Metastable alloy bulk bodies in the Fe–W system prepared by mechanical alloying and shock compression

Bulk bodies of metastable alloys including supersaturated solid solutions and amorphous phases in the iron (Fe)–tungsten (W) system were prepared by mechanical alloying (MA) and shock compression. The X-ray diffraction patterns of the W solid solutions were obtained for the MA-treated powders in the Fe_xW_100−x system with Fe content of x≤30 mol%, and that of Fe solid solution was obtained with an Fe content of x=90 mol%. For the mixed powders with Fe content of 40≤x≤70 mol%, the peaks of Fe completely disappeared, and the amorphous halo-like patterns were observed around the (110) peak of W solid solution. For the mixed powder with an Fe content of 80 mol%, an X-ray diffraction pattern of a two-phase mixture of Fe and W solid solutions was obtained. For the MA-treated powders, the lattice parameters of W solid solutions were smaller than that of pure W, and those of Fe solid solutions were larger than that of pure Fe. No large crack could be observed in shock-consolidated bulk bodies, and the cross sections of the bulk bodies showed a metallic gloss. The X-ray diffraction patterns of shock-consolidated bulk bodies formed in a specific low pressure range did not change significantly from those of the MA-treated powders, which indicated that the metastable phases were successfully consolidated by shock compression without decomposition or recrystallization. Above a driving shock pressure of 40.1 GPa in capsule for the 30:70 mol% Fe–W system and that of 30.5 GPa for the 50:50 mol% Fe–W system, the X-ray diffraction patterns of the recovered bulk bodies showed the appearance of the peaks of Fe₇W₆ intermetallic compound and the peaks of Fe. The recovered specimens of the metastable solid solution phases in the 80:20 mol% Fe–W system did not recrystallize or decompose up to a driving shock pressure of 39.5 GPa. It was confirmed by the Electron Probe Micro Analysis (EPMA) that Fe and W dispersed well at the submicron level in the shock-consolidated bulk bodies. The Vickers hardnesses of the bulk bodies were much higher than those of pure Fe and pure W polycrystals.     

Quasicrystalline phase formation in the mechanically alloyed Al–Cu–Fe system

Al–Cu–Fe samples were prepared by ball milling powders of elemental Al, Cu, Fe (first route) and of elemental Al mixed with previously mechanically alloyed Cu–Fe solid solution (second route). Phase and structure transformations by annealing the as-milled powders were investigated by differential scanning calorimetry, X-ray diffraction and Mössbauer spectroscopy. The influence of the thermodynamic driving forces, namely the heat of mixing, positive for the Cu–Fe system and negative for the Al–Fe and Al–Cu systems, was discussed and correlated to the sequence of phase transformations during heating.     

New phases in Fe−Nd alloys obtained by quenching from the liquid state

Conclusions In alloys of the Fe–Nd system obtained by quenching from the liquid state, we observe the following phases: for (28–58)% Fe–P₁ (T_C240°C); for <28% Fe–P₂ [T_C=(220±5)°C]. In the alloy based on Nd containing 5% Co and 23% Fe, we observe the P₃ phase with T_C=160°C (tentatively amorphous).The presence of the P₁ phase in Nd-(37–58)% Fe alloys is responsible for the increase in the coercive force_IH_C up to 0.4 MA/m. During annealing, the amount of P₁ phase is reduced, a stable Nd₂Fe₁₇ phase appears, which is accompanied by a sharp decrease in the coercive force. In the alloy based on Nd containing 5% Co and 23% Fe, after annealing the P₄ phase is formed (T_C=340°C, H_a4.8 MA/m), which causes the appearance of the coercive force_IH_C=1.52 MA/m.Moscow Institute of Steel and Alloys. Translated from Metallovedenie i Termicheskaya Obrabotka Metallov, No. 9, pp. 13–16, September, 1992.     

Carbon solubility in Cu-based composite prepared by mechanical alloying

The powder mixture of Cu and graphite was mechanically alloyed （MA） in an oscillating type ball mill. The milling time was varied in order to investigate its influence on the microstructural evolution of mechanically alloyed powders. The phase constituent, alloying characteristics, grain size and lattice distortion of these powders were determined by X-ray diffraction, X-ray photoelectron spectroscopy, scanning electron microscopy and transmission electron microscopy. The results show that the C is confirmed to dissolve in the Cu lattice, forming solid solution of carbon in copper the lattice parameter of copper increases with carbon concentration increasing, up to a saturation value of about 4%C（mass fraction）. Higher ball-mill energy is beneficial for twins and nanograin formation.     

