Grain refinement of a Fe3Al-based alloy using κ-Fe3AlC precipitate particles stimulating nucleation of recrystallization

Effects of particle distribution level on recrystallization were investigated in a Fe₃Al-based alloy containing coarse κ-Fe₃AlC precipitate particles. Volume fraction of 10–12% of rod-like κ particles with different size and interparticle spacing was introduced within the Fe₃Al matrix by changing the cooling rate from 1200 °C, which is above the precipitation temperature of the κ phase. These samples were warm rolled at 700 °C to a total reduction of 75%. Annealing of the warm rolled samples produced complete recrystallized structures. The average recrystallized grain size against interparticle spacing showed a valley-shaped curve with a minimum size of 20 μm. Orientation analyses of the warm rolled samples with high resolution EBSD method revealed that the valley shape of the curve may be explained by the particle stimulated nucleation density of recrystallization around κ particles, dependent on the particle distribution.     

The stress anomaly in FeAl–Fe3Al alloys

The anomalous stress peak observed near 500–600 °C in Fe–Al alloys has now been convincingly explained using a model of hardening by immobile thermal vacancies on the lower temperature side of the peak and the loss of hardening as these vacancies become mobile at higher temperatures. The large numbers of vacancies required for such hardening are associated with compositions close to stoichiometry, i.e. 40–50%Al, raising the question of whether such a vacancy hardening model can be adopted for Fe₃Al alloys, which show a similar stress peak anomaly. Examination of data on vacancy formation over the entire range of composition, Fe–Fe₃Al–FeAl, shows that, indeed, a vacancy hardening model appears capable of explaining the stress anomaly for both FeAl and Fe₃Al.     

HREM observation of grown-in antiphase boundaries in an Fe3Al based alloy

Atomic arrangements of grown-in antiphase boundaries (APBs) in Fe₃Al based alloy were observed by means of high resolution electron microscopy. According to the continuity of Fe and Al sublattices across the APBs in different crystallographic planes, all observed APBs were identified as next-nearest neighbour types. When observed edge-on, the grown-in APBs are very thin. The comparison of the contrast of the atomic columns in the close vicinity of the APBs and the interior of the domains indicates sharp, un-relaxed grown-in domain walls.     

Ordering in the sublattices of Fe3Al during the phase transformation B2↔D03

The temperature dependence of the iron concentrations in the individual sublattices of hyperstoichiometric binary Fe₇₂Al₂₈ and ternary Fe₆₈Al₂₈Cr₄ alloys were obtained from X-ray diffraction data measured in a high temperature vacuum chamber during linear heating around the phase transformation B2↔D0₃. A method for the processing of the diffraction pattern based on the splitting of the diffraction lines of the structure D0₃ into three groups is presented. Applying this method it was found that the structure B2 was not well developed in both samples. The maximum value of c_C≈0.8 gives S_B2 equal to 0.4 and 0.3 for binary and ternary alloy, respectively. The D0₃-order was not well developed too, because structure D0₃ arises from the structure B2. D0₃-ordering, i.e. redistribution of atoms within the sublattices A and B, is given only by the total number of iron atoms in these sublattices before the phase transformation B2↔D0₃.     

In-situ precipitation of Al2O3 and κ-Fe3AlC0.5 in iron aluminides through spark plasma sintering: Microstructures and mechanical properties

Iron aluminides are ordered intermetallic alloys which offer good resistance to corrosion and sulfidation. At the same time, their Achilles' heel is low ductility at room temperature and sometimes they have poor mechanical properties. By means of mechanical alloying and spark plasma sintering (MA–SPS) it is possible to obtain bulk nanostructured iron aluminides which show high hardness and high yield stress.

In this work we present the production of nanostructured powders and their consolidation through spark plasma sintering. The inevitable use of methanol as processing control agent (PCA) leads to a supersaturation in carbon and oxygen of the milled powder and a consequent in-situ precipitation of carbides and oxides during SPS. The presence of carbides, oxides and a nanostructured matrix leads to high mechanical properties with hardness 5.20 ± 0.05 GPa and a yield stress of 1305 MPa.     

