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).     

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.     

Vacancy strengthening in Fe3Al iron aluminides

The room temperature strength of FeAl alloys can be increased significantly by freezing in the high thermal vacancy concentrations present at elevated temperatures. In contrast, because of their lower thermal vacancy concentrations, vacancy strengthening in quenched Fe₃Al alloys is believed to be much smaller and has not received much attention to date. In the present work, the influence of annealing time and quench temperature on the room temperature strength of extruded and recrystallized Fe₃Al alloys is evaluated. For aluminum concentrations between 28 and 32 at% and quench temperatures between 400 and 900 °C both the magnitude and the kinetics of strengthening are found to be consistent with reported values for the thermal vacancy concentrations and vacancy migration rates. To assess the potential contributions of other strengthening mechanisms, appropriate heat treatments will need to be designed in follow-on studies that alter microstructural features relevant to those mechanisms while maintaining a constant vacancy concentration.     

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.     

Metal dusting of binary iron aluminium alloys at 600 °C

In this work experiments on metal dusting of binary iron aluminium alloys with 15, 26 and 40 at.% Al were performed in strongly carburising CO‐H₂‐H₂O gas mixtures at 600 °C. The mass gain kinetics was measured using thermogravimetric analysis (TGA). The carburised samples were characterised by means of light optical microscopy (LOM), scanning electron microscopy (SEM), X‐ray diffraction (XRD) and X‐ray photoelectron spectroscopy (XPS). It was found that the mass gain kinetics depends on the CO content of the gas mixtures and on the Al content of the alloys. With decreasing carbon activity the carburisation reaction kinetics decreases and the onset of metal dusting is retarded for increasing time periods. With increasing Al content of the alloys the carburisation reaction is slower and metal dusting sets on at later times. The samples were not pre‐treated for the formation of a protective oxide scale. By X‐ray Photoelectron Spectroscopy (XPS) analyses of the carburised iron aluminium samples it was found that the formation of Al₂O₃ layers has taken place in the CO‐H₂‐H₂O gas atmospheres. Needle‐ or plate‐like κ‐phase (Fe₃AlC_x) precipitates close to the surface of the carburised Fe‐15Al sample were detected by means of XRD and LOM. The coke on top of the carburised samples mainly consists of filamentous carbon with metal particles at their tips.     

Effect of Al concentration on pseudoelasticity in Fe3Al single crystals

Pseudoelasticity in Fe₃Al single crystals with different Al contents was investigated focusing on the dislocation configuration and the ordered domain structure. Giant pseudoelasticity only appeared in the D0₃-ordered Fe₃Al single crystals, while the B2-ordered crystals and those with the disordered phase exhibited small strain recovery. The amount of shape recovery in the D0₃-ordered crystals showed a maximum near 23.0at.%Al and decreased with increasing deviation from this Al concentration. In the D0₃ phase at 22.0–25.0at.%Al, 1/4[1 1 1] superpartial dislocations moved individually dragging the nearest-neighbour antiphase boundaries (NNAPB), while couplets of the superpartials were observed to bow out, dragging the next-nearest-neighbour antiphase boundaries (NNNAPB) in Fe–28.0at.%Al. In Fe–22.0–25.0at.%Al single crystals, the NNAPB pulled back the superpartials to decrease its energy during unloading, resulting in the giant pseudoelasticity. In contrast, the surface tension of the NNNAPB was lower than that of the NNAPB, leading to the small strain recovery in Fe–28.0at.%Al.     

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.     

Possibilities for high-temperature strengthening in iron aluminides

Iron aluminides based on Fe₃Al and on FeAl offer considerable possibilities for development as intermediate temperature materials operating in aggressive chemical environments. Two major property limitations restrict their application: low toughness, related to their environmental sensitivity, and poor high temperature creep resistance. Considerable attention has been given to the intermediate stress but, while many of its characteristics are well documented, there remains considerable uncertainty about the controlling mechanisms. Plastic deformation at temperatures above the stress peak can be analysed in terms of thermally-activated, creep-like flow, with a steady evolution during deformation of many of the controlling parameters. Two avenues can be explored for improving high temperature behaviour: modify the diffusive flow behaviour and restrict dislocation motion at dispersed particles. There is considerable evidence that control of matrix composition can lead to large changes in diffusion parameters and the motion of dislocations. Dislocation pinning at particles depends on the availability of suitable particle phases, and examples of precipitated carbides, dispersed oxides, and decomposed intermetallic mixtures will be considered.     

