Mechanism of Al2CuLi (T 1) nucleation and growth

Conventional strain contrast transmission electron microscopy (CTEM) and high-resolution transmission electron microscopy (HRTEM) were performed to establish the nucleation and growth mechanism of Al₂CuLi (T₁) precipitates in an Al-Li-Cu alloy. It is shown that the growth mechanism ofT ₁ precipitate plates occurs by the diffusional glide of growth ledges composed of b = 1/6〈112〉 partial dislocations on 111 matrix planes and that the growth ledges migrate by the ledge-kink mechanism, as previously suggested by Cassadaet al. 1 for this system.T ₁ plate nucleation is modeled as the dissociation of a perfect b = 1/2〈110〉 matrix dislocation in the vicinity of a dislocation jog. The coordinated dissociation of the dislocation line segments on each side of the sessile jog provides the displacement necessary for the formation of a new hexagonal plate or plate ledge. Strain contrast analysis of the Burgers vector of plate edges and the edges of growth ledges indicates the stacking of partial dislocations is of mixed displacement. Formerly Graduate Student, Department of Materials Science, University of Virginia,     

Phase transformations in the Al-Li-Hf and Al-Li-Ti systems

Phase transformations in Al-1, 9Li-1.6Hf and Al-1.5Li-0.7Ti (wt pct) alloys have been analyzed thoroughly using various electron microscopy techniques. An Ll₂-ordered ternary Al₃ (Li,X) phase, orά (X), forms in both alloys during heat treatment. Theά forms as spherical precipitates by normal nucleation and growth and in the Hf alloy as filaments by discontinuous precipitation. The X:Li ratio in these precipitates is found to be a function of the precipitation mode in the Hf alloy.ά is coherent with the Al matrix and serves as a preferred nucleation site for the precipitation of the Al₃Li orδ' phase when the alloy is aged at 190°C. Theδ', also Ll₂-ordered, grows as continous envelopes which completely enclose theα' phase. An altered morphology predominates forα'(Ti) after extended heat treatment. The major feature of the altered morphology is the incorporation of spiraled dislocations at theα'/matrix interface, which act to ease the misfit between theα' (Ti) and the matrix.δ' forms as caps on the alteredα'(Ti) in areas away from the dislocations. Disruption of theα' envelopes is attributed to the strain fields and loss of coherency associated with the presence of interfacial dislocations and a possible local shift from Ll₂ to DO₂₂ ordering in theα'(Ti) precipitates.     

Effect of T1 precipitate on the anisotropy of AlLi alloy 2090

A study has been made of the effect of T₁ precipitate on the anisotropy of an AlLi alloy 2090. The critical role of T₁ precipitates has been identified by comparing the behavior of the alloy with various microstructures. These include (1) T8E41 tempered specimen with T₁, θ′ and δ′, (2) reverted specimen with T₁, (3) re-solutioning specimen with very fine δ′, and (4) under-aged specimen with fine δ′ and θ′. It has been shown that the {110}〈112〉 crystallographic texture developed during thermomechanical treatment has a direct effect on the anistropy. It also has an indirect effect by causing an inhomogeneous distribution of nucleation sites for T₁ among four {111} habit planes during stretching and accordingly inhomogeneous distribution of T₁ precipitates among four possible {111} planes during aging. Such inhomogeneously distributed T₁ precipitates in both T8E41 tempered and reverted specimens affect the variation of tensile properties, particularly elongation with specimen orientation.     

The precipitation of Ni3Nb phases in a Ni−Fe−Cr−Nb alloy

The age hardening of a Ni?Fe?Cr?Nb alloy containing 4.85 wt pct Nb has been studied using transmission electron microscopy. The major hardening phase in this alloy isγ*, DO₂₂-ordered Ni₃Nb, which precipitates as a fine dispersion of square plates. It is shown that nucleation ofγ* plates may be dependent upon matrix excess vacancy concentration, but nucleation ofγ* plates is also observed at dislocations and extrinsic stacking faults. Theγ* phase is metastable with respect to the orthorhombic Ni₃Nb phase, β, which precipitates by either a cellular or an intragranular reaction, depending upon the aging temperature. It is proposed that the intragranular nucleation of β laths proceeds by the growth of stacking faults from withinγ* plates; theγ* plates subsequently dissolve in favor of the β laths. Room temperature deformation of theγ* dispersion is shown to produce faults within theγ* plates; possible dislocation reactions occurring during this deformation are discussed.     

