase boundary (PAPB) structure based on the spinel structure. The APBs are parallel to the {3?1?0} planes and the APB vectors are of the 1/4?1 1 0? type when referred to the spinel structure. This generally leads to the existence of 12 monoclinic twin variants in the studied samples. By comparing the X-ray or electronic diffraction patterns of both phases, it will be shown that the recently discovered?λ?transition-alumina has the same type of structure.