On the crystallographic characteristics of ion beam synthesised β–FeSi2

Nanometre-scale β–FeSi₂ precipitates were introduced in a single crystal silicon substrate by low-dose ion-beam synthesis (IBS). The crystallographic relationship between these nanometre β precipitates and the silicon substrate has been studied by high resolution electron microscopy (HREM). The results show that the orientation relationship (OR) between the nanometre β precipitates and the silicon substrate is [100]_β//[110]_Si and (001)_β//(1 1)_Si, with abnormally large strain between the precipitates and the substrate. This OR is important for the formation of 90°-OD boundaries within β–FeSi₂ grains. Also, the relationship between various reported low-index ORs has been analysed and a new low-index OR is predicted.     

Effect of Y203 on microstructure and oxidation of γ-Ni＋γ′-Ni3Al coatings transformed from electrodeposited Ni-Al films at 1 000℃

The electrodeposited Y2O3-dispersed γ-Ni＋γ-Ni3Al coatings on Ni substrates were developed by the conversion of electrodeposited Ni-Al-Y2O3 films with dispersed AI microparticles in Ni matrix into Ni3Al by vacuum annealing at 800 ℃ for 3 h. For comparison, Y2O3-free γ-Ni＋γ＇-Ni3Al coatings with a similar AI content were also prepared by vacuum annealing the electrodeposited microparticle-dispersed composite coatings of Ni-AI under the same condition. SEM and TEM characterizations show that the electrodeposited Y2O3-dispersed γ＋γ＇ coatings exhibit finer grains, a more homogeneous distribution of γ＇, and a narrowed γ＇ phase spacing compared with the electrodeposited Y2O3-free γ-γ＇ coatings. The oxidation at 1 000 ~C shows that the addition of Y2O3 significantly improves the oxidation resistance of the electrodeposited γ＋γ＇coatings. The effect of Y2O3 particles on the microstructure and oxidation behavior of the electrodeposited γ＋y＇ coatings was discussed in detail.     

The influence of hot deformation on the microstructure of Ni-Al and Ni-Al-Fe alloys with small Ti2B addition

Results of microstructure investigation of Ni-Al and Ni-Al-Fe alloys with addition of 0.5at.% Ti₂B after hot deformation are presented. Ti partially dissolves in the matrix, promoting formation of a discontinuous phase and precipitates of γ′ phase of Ll₂ structure during hot deformation of Ni-Al and Ni-Al-4.3at.%Fe alloys. In all investigated alloys precipitates of different compositions, enriched in Ti, were noticed. A compression test proved that due to the grain boundaries strengthening, the fracture mechanism changes into a transcrystalline one, improving fracture toughness of the hot deformed alloy. Fracture occurs in the deformation induced Ll₀ martensite.     

Towards understanding anelasticity of the β1′ martensitic phase of Cu–Al–Ni

The present work continues the series of experimental investigations undertaken in order to elucidate the mechanisms controlling elastic and anelastic properties of the β₁′ martensitic phase of Cu-based shape memory alloys. The paper reports an attempt to distinguish between ‘dislocation’ and ‘interface’ mechanisms of the internal friction in the β₁′ martensitic phase of Cu–Al–Ni single crystals. Two types of experiments have been performed. First, the ultrasonic strain amplitude-independent and amplitude-dependent internal friction (ADIF) of a monovariant specimen for temperatures 90–300 K is carefully re-examined. Second, in situ measurements of the ADIF and of the influence of ultrasonic oscillations on the plastic deformation (acoustoplastic effect) were carried out during quasistatic deformation of a quenched polyvariant specimen. Experimental results support a dislocation rather than an interface mechanism of anelasticity, at least at ultrasonic frequencies and moderate strain amplitudes.     

Formation of Al–Y oxide during processing of γ-TiAl

While processing Y₂O₃ dispersed γ-TiAl, Y₂O₃ particles which dissolved during hot isostatic pressing (HIP’ing) were found to precipitate during the heat treatment in the form of a mixed Al–Y oxide. To understand the chemical reaction that occurs between Y₂O₃ and γ-TiAl during the heat treatment cycle, a powder mixture comprising of γ-TiAl and 10 wt.% Y₂O₃ was mechanically alloyed (MA’d) for 8 h and the milled powder was subjected to differential thermal analysis (DTA) at 1150 °C prior to analyzing it using X-ray diffraction technique. The present study clearly demonstrates that aluminum in the combined form either as γ-TiAl or Al₂O₃ reacts in a similar manner with Y₂O₃ when milled and heat treated at 1150 °C. In either case there is formation of Al₂Y₄O₉ (2Y₂O₃.Al₂O₃).     