Microstructures and mechanical properties of Fe3Al-based Fe–Al–C alloys

In this paper results on the microstructures and mechanical properties of Fe₃Al-based Fe–Al–C alloys with strengthening precipitates of the perovskite-type κ-phase Fe₃AlC_x are presented. The alloys are prepared by vacuum induction melting and cast into Cu-moulds. The composition of the Fe₃Al matrix of the investigated Fe–Al–C alloys varies between 23 and 29 at.% Al. The ternary C-additions range from 1 to 3 at.%. The microstructures of the alloys are characterised by means of light optical microscopy (LOM). Phase identification is performed by means of X-ray diffraction (XRD). The strength of the alloys as a function of temperature is determined through compression tests. The room-temperature ductility is evaluated by tensile tests. The fracture surfaces of the tensile specimens are analysed using scanning electron microscopy (SEM).     

Processing of high carbon Fe3Al based intermetallic alloy

A melting procedure for air induction melting (AIM) of an Fe₃Al based intermetallic alloy Fe-15.38 wt%Al-1.1 wt%C is described. Use of an appropriate slag cover during AIM results in elimination of hydrogen gas porosity in cast AIM ingots. Criteria for slag selection and slag to metal ratio are discussed. Refining by slag-metal reactions results in significant reduction in impurity levels (S, O, N) during AIM. Consequently, low cost raw materials such as mild steel scrap and commercial aluminium were used for melting the alloy. The AIM ingot exhibited excellent tensile properties. The ductility and hot workability of the ingot may be further improved by subsequent processing through electroslag remelting. It is also argued that the presence of carbon may be necessary to get AIM castings with desirable mechanical properties.     

Formation of interfacial voids in cast and micro-grained γ′-Ni3Al during high temperature oxidation

Specimens of cast and micro-grained γ′-Ni₃Al, which were produced with vacuum casting and unbalanced magnetron sputter deposition, respectively, were isothermally oxidised in air at 1473 K for different periods of time. The formation of interfacial voids at the alloy/oxide interface was observed with SEM, which indicated that there were more interfacial voids formed in the cast Ni₃Al than in the micro-grained alloy under the same oxidation conditions. A phenomenological equation describing the fraction of the void projected areas was established, in which the impingement and coalescence between voids during their growth was taken into consideration. It was elucidated that low vacancy density in the micro-grained Ni₃Al due to the high creep, re-crystallisation and the enhanced Al diffusion reduced the void percentage. Also, it was confirmed that aluminium evaporation, perhaps supplemented by surface diffusion, supplied most Al to the oxide scales formed above the interfacial voids.     

Hot deformation behavior of a Fe3Al-binary alloy in the A2 and B2-order regimes

A binary Fe₃Al alloy is investigated with respect to hot deformation behavior and microstructural as well as microtextural modifications. Applying the hot deformation simulator (WUMSI) to hot rolling conditions in the A2 and B2-order regimes in combination with data analysis, significant changes in deformation behavior are identified. These conditions are selected for performing hot rolling experiments. The differences in microstructure are investigated. On the basis of microtexture investigations by means of electron backscatter diffraction (EBSD) differences concerning orientation gradients and sub-grain structures are found. A model of combined order-related and non-order related effects is proposed explaining the observed material behavior. The information gained is the basis for the optimization of the thermomechanical treatment to produce ductile Fe₃Al sheet material.     

Strengthening of iron aluminide alloys by atomic ordering and Laves phase precipitation for high-temperature applications

The ternary system Fe–Al–Ta allows the formation of the hard and brittle ternary Laves phase Ta(Fe_0.5+x,Al_0.5−x)₂ with hexagonal C14 structure. The present study concentrates on Fe–Al–Ta alloys with small Ta contents between 2 and 6 at.% and various Al contents between 0 and 45 at.%. The phase equilibria in the ternary Fe–Al–Ta system at 1000 °C are studied experimentally for determination of the solubility limits of Ta in iron aluminide matrices and types of phases and structures which may occur at high temperatures. It is observed that small amounts of Laves phase together with atomic ordering increase the yield stress and affect ductility in a complex way.     

Effective formation energies of atomic defects in D03Fe3Al: an ab-initio study

The effective formation energies of atomic defects in D0₃---Fe₃Al are determined within the framework of a grand-canonical statistical method. The grand-canonical defect formation energies entering this method are calculated by the ab-initio mixed-basis pseudopotential method. Thermal vacancies appear on the sublattice of the Fe atoms with an effective formation energy of 1.25 eV and on the Al sublattice (about 1.4 eV). The structural defects are Al antisite atoms on the γ sublattice of the Fe atoms or Fe antisite atoms on the Al sublattice.     