Microstructure and mechanical properties of bulk nanocrystalline Al–Fe alloy processed by mechanical alloying and spark plasma sintering

Nanocrystalline Al–5 at.% Fe alloy powders produced by mechanical alloying were consolidated by spark plasma sintering. The sintered sample showed high strength >1000 MPa with a large plastic strain of 15% at room temperature and 500 MPa at 350 °C. Microstructure characterizations by transmission electron microscopy and atom probe tomography revealed that the sintered samples are composed of α-Al and Al₆Fe nanocrystalline regions with 90 nm in diameter and a minor fraction of Al₁₃Fe₄ phase and coarsened 0.5–1 μm α-Al grains. This bimodally grained feature is attributed to the relatively large plastic strain for the strength level of 1000 MPa at room temperature.     

Study of the feasibility of producing Al–Ni intermetallic compounds by mechanical alloying

Mechanical alloying (MA) was employed to synthesize Al–Zn–Mg–Cu alloys of high weight percentage of the nickel component from the elemental powders of constituents via high-energy ball milling. The mixed powders underwent 15 h of milling time at 350 rpm speed and 10: 1 balls/powder weight ratio. The samples were cold-compacted and sintered thereafter. The sintered compacts underwent homogenization treatments at various temperatures conditions and were aged at 120°C for 24 h (T6). The milled powders and heat-treated Al alloy products were characterized via X-ray diffraction (XRD), scanning electron microscopy (SEM), and energy dispersive spectroscopy (EDS). The crystallite sizes and microstrains of the alloyed powder were estimated via measuring the broadening of XRD peaks using the Williamson–Hall equation. The results have revealed that optimum MA time of 15 h has led to the formation of Al-based solid solutions of Zn, Mg, Cu, and Ni. The outcomes showed that the Vickers hardness of the sintered Al–Zn–Mg–Cu compacts of Ni alloys was enhanced following aging at T6 tempering treatments. Higher compression strength of Al-alloys with the addition of 15% nickel was obtained next to the aging treatment.     

Experimental investigation of phase equilibria in the Ru–Fe–Al system at 1473 K

The low-Al part of the ternary Ru–Fe–Al phase diagram at 1473 K is established in this work. Due to the very promising properties of B2 ruthenium aluminide, the investigation of the B2 region of this system is of special interest. The experimental work includes diffusion methods, as well as quenching of annealed single-phase and two-phase alloys. The results of the different methods are in good agreement. Optical and scanning electron microscopy, energy dispersive X-ray spectroscopy and X-ray diffraction are used to investigate the samples. It is shown in this work that a three-component B2 phase exists over a wide composition range.     

New modelling of the B2 phase and its associated martensitic transformation in the Ti–Ni system

A symmetric two-sublattice model (Ni, Ti, Va)_0.5(Ni, Ti, Va)_0.5 is applied to describe the intermediate B2 compound in order to cope with the order–disorder transition in the Ti–Ni system. Using this model, the ordered B2 and the disordered Ti-rich b.c.c. are described by a single Gibbs free energy function. The B2 phase is the parent phase of the martensitic transformation in the TiNi shape memory alloys (SMAs), and its thermodynamic properties are then reassessed with emphasis on its composition range that is critical for SMAs. The low temperature B19′ phase is also evaluated on the basis of the selected experimental data from the martensitic transformation. Properties related to the transformation are studied in comparison with experimental data. The magnetic contribution is examined for the martensitic transformation. All calculations are in satisfactory agreement with experimental phenomena.     

Thermal conductivity mapping of the Ni–Al system and the beta-NiAl phase in the Ni–Al–Cr system

Micron-scale-resolution thermal conductivity mapping on graded compositions created in diffusion-multiple samples can be used to rapidly establish composition-phase-property relationships and to reveal the effects of solid-solutioning, order-disorder transition, compositional point defect, and site preference on thermal conductivity.

