Fabrication of W–20 wt.%Cu alloys by powder injection molding

W–20 wt.% Cu balls were fabricated by powder injection molding using a binder system consisted of paraffin wax, high density polyethylene, ethylene vinyl acetate and stearic acid. By optimizing the injection molding parameters, defect-free green parts were obtained. A two-step debinding process was employed to extract the binders in the molded samples. All soluble ingredients of the binders in the green parts were extracted during solvent debinding, and the residual binders can be removed in thermal debinding. The debound W–Cu samples were sintered in H₂ atmosphere at temperatures ranging 1050–1150 °C for 2 h. It was shown that relative density of the sintered W–Cu samples increases from 87.37% of the theoretical to 95.58% as sintering temperature rises from 1050 °C to 1150 °C. Microstructures of the molded, the debound and the sintered W–Cu samples were observed by scanning electron microscope, and the sintered W–Cu balls have fine and homogeneous microstructures. Maximum compressive strength of W–Cu balls with 8.5 mm diameter reaches 58 kN.     

Fabrication of 93W–Ni–Fe alloy large-diameter rods by powder extrusion molding

A powder extrusion molding (PEM) process has been used for the manufacturing of tungsten heavy alloy rods with large length to diameter ratio. An improved wax-based multi-component binder was developed for PEM of 93W–Ni–Fe alloy. The miscibility of its components and the characteristics of the binder were evaluated and good thermal–physical properties were obtained. Also, the feedstock rheological properties, extrusion molding and debinding process were studied. The feedstock exhibited a pseudo-plastic flow behavior. The large length to diameter ratio rods, with diameters up to 36 mm were extruded at 65 °C by optimizing the extrusion process. A two-step debinding process was employed to remove the binder in the extruded rods. Solvent debinding was carried out in n-heptane at 45 °C to extract the soluble components. A process of repeated short time immersion and drying of the extruded rods (called short-period solvent debinding) was developed and using this novel technique the binder removed was raised from 45% to 60%. SEM analyses indicated that a large volume of pores was formed in debound rods, but had not created interpenetrating pore channels yet. The rest of the binder could be thermally extracted at a high heating rate without defects.     

Kinetics of austenitization under uniaxial compressive stress in Fe–2.96 at.% Ni alloy

Differential dilatometry has been employed to study the kinetics of the massive ferrite (α) → austenite (γ) transformation upon isochronal heating (i.e. austenitization) of the substitutional Fe–2.96 at.% Ni alloy subjected to a range of applied constant uniaxial compressive stresses. A phase-transformation model, involving site saturation, interface-controlled (continuous) growth and incorporating an impingement correction for an intermediate of the cases of ideally periodically and of ideally randomly dispersed growing particles, has been employed to extract the interface-migration velocity of the α/γ interface and the transformation-induced deformation energy taken up by the specimen. The value obtained for the energy corresponding with the elastic and plastic deformation associated with the accommodation of the α/γ volume misfit depends on the austenite fraction and increases distinctly with an increase in the applied uniaxial compressive stress, which is compensated by, in particular, an increase in the chemical driving force corresponding to an increase in the onset temperature. The opposite effects of an applied uniaxial compressive stress on the α → γ transformation and on the γ → α transformation can be discussed as the outcome of constrained plastic deformation due to transformation-induced strain.     

Comparison of Cu–Al–Ni–Mn–Zr shape memory alloy prepared by selective laser melting and conventional powder metallurgy

This work aimed to investigate and critically analyze the differences in microstructural features and thermal stability of Cu−11.3Al−3.2Ni−3.0Mn−0.5Zr shape memory alloy processed by selective laser melting (SLM) and conventional powder metallurgy. PM specimens were produced by sintering 106−180 µm pre-alloyed powders under an argon atmosphere at 1060 °C without secondary operations. SLM specimens were consolidated through melting 32−106 µm pre-alloyed powders on a Cu−10Sn substrate. Mechanical properties were measured through Vickers hardness testing. Differential scanning calorimetry was conducted to assess the martensitic transformation temperatures. X-ray diffraction patterns were collected to identify the metallurgical phases. Optical and scanning electron microscopy was used to analyze the microstructural features. β′₁ martensite was found, irrespective of the processing route, although coarser martensitic variants were present in PM-specimens. In conventional powder metallurgy samples, intergranular eutectoid constituents and stabilized austenite also formed at room temperature. PM-specimens showed similar average hardness values to the SLM-specimens, albeit with high standard deviation linked to the porosity. The specimens processed by SLM showed reversible martensitic transformation (T₀=171 °C). PM-processed specimens did not show shape memory effects.     