Shear-induced chemical disordering in Ni3Al at different temperatures

Molecular dynamics simulations have been used to study shear-induced chemical disordering in Ni₃Al lattices at different temperatures and strain rates. Shearing determines the formation of an amorphous layer, the thickness of which increases linearly with the square root of time. The rate at which the amorphous layer grows is both shearing rate- and temperature-dependent. A linear correlation between the amorphous layer growth rate and the shear modulus is found. This suggests that mechanical properties could play a central role in shear-induced disordering processes.     

Strong bonding of infrared brazed α2-Ti3Al and Ti–6Al–4V using Ti–Cu–Ni fillers

Infrared dissimilar brazing of α₂-Ti₃Al and Ti–6Al–4V using Ti–15Cu–25Ni and Ti–15Cu–15Ni filler metals has been performed in this study. The brazed joint consists primarily of Ti-rich and Ti₂Ni phases, and there is no interfacial phase among the braze alloy, α₂-Ti₃Al and Ti–6Al–4V substrates. The existence of the Ti₂Ni intermetallic compound is detrimental to the bonding strength of the joint. The amount of Ti₂Ni decreases with increasing brazing temperature and/or time due to the depletion of Ni content from the braze alloy into the Ti–6Al–4V substrate during brazing. The shear strength of the brazed joint free of the blocky Ti₂Ni phase is comparable with that of the α₂-Ti₃Al substrate, and strong bonding can thus be obtained.     

Small punch creep in Fe28Al3Cr0.02Ce alloy

Small punch testing of Fe₃Al-based intermetallic alloy with Cr, Mn and Ce additions was performed in temperature range 773–873 K. It is shown that the testing procedure enables to study the creep properties of the alloy. The time dependence of the central deflection resembles creep curves observed in conventional uniaxial creep testing and the minimum deflection rate can be determined. Similarly as in conventional creep tests, the deflection process is then analyzed in terms of the activation energy and force exponent. In accordance with the phase structure of the alloy, two distinct areas can be observed. In the B2 range, the activation energy equals 181 kJ/mol; the force exponent is about 4.6. In the DO₃ range, the activation energy equals 82 kJ/mol and the stress exponent is about 44. The transformation temperature DO₃B2 is close to 812 K. The technique can be used for an estimation of creep resistance.     

The oxidation of nanocrystalline Ni3Al fabricated by mechanical alloying and spark plasma sintering

Nanocrystalline Ni₃Al was fabricated through mechanical alloying of elemental powders and spark plasma sintering. The nanocrystalline Ni₃Al has a nearly full density after being sintered at 1223 K for 10 min under a pressure of 65 MPa. Isothermal and cyclic oxidations of nanocrystalline Ni₃Al were tested at 1173–1373 K with intervals of 100 K. The results indicate that nanocrystalline Ni₃Al exhibits excellent isothermal and cyclical oxidation resistance. The oxide scales consist primarily of dense and continuous -Al₂O₃. The grain refinement is beneficial for improving the oxidation resistance of Ni₃Al by providing more nucleation centers for the Al₂O₃ formation, promoting the selective formation of Al₂O₃ and improving the adhesion of oxide scales to the matrix.     

Evaluation of high temperature corrosion resistance of a Ni3Al (Mo) alloy

The sulfidation/oxidation and carburization resistances of a Ni₃Al(Mo) (IC-6) alloy at high temperatures were investigated in this work. The corrosion kinetics of the IC-6 alloy was found to follow parabolic rate law in an environment of high partial pressures of sulfur (10⁻⁵ atm) and low partial pressures of oxygen (<10⁻²⁰ atm) at 700 °C. Because the Ni sulfides are readily formed at the testing temperature, the sulfidation/oxidation resistance of the IC-6 alloy is similar to that of commercial Ni–Cr alloys in the current environments, although IC-6 is alloyed with Al. Compared with the HP heat resistant steel which is commonly used in the petrochemical industry, the IC-6 alloy possesses significantly improved resistance to carburization at 1100 °C. The mechanisms governing the corrosion attack in the environments used in this investigation were also discussed.     