The effect of plastic deformation on Al2CuLi (T 1) precipitation

The enhancement ofT ₁ precipitation in Al-Li-Cu alloys by plastic deformation prior to aging (that is, cold work) and the subsequent increase in alloy strength is investigated. The increased understanding of the role of matrix dislocations in the nucleation and growth ofT ₁ plates, discussed in the previous paper,^[1] permits a detailed study of the phenomenon. In this paper, the effect of different levels of plastic strain on theT ₁ particle distributions as a function of aging time at 190 °C is quantified, and the subsequent influence on tensile properties is thereby described. The effect of plastic deformation is shown to decrease theT ₁ plate length and thickness, increase the number density by almost two orders of magnitude, increase the yield strength by 100 MPa, while simultaneously reaching peak strength in 20 pct of the time required without plastic deformation. Formerly Graduate Student, Department of Materials Science, University of Virginia,     

Plastic deformation and fracture of binary TiAl-base alloys

The mechanical behavior of binary TiAl alloys containing 46 to 60 at. pct Al has been studied in bulk materials preparedvia rapid solidification processing. Bending and tensile tests were carried out at room temperature as a function of Al concentration. A few alloys were also tested from liquid nitrogen temperature to ∼ 1000°C. Deformation substructures were studied by analytical transmission electron microscopy and fracture modes by scanning electron microscopy (SEM). It was found that both microstructure and composition strongly affect the mechanical behavior of TiAl-base alloys. A duplex structure, which contains both primary y grains and transformedγ/α ₂ lamellar grains, is more deformable than a single-phase or a fully transformed structure. The highest plasticities are observed in duplex alloys containing 48–50 at. pct Al after heat treatment in the center of theγ + α phase field. The deformation of these duplex alloys is facilitated by 1/2[110] slip and {111} twinning, but very limited superdislocation slip occurs. The twin deformation is suggested to result from a lowered stacking fault energy due to oxygen depletion or an intrinsic change in chemical bonding. Other factors, such as grain size and grain boundary chemistry and structure, are important from a fracture point of view. The results on the deformation and fracture modes as a function of test temperature are also discussed.     

Microscopy and tensile behavior of melt-spun Ni-Al-Fe alloys

Microscopy and room-temperature tensile tests were performed on as-spun and annealed ribbons of Ni-20 (at. pet) Al-Fe alloys containing 20 to 40Fe. The ribbons had the duplex structures consisting of grains of ordered bec β-NiAl and grains of disordered fee γ-Ni, which contains precipitates of γ′-Ni₃Al. The 25 to 30Fe alloys exhibited high ductility (∼10 pet elongation) in both the as-spun and annealed conditions. These results indicate that rapid solidification-induced effects, such as the suppression of ordering, do not enhance ductility as previously reported. The ductile alloys were found to contain high dislocation densities in both they and β grains, with no evidence of stress-induced martensite formation in the β phase. Dislocation analysis revealed that the vast majority of dislocations in theβ had ≤100≥Burgers vectors; however, ≤111≥ dislocations were also observed. Additionally, slip bands were frequently observed meeting at γ-β grain boundaries. Since they tend to align across the interphase grain boundary, deformation transfer between γ and β is inferred. The deformation transfer was found to be facilitated by a specific orientation relationship between the grains. The unusual deformation of ββby ≤111≥ slip and by deformation transfer from neighboring grains may be responsible for the high ductility.     

Transformation characteristics of α1 Plates in Cu-Zn-Al Alloys

The formation of α₁ plates during isothermal aging of a Cu-26.7 wt pct Zn-4.0 wt pct Al alloy at 150 °C to 350 °C follows thermally activated incubation kinetics. Early stage α₁ plates possess an ordered 18R or 9R long-period stacking order (LPSO) crystal structure, with antiphase domain boundaries running continuously across the interface. The plates also exhibit invariant plane strain (IPS) crystallography consistent with calculations of the phenomenological theory of martensite crystallography (PTMC). The ordered LPSO structure and IPS crystallography are gradually annealed out only after extended aging as the structure changes to the equilibrium disordered face-centered cubic (fcc) one. High-resolution transmission electron microscopy (TEM) analyses reveal that early stage α₁ plates have straight coherent interfaces. Prolonged aging induces misfit dislocations at the interface and causes the interface to protrude into the parent phase. Although microanalytical analyses indicate that a composition difference exists between the α₁ plates and the parent matrix, solute depletion was observed at neighboring defects. These observations support the proposed transformation mechanism that the α₁ plates nucleate at solute depleted defects through a shear mechanism and that subsequent plate growth is then controlled by a diffusional process. Formerly Visiting Scientist, with the Department of Materials Science and Engineering, University of Illinois     

Effects of carbon content and ausaging on γ ↔ α′ transformation behavior and reverse-transformed structure in Fe-Ni-Co-Al-C alloys

The effects of carbon content and ausaging on austenite γ ↔ martensite (α′) transformation behavior and reverse-transformed structure were investigated in Fe-32Ni-12Co-4Al and Fe-(26,28)Ni-12Co-4Al-0.4C (wt pct) alloys. TheM _s temperature, the hardness of γ phase, and the tetragonality of α′ increase with increasing ausaging time, and these values are higher in the carbon-bearing alloys in most cases. The γ → α′ transformation behavior is similar to that of thermoelastic martensite; that is, the width of α′ plate increases with decreasing temperature in all alloys. The αt’ → γ reverse transformation temperature is lower in the carbon-bearing alloys, which means that the shape memory effect is improved by the addition of carbon. The maximum shape recovery of 84 pct is obtained in Fe-28Ni-12Co-4Al-0.4C alloy when the ausaged specimen is deformed at theM _s temperature and heated to 1120 K. There are two types of reverse-transformed austenites in the carbon-bearing alloy. One type is the reversed y containing many dislocations which were formed when the γ/α′ interface moved reversibly. The plane on which dislocations lie is (01 l)_γ if the twin plane is (112)_α′. The other type of reverse-transformed austenite exhibits γ islands nucleated within the α′ plates.     