Stability of rolling texture during heat treatment in a two-phase Ti3Al base intermetallic alloy

The stability of hot rolling texture developed in the ₂ phase of a two-phase Ti₃Al base intermetallic alloy, during subsequent heat treatment, has been systematically investigated. The basal hot rolling texture remains rather stable during recrystallization annealing at temperatures within the single phase ₂ range. Grain growth after recrystallization produces extra orientations other than the basal. For the material with a starting basal texture, heat treatment in the upper ₂, (₂+β) or β phase fields does not change the basic character of the texture, although the sharpness and especially the width of the basal component increase to some extent with the increase in the heat treatment temperature. Heat treatment of material with starting non-basal texture in the upper ₂, (₂+β) or β phase fields does not produce any basal component irrespective of the heat treatment temperature. When the starting material is reasonably strain free and possesses a weak basal texture, heat treatment in the upper ₂, (₂+β) or β phase fields helps in intensifying the basal component to a certain extent.     

Oxygen release behaviour of Ce(1−x)ZrxO2 powders and appearance of Ce(8−4y)Zr4yO(14−δ) solid solution in the ZrO2–CeO2–CeO1.5 system

To clarify the existence of metastable phases in the ZrO₂–CeO₂–CeO_1.5 system, evolved-oxygen gas analyses, (EGA), by heating a single phase of t′ and t″ (Ce_(1−x)Zr_xO₂) with various compositions, x, in a reducing gas and successive oxidation were carried out repeatedly. The oxygen release behaviour of the t′ and t″ phases was very complicated. The single κ phases, (Ce_(1−x)Zr_xO₂) with the composition, x=0.5 and 0.6, which were obtained by oxidizing the resulting pyrochlore as a precursor in O₂ gas at 873 K, exhibited a sharp oxygen release at the lowest temperature; the composition range of κ phase may be x=0.450.65. A new tetragonal phase t*, (Ce_(1−x)Zr_xO₂), which was attained by cyclic redox process together with annealing in O₂ gas at 1323 or 1423 K, exhibited a sharp oxygen release at the highest temperature; the composition range of t* phase may be as wide as x=0.200.65. A metastable solid solution expressed by a chemical formula of Ce_(8−4y)Zr_4yO_(14−δ) (y=01) possessing a CaF₂-related structure appeared on deoxidation of the t* phase. A ternary phase diagram containing the t* and Ce_(8−4y)Zr_4yO_(14−δ) solid solution was proposed.     

Coarsening of γ (Ni–Al solid solution) precipitates in a γ′ (Ni3Al) matrix; a striking contrast in behavior from normal γ/γ′ alloys

Coarsening of γ precipitates in a γ′ (Ni₃Al) matrix depends strongly on volume fraction, in dramatic contrast with coarsening of γ′ precipitates. Coalescence of γ precipitates is easy, unlike the resistance to coalescence of γ′ precipitates. We regard this as indirect proof that anti-phase relationships among γ′ precipitates inhibit coalescence.     

Evolution of hot rolling textures in a two-phase (α2+β) Ti3Al base alloy

Texture development during thermomechanical processing of two-phase (α₂+β) Ti–24Al–11Nb alloy was studied as a function of variables like initial microstructure, rolling temperature, cooling conditions, etc. The evolution of texture in different conditions has been critically analysed. It has been found that unrestricted rolling of primary α₂ at lower temperature leads to a good basal {0001}uvtw texture, while at higher temperatures, the α₂→β→α₂ phase transformation leads to weakening of the basal texture. Texture of secondary α₂ derived from rolled β is generally non-basal. However, the texture of secondary α₂ derived from recrystallized β has a basal character.     