Grain boundary self-diffusion of Ni in pure and boron-doped Ni3Al

Grain boundary (gb) self-diffusion in pure Ni-rich Ni₃Al was measured between 882 and 1374 K using the radiotracer ⁶³Ni, a serial sectioning technique and sensitive liquid scintillation counting. The results of the gb diffusivity P = δD_gb (δ : gb width, D_gb : gb diffusion coefficient) can be represented by the Arrhenius parameters P₀ = 3.27 · 10¹³and Q_gb = 168 kJ/mol. Additionally gb diffusion was investigated in boron-doped (0.24 at%) Ni-rich Ni₃Al in the range from 882 to 1352 K yielding P₀ = 1.24 · 10⁻¹² m³/s and Q_gb = 187 kJ/mol. The increase in the activation enthalpy Q_gb and the decrease of P upon boron-doping is explained by the segregation of B in Ni₃Al gbs, which may lead to an increase in the vacancy formation enthalpy and to a blocking of energetically favourable diffusion paths in the gbs. For comparison gb self-diffusion in pure Ni was remeasured yielding Q_gb = 112 kJ/mol. Ordering of the lattice and the preservation of ordering up to the gb planes, as predicted in Ni₃Al, therefore has a pronounced decelerating influence on gb diffusion, stronger than on bulk diffusion. Applying the semi-empirical relation of Borisov et al. (Phys. Met. Metallogr., 17 (1964) 80) gb energies γ_gb were determined for arbitrary high angle gbs in pure and B-doped Ni₃Al, resulting in 915 and 870 mJ/m², respectively, at 1100 K.     

On the parameters affecting the formation of iron aluminides during pressure-assisted infiltration of aluminium into a preform of steel fibres

The parameters affecting the formation of iron aluminides during reactive infiltration of iron-based fibre preforms in a squeeze-casting equipment were investigated. The volume fraction of intermetallic phases was found to increase when the fibre volume fraction and size decreased. The increase of the temperatures of the die, aluminium and preform allowed avoiding premature chocking of the preforms, reducing the gradient of reaction and increasing the extent of exothermic reactions. As-infiltrated material with overall chemical composition corresponding to Fe₃Al was studied by SEM, X-ray diffraction and TEM. The unreacted iron fibres were surrounded by iron-rich FeAl phases. The single-phase grains adjacent to the boundary layer were identified as Fe₂Al₅ whereas the grains with lamellar morphology were identified as consisting of a mixture of FeAl and FeAl₂ lamellae. Heat treatment of such an as-infiltrated material resulted in the formation of a fine-grained structure composed of FeAl and Fe₃Al phases.     

Deformation behaviour and oxidation resistance of single-phase and two-phase L21-ordered Fe–Al–Ti alloys

Single-phase Fe–Al–Ti alloys with the Heusler-type L2₁ structure and two-phase L2₁ Fe–Al–Ti alloys with MgZn₂-type Laves phase or Mn₂₃Th₆-type τ₂ phase precipitates were studied with respect to hardness at room temperature, compressive 0.2% yield stress at 20–1100 °C, brittle-to-ductile transition temperature (BDTT), creep resistance at 800 and 1000 °C and oxidation resistance at 20–1000 °C. At high temperatures the L2₁ Fe–Al–Ti alloys show considerable strength and creep resistance which are superior to other iron aluminide alloys. Alloys with not too high Ti and Al contents exhibit a yield stress anomaly with a maximum at temperatures as high as 750 °C. BDTT ranges between 675 and 900 °C. Oxidation at 900 °C is controlled by parabolic scale growth.     

Grain growth and precipitation in an annealed cold-rolled Ni50.2Ti49.8 alloy

In this paper we present a transmission electron microscopic study on the effect of annealing on the microstructure of a cold-rolled Ni_50.2Ti_49.8 ribbon. Transmission electron microscopy of the as-received sample shows the presence of alternating amorphous and crystalline bands. The crystalline bands have widths of the order of a few microns and contain amorphous nanopockets and B2 nanograins, the latter at around 20 nm diameter and preferentially oriented with their normal along the 111 direction and perpendicular to the strip surface. As-received samples were annealed for 30 min at different temperatures up to 800 °C. Crystallization starts in the amorphous bands at around 350 °C and finally ends up with the coarsening of the grains in the entire sample. Annealing of the samples at 450 °C entirely transforms the amorphous bands into crystalline bands. At 800 °C the grain size increases to 30–50 μm with a formation of a tweed kind of morphology inside the grains when observed at room temperature. Diffraction patterns from such grains reveal the presence of diffuse intensity around 1/3110^* indicating the formation of the R-phase. NiTi₂ precipitates form at 450 °C while annealing at 600 °C and higher yields Ni₃Ti₂ precipitates. For samples annealed at 500 °C for a longer time, Ni₄Ti₃ precipitates have been observed along with the austenite to martensite transformation in the grains.