The influence of order on the recovery and recrystallization of a Fe3Al alloy

The influence of annealing treatments over a range of temperatures encompassing the critical ordering temperature for the B2-DO₃ change and inducing recovery and recrystallization have been examined for a deformed alloy based on the Fe₃Al composition. The initial ordered state before heavy deformation plays no role on subsequent recovery and recrystallization, essentially because the heavy deformation destroys the prior order. Recovery occurs faster relative to the rate of recrystallization at higher temperatures. The extended period at lower temperatures where poorly recovered structures remain allows grain nucleation mechanisms to remain activated, in contrast to higher temperature situations where grain nucleation slows as grain growth dominates recrystallization. This evolution is slightly enhanced at lower temperatures as DO₃ order appears, and leads to finer final grains after such lower temperature anneals. There is no evidence to indicate that dislocations influence the rate of ordering of this material.     

High temperature oxidation behaviour of a TiAl-Al2O3 intermetallic matrix composite

A TiAl-based intermetallic matrix composite has been produced through sintering of mechanically milled Al/TiO₂ composite powder. The composite contains 42-50 vol.% of α-Al₂O₃ as the particulate reinforcement phase. Oxidation experiments were carried out at 800-900 °C in air up to 500 h to evaluate its oxidation and scale spallation resistance. A cast Ti-50at.%Al alloy was also tested for comparison. The composite samples showed much lower oxidation mass gain than the cast alloy under all testing conditions. Moreover, the composite samples exhibited extremely strong scale spallation resistance. Spallation could never be recorded and observed even under long-time intensive cyclic oxidation exposure. Based on the kinetic and microstructural studies, the mechanisms for the improved oxidation and spallation resistance are discussed.     

Fe3Nb3N precipitates of the Fe3W3C type in Nb stabilized ferritic stainless steel

A Nb stabilized ferritic stainless steel with 0.45 wt.%Nb, 82 ppm C and 170 ppm N is investigated to reveal the nature of the precipitates present at 950 °C. In particular, Fe₃Nb₃X precipitates of the Fe₃W₃C type are analyzed with WDS and EELS to determine the light elements X stabilizing this phase in the steel. According to WDS on large precipitates after 500 h at 950 °C, the Fe₃Nb₃X phase contains 10.4 at.% N, 1.2 at.% O and 1.0 at.% C. Auger Electron Spectroscopy on the same precipitates confirms the presence of N. In addition, it is revealed that the C and O peaks observed with WDS result from surface contamination as they disappear after Ar sputtering. The presence of a N peak in the EELS spectra of small Fe₃Nb₃X precipitates which have formed after 6 min at 950 °C indicate that N stabilizes this phase already from the initial precipitation stage. With this analysis it is demonstrated that N is an effective stabilizer of Fe₃Nb₃X precipitates in ferritic stainless steels. The formation of this phase should therefore be considered when predicting the precipitation behavior of Nb in industrial Nb stabilized ferritic stainless steels containing residual N.     

The effect of carbon and reactive element dopants on oxidation lifetime of FeAl

Wrought Fe–40 at.%Al has an unexpectedly short time to breakaway oxidation at 1200 °C compared to Fe₃Al. Optimizing the reactive element to C ratio by either removing the C addition or by replacing Zr with Hf, increased the oxidation lifetime by a factor of two or six, respectively.     

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.     

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.     

Pt改性Ni3Al基合金短时高温氧化行为研究

用冷坩埚悬浮熔炼制备了Ni-xPt-25Al(x=0,10,20,30,at%)系列合金,利用X射线衍射仪、同步热分析仪、扫描电镜和光电子能谱仪(XPS)分析了Pt的添加对晶体结构的影响,研究了Ni-xPt-25Al合金的氧化动力学曲线、氧化物形貌以及抗氧化性能。结果表明:随着Pt含量的升高,Pt改性Ni_3Al基合金仍保持γ′相。升温过程和短时等温阶段合金的氧化动力学特征分别符合线性和抛物线氧化物生长动力学规律。Pt有利于氧化物的快速形成,且随Pt含量的增加,氧化膜的完整性和致密性均有所改善。     

Effects of Cr-addition and lamellar microstructure on the oxidation behavior of single crystal (Mo0.85Nb0.15)Si2

The oxidation behavior of (Mo_0.85Nb_0.15)Si₂ single crystals and the influence of Cr-addition were studied focusing on its microstructure dependence. Cr-addition to single-phase C40-structured (Mo_0.85Nb_0.15)Si₂ crystal induced the formation of crystalline silica, leading to slightly larger weight gain during the oxidation test at 1200 °C. Furthermore, Cr-addition to C40/C11_b duplex-phase (Mo_0.85Nb_0.15)Si₂ crystal with lamellar structure strongly suppressed the internal oxidation of the C11_b phase, resulting in excellent oxidation resistance. C40/C11_b lamellae-structured crystals showed better oxidation resistance than the C40-structured crystals.     