Structural chemistry and phase relations in intermetallic systems Ti–{Pd,Pt}–Al

Phase relations in the ternary systems Ti–{Pd,Pt}–Al have been experimentally established for the partial isothermal sections at 950°C in the Pd/Pt-poor region (<25 at.% Pd/Pt). The investigation is based on X-ray powder diffraction, metallography, SEM and EMPA techniques on about 45 alloys, which were prepared by various methods employing arc melting, levitation melting under argon or by powder reaction sintering in closed crucibles. Three ternary compounds were observed at 950°C in the Ti–Pd–Al system: τ₃-(Ti,Pd)(Ti,Pd,Al)₂ with Laves-MgZn₂-type, τ₂-(Ti,Al)₆(Ti,Pd,Al)₂₃₊₁ with a filled Th₆Mn₂₃₊₁-type and τ₁-(Ti,Pd,Al)(Ti,Pd,Al)₃ with AuCu₃-type. Due to the wide extension of the Laves phase field, there is no compatibility among γTiAl and τ₂-(Ti,Al)₆(Ti,Pd,Al)₂₃₊₁. The Ti–Pt–Al system at 950°C contains three ternary compounds: τ₃-(Ti,Al)(Ti,Pt,Al)₂ with Laves-MgZn₂-type, τ₂-(Ti,Al)₆(Ti,Pt,Al)₂₃₊₁ with the filled Th₆Mn₂₃₊₁-type and τ₁-(Ti,Pt,Al) with Cu-type. Compatibility exists for Al-rich γTiAl and τ₂-(Ti,Al)₆(Ti,Pt,Al)₂₃₊₁. The typical feature for both alloy systems studied is the three-phase equilibrium: ₂Ti₃Al+γTiAl+τ₃-(Ti,Pd/Al)(Ti,Pd/Pt,Al)₂. The solid solubility of palladium and platinum in the binary titanium aluminides, as observed from EMPA and X-ray data, is rather small and at 950°C accounts to about 2.5 at.% Pd and 2.0 at.% Pt. Two new oxide compounds Ti₃PdAl₂O_x and Ti₃PtAl₂O_x with a filled Ti₂Ni-type are observed in both quaternary systems.     

Achieving Superior Superplasticity in a Mg-6Al-Zn Plate via Multi-pass Submerged Friction Stir Processing

A large-scale Mg-6Al-Zn plate was prepared by multi-pass submerged friction stir processing (M-SFSP) and its superplastic deformation behavior was investigated. The maximum elongation of 467%, 332% and 421% was attained for the samples oriented in the processing direction (PD), 45° tilted toward the PD, and transverse direction (TD), respectively, when deformed at 623 K and a strain rate of 1 × 10^-3 s^-1. This was attributed to the homogeneous and fine-grained structure with mostly high-angle grain boundaries facilitating the prevalent deformation mechanism of grain boundary sliding, along with the weakened texture and dynamic recrystallization during hot deformation.     

Transmission electron microscopy of the iron-zinc δ1 intermetallic phase

1. 1. Two kinds of polycrystalline specimens, which fall in the δ₁ single phase of the Bastin et al.'s binary phase diagram of the Fe-Zn system but fall in the δ_1K, and the δ_1P phases in Ghoniem et al's phase diagram have been prepared. The hardness of the δ_1K, phase is higher than that of the δ_1P, phase.

2. 2. The density of stacking faults and internal strain in the δ_1P phase are higher than that of the 8 Ip phase.

3. 3. Electron di,tkction shows that ordering takes place in δ_1K phase, while no ordering takes place in δ_1P phase, the lattice parameter of δ_1K phase being three times as large as that of δ_1P phase.

     

Eutectoid transformations accompanied by ordering

Eutectoid transformations accompanied by ordering, unlike ordinary ones, proceed through non-pearlitic modes of transformations. Eutectoid invariants are classified into two categories in binary systems. The eutectoid invariant of A3()→D0₁₉(₂) + L1₀(γ) in the Ti-Al binary system belongs to the first category, in which one product phase has an ordered structure of a parent phase. Its transformation product exhibits a γ/₂ lamellar structure consisting of nearly perfectly aligned alternate lamellae of γ and ₂, which is formed by precipitation of γ plates in either or ₂ matrix with the Blackburn orientation relationship. The eutectoid invariant of A1(γ)→D0₂₂(γ″) + L1₂(γ′) in the Ni₃V-Ni₃Al pseudo-binary system is an example of the second category, in which both product phases have different ordered structures of a parent phase. The transformation of a 75Ni-18V-7Al alloy results in a ‘checkerboard’ pattern consisting of a periodic array of columns of γ′ and two γ″ orientation variants, which are formed by phase separation simultaneous with ordering.     