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The crystal structure of the equilibrium Φ phase in Mg–Zn–Al casting alloys

The crystal structure of the equilibrium intermetallic Φ phase formed in a Mg–Zn–Al casting alloy has been characterised using transmission electron microscopy. Electron diffraction patterns recorded from particles of the Φ phase in the casting alloy can be well indexed according to a primitive orthorhombic unit cell, with lattice parameters a=0.90 nm, b=1.70 nm, and c=1.97 nm. Examination of the whole pattern symmetry of principal zone axis diffraction patterns indicates a space group of Pbcm. A model for the decoration of the unit cell of the Φ phase is proposed, in which the Mg₅(Zn,Al)₁₂ Friauf polyhedron is the key structural unit. The Zn and Al atoms are all in icosahedral coordination, but their icosahedral shells are distorted due to the presence of Mg atoms. A total of 84 Mg atoms and 68 Zn/Al atoms can be accommodated in the orthorhombic unit cell, resulting in a formula of Mg₂₁(Zn,Al)₁₇ that is consistent with the composition obtained experimentally. Computer simulations of electron diffraction patterns provide very good agreement with experimental observations.     

Structural and phase transformations during copper and iron mechanical alloying in liquid medium studied by Mössbauer spectroscopy

Mössbauer spectroscopy and X-ray diffraction have been used to study the kinetics of structural and phase transformations in Cu + 2 at% ⁵⁷Fe during mechanical activation in liquid media (heptane, distilled water) and subsequent heat treatment (600 and 700 °С). The initial stages of mechanical alloying are associated with the transition of components to the nanostructural state. Iron atom groups form near the grain boundaries, and isolated iron atoms penetrate from the boundaries into the grains. Oxidation of groups of iron atoms that form highly dispersed phases of ternary oxide and magnetite occur in the initial stages of mechanical alloying of Cu + 2 at% ⁵⁷Fe in water. The formation of the solid solution in the form of isolated iron atoms in the lattice of copper proceeds, regardless of the milling media used. Samples prepared in heptane contain carbon and oxygen, and upon heat treatment, carbide and oxide phases are formed.     

The FeAl–30%TiC nanocomposite produced by mechanical alloying and hot-pressing consolidation

Intermetallic matrix composites reinforced with particles such as TiC have attracted a great deal of attention over the past few years. In the present study, the mechanical alloying process followed by hot-pressing consolidation was used to produce FeAl–30%TiC nanocomposite. Since the reduction of grain size to the nanometer scale improves mechanical properties of materials, this composite may be attractive for structural applications. An elemental powder mixture of Al35Fe35Ti15C15 (in at.%) was milled in a high-energy ball mill. The phase transformations in the powder during milling were studied with the use of X-ray diffraction (XRD). Transmission electron microscopy and differential scanning calorimetry were used for examining the microstructure and the thermal stability of the milling product. The results obtained show that high-energy ball milling as performed in this work leads to the formation of a bcc phase identified as the Fe(Al) solid solution and a fcc phase identified as TiC, and that both phases are nanocrystalline. Subsequently, the milled powder was sintered at 750 °C under pressure of 4 GPa. The XRD investigations of the consolidated pellet revealed that after sintering, the material remained nanocrystalline and that there were no phase changes, except for the ordering of Fe(Al), i.e. formation of FeAl intermetallic compound, during the sintering process. The average hardness of the obtained nanocomposite is 1287 HV_0.2 (12.6 GPa) and its density is 98% of the theoretical value.     

Phase equilibria of the long-period stacking ordered phase in the Mg–Ni–Y system

Phase equilibria in the Mg-rich Mg–Ni–Y system at 300, 400 and 500 °C have been experimentally investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM), differential scanning calorimetry (DSC), electron probe micro-analyzer (EPMA) and transmission electron microscopy (TEM). The results show that a long-period stacking ordered (LPSO) phase with 14H structure is thermodynamically stable in the Mg–Ni–Y system in a wide temperature range, but it dissolves varying from 492 to 559 °C depending on the alloy composition. The equilibrium 14H phase has a very limited solid solution range, and can be nearly regarded as a ternary stoichiometric compound with a formulae as Mg₉₁Ni₄Y₅. The isothermal sections of the Mg-rich Mg–Ni–Y system at 300, 400 and 500 °C have been finally established, and a eutectic reaction, Liquid ↔ α-Mg + 14H + Mg₂Ni, has been determined occurring at 492 °C with a liquid composition about Mg_84.8Ni_12.0Y_3.2.     