Effect of grain boundary orientation on radiation-induced segregation in a Fe–15.2 at.% Cr alloy

Ferritic chromium steels are important structural materials for future nuclear fission and fusion reactors due to their advantages over traditional austenitic steels, such as higher thermal fatigue resistance, lower thermal expansion coefficients and reduced swelling. However radiation-induced segregation or depletion (RIS/RID) of solute atoms at grain boundaries in these materials is a concern because these phenomena could adversely affect their mechanical properties. In an effort to develop a full mechanistic understanding of RIS/RID, a systematic approach combining orientation imaging, site-specific specimen preparation and three-dimensional atomic-scale analysis has been developed to characterize the behaviour of Cr and C at grain boundaries during irradiation. This methodology has been applied to a Fe–15.2 at.% Cr alloy to investigate the effects of grain boundary misorientation, irradiation depth and impurities. Systematic differences in Cr segregation are reported as a function of grain boundary character and irradiation conditions. The similar properties demonstrated by grain boundaries of similar type means that it should be possible to apply relatively simple models to predict the long-term behaviour of these materials under irradiation conditions.     

Effects of plastic deformation on lamellar structure formation in Ti–39 at.% Al single crystals

The effects of plastic deformation on lamellar structure formation in solution-treated Ti–39 at.% Al single crystals were investigated, focusing on the role of dislocations of different slip systems. The dislocations were introduced by indentation on the surfaces of solution-treated single crystals with different crystallographic orientations. Traces of basal and prism slips were observed, depending on the position relative to the indentation. During annealing at α₂ + γ dual-phase temperatures, lamellar structures were formed faster where basal slip had occurred than where prism slip had occurred. After long annealing, the length scale of lamellar structures formed depends on the slip system operated during prior deformation: in the region where only one of either basal or prism slip had occurred the lamellar structure was coarser than in undeformed crystal, while in the region where both basal and prism slips occurred the lamellar structure was finer than those formed in undeformed crystal. The reasons for the differences in lamellar structures are discussed on the basis of the frequencies of stacking fault formation on (0 0 0 1) planes as precursors to γ-precipitates. The results suggest that the cross-slip of dislocations between basal and prism planes, which gives rise to the formation of multiple stacking faults on many parallel (0 0 0 1) planes, is responsible for the refinement of lamellar structures.     

Study of the martensitic transformation in the Co–9 at % Al alloy

Phase transformations in the Co–9 at % Al have been investigated after slow furnace cooling. It has been shown that the structure and phase composition of the alloy after slow cooling do not correspond to the equilibrium phase diagram of the alloy of this chemical composition. It has been established that the α → ε martensitic transformation does not require overcooling and occurs even during a slow cooling of the alloy. It has been found that the formation of 4H modulated martensite is a specific feature of the binary alloys of cobalt and is not connected with the rate of their cooling. The Curie temperatures for the B2, α, and ε phases have been determined.     

Experimental investigation on the phase equilibria of the Mn–Ni–Zn system at 400 °C

Partial isothermal section of the Mn–Ni–Zn system at 400 °C was experimentally established by means of XRD and SEM/EDS techniques. Three ternary compounds, i.e. T, τ₁ and τ₂, were found to exist at 400 °C for the first time. The compound T having an approximate formula of Mn₇Ni₇Zn₈₆ was indexed as fcc structure with a lattice parameter of a = 1.81476 (1) nm. τ₁, the structure of which is unknown, has an approximately stoichiometric composition of about 29 at.% Mn, 38 at.% Ni and balanced Zn. τ₂ has fcc structure and a composition range of about 46–40 at.% Mn and constant 30 at.% Zn. Extended single-phase regions of the phases Mn₅Zn₂₁, Ni₂Zn₁₁, NiZn₃, NiZn and β-Mn were observed. The maximum solubility of Ni in Mn₅Zn₂₁ and those of Mn in Ni₂Zn₁₁, NiZn₃ and NiZn were determined to be 10, 6, 26 and 25 at.% at 400 °C, respectively.     