Phase Evolution and Thermal Expansion Behavior of a γ′ Precipitated Ni-Based Superalloy by Synchrotron X-Ray Diffraction

The phase evolution and thermal expansion behavior in superalloy during heating play an essential role in controlling the size and distribution of precipitates, as well as optimizing thermomechanical properties. Synchrotron X-ray diffraction is able to go through the interior of sample and can be carried out with in situ environment, and thus, it can obtain more statistics information in real time comparing with traditional methods, such as electron and optical microscopies. In this study, in situ heating synchrotron X-ray diffraction was carried out to study the phase evolution in a typical γ′ phase precipitation strengthened Ni-based superalloy, Waspaloy, from 29 to 1050 °C. The γ′, γ, M₂₃C₆ and MC phases, including their lattice parameters, misfits, dissolution behavior and thermal expansion coefficients, were mainly investigated. The γ′ phase and M₂₃C₆ carbides appeared obvious dissolution during heating and re-precipitated when the temperature dropped to room temperature. Combining with the microscopy results, we can indicate that the dissolution of M₂₃C₆ leads to the growth of grain and γ′ phase cannot be completely dissolved for the short holding time above the solution temperature. Besides, the coefficients of thermal expansions of all the phases are calculated and fitted as polynomials.     

Microstructure and mechanical properties of a directionally solidified and aged intermetallic Ni–Al–Cr–Ti alloy with β-γ′-γ-α structure

Microstructure and mechanical properties were investigated in a directionally solidified (DS) Ni–21.7Al–7.5Cr–6.5Ti (at.%) alloy. The dendrites of the as-grown alloy were composed of β(B2)-matrix (NiAl), coarse γ′(L1₂)-particles (Ni₃Al), fine γ′-needles and spherical α(A2)-precipitates (Cr-based solid solution). The majority of fine γ′-precipitates was found to be twinned. The interdendritic region contained γ(A1)-matrix (Ni-based solid solution) separating ordered domains of γ′-phase and fine lath-shaped α-precipitates. Ageing in the temperature range 973–1373 K decreased the volume fraction of dendrites from about 50 vol.% measured in the as-grown material to about 38 vol.% in the material aged at 1373 K for 300 h. During ageing in the temperature range 973–1273 K the γ-phase transformed to the γ′-phase in the interdendritic region. This transformation was connected with precipitation of lath-shaped α-precipitates. Ageing at higher temperatures of 1373 and 1473 K resulted in stabilisation of the γ-phase and precipitation of spherical γ′-particles in the interdendritic region. Ageing at 973 K significantly increased the microhardness, hardness and decreased room-temperature tensile ductility. Neither ageing nor finer dendritic microstructure were found to be effective in increasing the ductility of the alloy. The measured tensile ductility up to 1.1% can be attributed to the effect of extrinsic toughening mechanisms operating in the β-phase such as blunting and bridging of cracks by the α- and γ′-precipitates.     

Synthesis and characterization of proton conducting Sr(Ce1−xZrx)0.95Yb0.05O3−δ by the citrate method

The citrate method was used to synthesize Sr(Ce_1−xZr_x)_0.95Yb_0.05O_3−δ (x = 0.1, 0.2, 0.3, 0.4) and to avoid the drawbacks of the conventional solid state reaction method. The products were characterized by thermal analysis (TG-DTA), X-ray diffraction (XRD), scanning electron microscopy (SEM) and electron probe X-ray microanalyzer (EPMA). The results indicate that the citrate method is an advantageous route in producing Sr(Ce_1−xZr_x)_0.95Yb_0.05O_3−δ materials. Sr(Ce_0.9Zr_0.1)_0.95Yb_0.05O_3−δ powders are composed of nanoscaled crystallites with the average grain size in the range of 60–70 nm. Single phase is confirmed over the whole x range. In addition, chemical stability against CO₂ and electrical conduction behavior of the sintered Sr(Ce_1−xZr_x)_0.95Yb_0.05O_3−δ ceramics were investigated. The chemical stability of the ceramics against CO₂ is certified to increase with the increase in zirconium content. Impedance spectroscopy was used to study the electrical conduction behavior of Sr(Ce_0.9Zr_0.1)_0.95Yb_0.05O_3−δ ceramic.     