Phase stability in the Fe–Ni system: Investigation by first-principles calculations and atomistic simulations

First-principles calculations of the energy of various crystal structures of Fe, Ni and ordered Fe–Ni compounds with different stoichiometries have been performed by the linearized augmented plane wave (LAPW) method in the generalized gradient approximation. The most stable compounds are L1₂–Ni₃Fe, L1₀–FeNi, C11_f–Ni₂Fe and C11_f–Fe₂Ni. The L1₂–Ni₃Fe compound has the largest negative formation energy, which is consistent with the experimental Fe–Ni phase diagram. The L1₀–FeNi compound has also been observed experimentally in meteorite samples as a metastable phase. It is suggested here that the C11_f compounds could also form in Fe–Ni alloys at low temperatures. A new semi-empirical interatomic potential has been developed for the Fe–Ni system by fitting to experimental data and the results of the LAPW calculations. Recognizing the significance of the covalent component of bonding in this system, the potential is based on the embedded-atom method (EAM) but additionally includes a bond-angle dependence. In comparison with the existing modified EAM method, our potential form is simpler, extends interactions to several (3–5) coordination shells and replaces the screening procedure by a smooth cutoff of the potential functions. The potential reproduces a variety of properties of Fe and Ni with a reasonable accuracy. It also reproduces all stability trends across the Fe–Ni system established by the LAPW calculations. The potential can be useful in atomistic simulations of the phases of the Fe–Ni system.     

Phase equilibria and structural investigations in the system Al–Fe–Si

The Al–Fe–Si system was studied for an isothermal section at 800 °C in the Al-rich part and at 900 °C in the Fe-rich part, and for half a dozen vertical sections at 27, 35, 40, 50 and 60 at.% Fe and 5 at.% Al. Optical microscopy and powder X-ray diffraction (XRD) was used for initial sample characterization, and Electron Probe Microanalysis (EPMA) and Scanning Electron Microscopy (SEM) of the annealed samples was used to determine the exact phase compositions. Thermal reactions were studied by Differential Thermal Analysis (DTA). Our experimental results are generally in good agreement with the most recent phase diagram versions of the system Al–Fe–Si. A new ternary high-temperature phase τ₁₂ (cF96, NiTi₂-type) with the composition Al₄₈Fe₃₆Si₁₆ was discovered and was structurally characterized by means of single-crystal and powder XRD. The variation of the lattice parameters of the triclinic phase τ₁ with the composition Al_2+xFe₃Si_3?x (?0.3 < x < 1.3) was studied in detail. For the binary phase FeSi₂ only small solubility of Al was found in the low-temperature modification LT-FeSi₂ (ζ_β) but significant solubility in the high-temperature modification HT-FeSi₂ (ζ_α) (8.5 at.% Al). It was found that the high-temperature modification of FeSi₂ is stabilized down to much lower temperature in the ternary, confirming earlier literature suggestions on this issue. DTA results in four selected vertical sections were compared with calculated sections based on a recent CALPHAD assessment. The deviations of liquidus values are significant suggesting the need for improvement of the thermodynamic models.     

Hydrogen storage properties of Mg-doped Ti_(1.2)Fe alloys synthesized by mechanical alloying

1　INTRODUCTIONHydrogenstoragematerials ,usedinhydrogensourcesystemsforfuelcellshavebeeninvestigatedduetotheirhighvolumetricdensity ,safety ,easyminiaturizationandconvenientoperation .Consider ingallkindsofhydrogenalloysasawhole ,AB typeTiFealloysareknowntobemuchmoresuitableforusingin portableormobilePEMFCbecauseofitshighreversiblehydrogenstoragecapacity ,whichismuchhigherthanthatofAB5 typealloys.Ontheotherhand ,theactivationpropertiesoftheTiFeal loysare poor .Forexample ,typically ,…     

Synthesis of TiB2 nanocrystalline powder by mechanical alloying

1 Introduction TiB2 has been widely used in some industrial fields owing to its high melting temperature, hardness, elastic modulus, electro-conductibility and thermal diffusivity, and excellent refractory properties and chemical inertness. Usually, TiB2…     

Powder metallurgy preparation of Al–Cu–Fe quasicrystals using mechanical alloying and Spark Plasma Sintering

This work is devoted to the preparation of ultrafine material based on Al–Cu–Fe quasicrystalline phase by powder metallurgy using mechanical alloying and Spark Plasma Sintering. The dependence of microstructure and phase composition of powders on the conditions of mechanical alloying was described. It was found that the Al₆₀Cu₃₀Fe₁₀ quasicrystalline phase forms directly already after 2 h of milling under optimized conditions. The stability of this quasicrystalline phase was studied at various temperatures of Spark Plasma Sintering compaction process.