Oxidation behavior of a Zr–Cu–Al–Ni amorphous alloy in air at 300–425 °C

The oxidation behavior of Zr–30Cu–10Al–5Ni bulk metallic glass and its crystalline counterpart was studied over the temperature range of 300–425 °C in dry air. In general, the oxidation kinetics of both amorphous and crystalline alloys followed a two- or three-stage parabolic rate law at T⩾350 °C, while at 300 °C the amorphous alloy oxidized following a linear behavior. The oxidation rate constants for the amorphous alloy are slightly higher than those for the crystalline alloy at 350–400 °C. The scale formed on the amorphous alloy consists of mainly tetragonal-ZrO₂ at 300 °C, while a mixture of monoclinic-ZrO₂ (m-ZrO₂) and tetragonal-ZrO₂ (t-ZrO₂) and some CuO were detected at higher temperatures. The scale formed on the crystalline alloy, on the other hand, consists of mainly Al₂O₃, some tetragonal-ZrO₂, and a slight amount of monoclinic-ZrO₂ at 300 °C. At higher temperatures, the crystalline alloy consists of mainly monoclinic-ZrO₂, some CuO and Cu₂O, and limited tetragonal-ZrO₂. It is suggested that the formation of Al₂O₃ (at 300 °C) and CuO/Cu₂O (at 350-400 °C) on the crystalline alloy is responsible for the reduced oxidation rates as compared with those of amorphous alloy.     

Microstructure and mechanical properties of WC Ni–Si based cemented carbides developed by powder metallurgy

In this paper the influence of the Ni binder metal and silicon as an additional alloying element on the microstructure and mechanical properties of WC-based cemented carbides processed by conventional powder metallurgy was studied. Microstructural examinations of specimens indicated the presence of a very low and even distributed porosity and the presence of islands of metal binder in the microstructure of the cemented carbides. Furthermore, despite the addition of silicon and carbon in the cemented carbides, it was not observed the presence of small fractions of undissolved SiC and free graphite nodules in their microstructure. Vickers hardness and Flexural strength tests indicated that the cemented carbide WC–Ni–Si with 10 wt.% of binder presented bulk hardness similar to the conventional WC–Co cemented carbides and superior flexure strength and fracture toughness.     

Reaction behavior and pore formation mechanism of TiAl–Nb porous alloys prepared by elemental powder metallurgy

Ti–48Al–6Nb (at.%) porous alloys are fabricated by elemental powder metallurgy to study the pore formation and propagation mechanism. Reactive diffusion, pore formation process, and pore characteristics of the porous TiAl–Nb alloys are investigated at different temperatures. It is found that the porous alloys exhibit a uniform, maze-like network skeleton, viz., a typical α₂-TiAl₃/γ-TiAl fully lamellar microstructure. The reactive diffusivities between Ti and Al powders are dominant during the Ti–Al–Nb powder sintering. Gas release during sintering also plays an important role in the pore propagation and the compact expanding process. In addition, a pore-formation model is proposed to interpret the growth mechanism of pores and skeletons.     

A Study of the Magnetoelastic Effect of Metal Textured Ni–5 at % W Tapes

In the temperature range of 50–360 K, the effect of the plane mechanical deformations on the magnetic susceptibility χ_ac(T) of metal biaxially textured Ni–5.0 at % W tapes has been investigated. To create the state of plane stress, the temperature cycling of thin tapes cemented to thick substrates of Si, Mo, Ti, and D16T aluminum alloy has been performed. It has been shown that the main features of the magnetic susceptibility behavior can be explained by magnetoorientation transitions and the appearance of internal stresses σ(T) exceeding the yield strength of the tape material.     

Structural and mechanical stability of the nano-crystalline Ni–Ti (50.9 at.% Ni) shape memory alloy during short-term heat treatments

In this study, the nano-crystalline Nitinol (50.9 at.% Ni) was prepared by 40% cold deformation. Subsequently it was subjected to 15-min-heat treatments at 300–550 °C. Changes of the structure and mechanical properties were studied by transmission electron microscopy, micro X-ray diffraction, differential scanning calorimetry, Vickers hardness measurements, tensile and bend-type fatigue testing. It was shown that the cold drawn material contains textured nano-crystalline B2 grains of 50 nm in thickness and a high concentration of lattice defects. Its tensile strength, hardness and fatigue life were 1521 MPa, 421 HV0.05 and 2435 bending cycles to fracture, respectively. After heat-treatment up to 450 °C/15 min the material underwent Ni₄Ti₃ precipitation and partial recovery processes. Heat-treatments at above 450 °C induced recrystallization, grain and precipitate growth. Hardness and fatigue lives showed maxima of 692 HV0.05 and 5883 cycles, respectively, after heat-treatments at 450 °C/15 min. In contrast, both tensile strength and B2 → B19′ transformation stress decreased with increasing heat-treatment temperature, but a decrease of the tensile strength after heat-treatments at 300–450 °C was slow (tensile strength after heat-treatment at 450 °C/15 min was 1486 MPa). The observed variations of mechanical characteristics were discussed in relation to structural changes observed.     