Effect of hot and cold deformation on the β fiber rolling texture in continuous cast AA 5052 aluminum alloy

The texture evolution of continuous cast AA 5052 aluminum alloy during hot rolling was investigated by X-ray diffraction. The β fiber rolling texture formed under various hot and cold deformation conditions was compared. The results show that deformation at elevated temperatures results in a stronger β fiber rolling texture than that at room temperature.     

{411}<148> Texture in Thin-Gauge Grain-Oriented Silicon Steel

The significant occupancy of {411}<148> texture exists in the thin-gauge grain-oriented silicon steel (TG-CRGO is defined that thickness of the sheet is <0.25 mm and the reduction in cold rolling is more than 90%) which has been considered to have obviously effects on the abnormal growth of Goss-oriented grains during the secondary recrystallization process. The microstructures of the TG-CRGO were investigated by X-ray diffraction and electron back-scattered diffraction in this study. It was found that {411}<148> texture mainly exists in the center layer of hot-rolled as well as normalized plates. With the increase in cold rolling reduction, {411}<148> orientation gradually rotates to α-fiber texture (<110>//RD). Finally, few {411}<148> would retain at the boundaries of deformed α-fiber grains (<110>//RD) as the reduction in cold rolling reaches 90%. After annealing treatment, a small amount of γ-fiber textures (<111>//ND) preferably nucleates and recrystallizes between the DBs (deformation bands) at first; then, the {411}<148> recrystallization texture occurs and mainly nucleates at the grains boundaries of the deformed α-fiber grains, and also quite a few {411}<148> orientation grains nucleate in the inner of {112}<110> grains. But this phenomenon was not observed in the {100}<011> deformation grains. With respect to the occurrence of {411}<148> recrystallization texture, it is mainly induced by strong α-fiber as well as weak γ-fiber textures formed during cold rolling other than originating from {411}<148> regions in hot bands.     

Preparation and properties of a γ-Al2O3 washcoat deposited on a ceramic honeycomb

Washcoat deposited on ceramic honeycomb was prepared using pseudoboehmite, the CeO₂–ZrO₂–La₂O₃ solid solution, pore enlarger and other additives. The microstructures and surface performances of washcoat/honeycomb were investigated by SEM, BET surface area, XRD, ultrasonic vibration and hot shock simulation. The results show that the performance and loading of washcoat are affected obviously by the properties of slurry gel, such as the apparent viscosity, solid content, particle size and its distribution. When the apparent viscosity of slurry is lower, the gel with a narrow particle size distribution and finer particles can be obtained, with which the coating having an excellent performance can be prepared. Adding a small quantity of the CeO₂–ZrO₂–La₂O₃ solid solution can promote the thermal stability of washcoat, such as, after calcined at 1000 °C for 5 h the sample exhibits mainly the γ-Al₂O₃ phases and the θ-Al₂O₃ -Al₂O₃ and κ-Al₂O₃ phases have not been detected in the XRD spectra. It is found also that the washcoat prepared has excellent properties of the vibration-resistant, heat-resistant and its BET surface area reaches 50 m²/g.     

Characterization of the microstructure evolution in a nickel base superalloy during continuous cooling conditions

The solidification characteristics of the γ phase from the liquid and the subsequent decomposition of the γ phase control the evolution of the microstructure in nickel–base superalloy welds. The precipitation of the γ′ phase from the γ phase during continuous cooling conditions (0.17–75 K s⁻¹) from the solutionizing temperature was characterized in a directionally solidified CM247DS alloy with thermomechanical simulator, and by transmission electron microscopy, atom probe field ion microscopy and atom probe tomography. The number density increased; size decreased and morphology of the γ′ precipitates changed with an increase in cooling rate. Under rapid water-quenched conditions, complex partitioning of the alloying elements between γ and γ′ phases was observed. Atom probe tomography on samples subjected to slower cooling rates showed different partitioning behavior compared to that of water-quenched samples and the presence of secondary γ′ precipitates in the samples subjected to a cooling rate of 1 K s⁻¹.