Processing of Fe3Al and FeAl alloys by reaction synthesis

The effects of powder particle size, alloy composition, and reaction atmosphere on reaction synthesis of binary Fe---Al alloys were studied. Reactions were observed in an open (air) furnace, under static vacuum (in an evacuated quartz tube) and in a dynamic vacuum furnace. Reactions occurring in the open furnace and in the evacuated quartz tube were recorded using high-speed video equipment. High-speed videotapes of reaction synthesis of compacts formed from 45 μm Fe and 10 μm Al particles reacted in air and under static vacuum revealed that an unusual ‘two-stage’ reaction exists in this system under these conditions. Compacts formed from 9 μm Fe and 3 μm Al powder particles do not exhibit a two-stage reaction under any of the conditions examined in this work. The first stage of the two-stage reaction lasts several seconds and starts at round 650 °C. The second stage begins at about 900 °C, reaching temperatures between 1250 and 1350 °C. The progress of the reaction to the second stage is sensitive to the alloy composition and reaction atmosphere. The reaction behavior is explained in terms of thermodynamics and heat transfer, which control the delicate balance between heat accumulation and heat loss during reaction synthesis.     

High-temperature oxidation of SiC in a glow-discharge oxygen plasma

The oxidation kinetics and structure of the oxide scales formed on high-density SiC were studied in molecular oxygen at 740 Torr and in a glow-discharge oxygen plasma at 0.1 Torr at temperatures of 1000, 1100, and 1200°C. The monatomic oxygen formed by the glow discharge markedly increased the reaction rate and the vaporization of some of the oxidation products. The marked differences in kinetics suggest that the rate-controlling step during oxidation in molecular oxygen is the dissociation of adsorbed diatomic oxygen to the monatomic species. Films formed in molecular oxygen were mostly amorphous SiO₂ with small inclusions of SiC and graphite, whereas films formed in dissociated oxygen were primarily amorphous SiO₂ containing SiO, S₂O₃, and the coesite form of SiO₂.     

Optimisation of precipitation for controlling recrystallisation of wrought Fe3Al based alloys

A Fe–26Al–5Cr (at.%) single-phase (:A2/B2/D0₃) alloy and two-phase (+TiC) alloys with different amounts of TiC particles have been hot rolled at 800 °C and the kinetics of static recrystallisation have been studied. In the alloys with a high amount of TiC, needle-like TiC of more than 1 μm in length formed during cooling after homogenisation in the single-phase region and coarsened during hot rolling. The large particles cause particle stimulated nucleation (PSN) and hence accelerate recrystallisation. In order to accomplish both strengthening by precipitates and inhibition of recrystallisation that deteriorates room-temperature ductility, a thermo-mechanical treatment consisting of hot deformation with a low amount of precipitates and a subsequent heat treatment for further precipitation is proposed. This process is difficult to carry out in the (Fe–26Al–5Cr)–TiC system due to the high precipitation temperature of TiC. The precipitation temperature is significantly decreased by replacing TiC by VC or MoC.     

High-temperature oxidation of a nickel base superalloy at different oxygen partial pressures

A series of oxidation tests were conducted for a nickel base superalloy, as these materials are used at high temperature in aggressive conditions, thus the influence of oxygen on their degradation mechanisms must be known. The material was treated for up to 150?h at 900 and 1000°C in a furnace able to control and maintain atmospheres with different partial oxygen pressures. The oxidation rate of the material was determined by gravimetric means. In all cases, the rate of oxidation followed parabolic regimes that depended on the value of oxygen partial pressure. The oxide scale formed was characterised by X-ray diffraction and scanning electron microscopy; these analyses revealed that the oxide scale consisted of an outer TiO₂ layer and inner Cr₂O₃ layer under all experimental conditions. Cross-section analyses indicated the development of internal oxidation and the presence of gamma-prime free zones.