Phase equilibria of the Ni–Si–Zn system at 600 °C

The phase equilibria at 600 °C of the Ni–Si–Zn system were investigated by using 19 alloys and four reaction diffusion couples. The alloys were prepared by melting the pure elements in the alumina crucibles capsulated in evacuated quartz tubes. The samples were examined by means of optical microscopy, X-ray diffraction, scanning electron microscopy with energy dispersive X-ray spectroscopy, and electron probe microanalysis. The presented isothermal section at 600 °C is characterized by the existence of five ternary phases, which are labeled as T₁, T₂, τ₃, τ₄ and β′, respectively. Three previously reported ternary compounds, viz. Ni₃Si_0.33Zn_0.67 (T₂), Ni₂SiZn₃ (τ₃), and Ni₃Si₂Zn (τ₄), were confirmed to exist at 600 °C. β′-NiZn was assumed to be the Si-stabilized β-NiZn phase in the Ni–Zn binary system. T₁ is a newly found ternary compound. It should be noted that the phase relationships at 600 °C are significantly different from the previously reported ones at 800 and 297 °C. γ₁-NiZn₃, the existence of which is still controversial in the literature, was observed at 600 °C. The solubilities of Zn in Ni₃₁Si₁₂, Ni₃Si₂ and NiSi, and those of Si in γ₁-NiZn₃ and γ-Ni₂Zn₁₁ are negligible. The solubilities of Zn in α-NiSi₂ and δ-Ni₂Si were determined to be 8.5 and above 3.1 at.% Zn, respectively. α-NiSi₂ and δ-Ni₂Si extend into the ternary system at constant Ni content with Zn substituting for Si.     

Creep- and coarsening properties of Al–0.06 at.% Sc–0.06 at.% Ti at 300–450 °C

Upon aging at 300–450 °C, nanosize, coherent Al₃(Sc_1−xTi_x) precipitates are formed in pure aluminum micro-alloyed with 0.06 at.% Sc and 0.06 at.% Ti. The outstanding coarsening resistance of these precipitates at these elevated temperatures (61–77% of the melting temperature of aluminum) is explained by the significantly smaller diffusivity of Ti in Al when compared to that of Sc in Al. Furthermore, this coarse-grained alloy exhibits good compressive creep resistance for a castable, heat-treatable aluminum alloy: the creep threshold stress varies from 17 MPa at 300 °C to 7 MPa at 425 °C, as expected if the climb bypass by dislocations of the mismatching precipitates is hindered by their elastic stress fields.     

The isothermal section of the Ni–Sn–Zn phase diagram at 873 K

The phase equilibria of the Ni–Sn–Zn ternary system were experimentally investigated at 873 K in the framework of the COST Action MP0602. Six ternary phases have been observed and their composition ranges have been determined by EPMA analysis on the annealed alloys. All the binary compounds, excluding Ni₃Sn₄, show a large solubility of the third element. The isothermal section at 873 K, including 17 three phase fields, has been determined.     

Characterization and formation mechanism of nanocrystalline W–Al alloy prepared by mechanical alloying

Tungsten and aluminum elemental powders with composition W–20 wt.% Al were mechanical alloyed in high energy planetary ball mill. Structural and morphological changes of powder particles after different milling times were studied by X-ray diffractometer, scanning electron microscopy and microhardness measurements. Mechanical alloying of this system led to the formation of W–Al alloy as a result of formation of W/Al layered microstructure having faceted interface between layers. This alloy indicated high microhardness value of about 570 Hv.     

Preparation and microstructure characterization of W–0.1 wt.%TiC alloy via chemical method

W–0.1 wt.%TiC materials with and without the addition of PVP were fabricated by wet-chemical method and spark plasma sintering. The microstructures were characterized by FESEM and TEM. The results revealed that the addition of PVP remarkably improved the uniform dispersion of TiC particles during the synthesis process. W–TiC without PVP showed dispersoids with size of 100–1000 nm were distributed unevenly in the tungsten matrix; only a few particles with the size of about 80–300 nm were located in tungsten grain interior. Conversely, the microstructure of W–TiC with PVP showed that dispersoids were dispersed well and kept about 80 nm. Moreover, the majority of them were uniformly distributed in the grain interior. The EDS analyses revealed that the dispersoids were composed of Ti, C, O and W. TEM observations further verified that the dispersoids were TiC particles. W–TiC with PVP showed better mechanical properties when compared with the samples of W–TiC without PVP and pure tungsten.