Deformation and transition behavior associated with theR-phase in Ti-Ni alloys

Deformation behavior associated with theR-phase (rhombohedral phase) transition and the subsequent martensitic transformation was studied systematically in Ti-Ni alloys by tensile testing over a wide temperature range covering belowM _f to aboveT′ _R (>A_f). Since the deformation and transition characteristics showed a strong dependence on thermo-mechanical treatment and Ni-content, internal structures were examined by electron microscopy in specimens with various Ni-content and thermo-mechanical treatment. As a result precipitates and/or dislocations were revealed in the specimens in which theR-phase transition occurs. Based on the above results, the effects of thermo-mechanical treatment and Ni-content on the deformation and transition characteristics were clarified for both theR-phase transition and the martensitic transformation.     

On the formation of 2H stacking sequence in 18R martensite plates in a precipitate containing CuAlNiTiMn alloy

Basal planes stacking sequence variation in M18R martensite of CuAlNiTiMn alloy have been studied by means of electron diffraction and lattice imaging. Samples subjected to two different homogenisation temperatures (1173 and 973K) and two different cooling rates—water quenched and air cooled were analysed. The observed changes in stacking sequence have been attributed mainly to stress accomodation around X_L and X_S precipitates. Very small X_SS precipitates of the same phase have been observed and their high influence on the stacking sequence of martensite plates have been explained by means of a new “dislocation” mechanism related to their coherency loss into the matrix.     

The identification of hydrogen trapping states in an Al-Li-Cu-Zr alloy using thermal desorption spectroscopy

Thermal desorption spectroscopy (TDS) was utilized to identify several metallurgical states in an Al -2Li - 2Cu-0.1Zr (wt pct) alloy, which trap absorbed hydrogen. Six distinct metallurgical desorption states for hydrogen were observed for tempers varying from the T3 to peakaged condition. Lower energy thermal desorption states were correlated with interstitial sites, lithium in solid solution, and δ′ (Al₃Li) precipitates. These states have trap-binding energies ≤25.2 kJ/mol. Under the charging conditions utilized, approximately 4 pct of the total (e.g., trapped and lattice) hydrogen content was associated with interstitial sites, consistent with the view that the intrinsic lattice solubility of hydrogen in aluminum is very low. In contrast, dislocations, grain boundaries, and T₁ (Al₂CuLi) particles were found to be higher energy-trap states with trap-binding energies ≥31.7 kJ/mol. Approximately 78 pct of all absorbed hydrogen occupied these states. Moreover, greater than 13 pct of the available trap sites at grain boundaries were occupied. Such a high hydrogen coverage at grain-boundary sites supports the notion that hydrogen contributes to grain-boundary environmental cracking in Al-Li-Cu-Zr alloys. Also, it points out the error in assuming that hydrogen cannot play a major role in cracking of Al-based alloys due to the low lattice solubility.     

General existence of ledges on α1 plates in Cu-Zn-Al alloys

A transmission electron microscopy (TEM) study was made of the interphase boundary structure between the matrix and α₁ plates formed at 250 °C, 300 °C, and 350 °C in three Cu-Zn-Al alloys. The experiments showed that the α₁ plates formed at each temperature studied in all of the alloys are initially free of stacking faults. This observation, confirming the results of previous investigations, shows that these plates cannot have formed by a shear mechanism. Ledges were shown to exist on the broad faces and/or at the growth edges of the α₁ plates. Indirect evidence implies that the ledges are mobile and that they can migrate along different directions on the broad faces.     

Al–Cu–Li and Al–Mg–Li alloys: Phase composition,texture, and anisotropy of mechanical properties (Review)

The results of studying the phase transformations, the texture formation, and the anisotropy of the mechanical properties in Al–Cu–Li and Al–Mg–Li alloys are generalized. A technique and equations are developed to calculate the amounts of the S₁ (Al₂MgLi), T₁ (Al₂CuLi), and δ' (Al₃Li) phases. The fraction of the δ' phase in Al–Cu–Li alloys is shown to be significantly higher than in Al–Mg–Li alloys. Therefore, the role of the T₁ phase in the hardening of Al–Cu–Li alloys is thought to be overestimated, especially in alloys with more than 1.5% Li. A new model is proposed to describe the hardening of Al–Cu–Li alloys upon aging, and the results obtained with this model agree well with the experimental data. A texture, which is analogous to that in aluminum alloys, is shown to form in sheets semiproducts made of Al–Cu–Li and Al–Mg–Li alloys. The more pronounced anisotropy of the properties of lithium-containing aluminum alloys is caused by a significant fraction of the ordered coherent δ' phase, the deformation mechanism in which differs radically from that in the solid solution.     

Dislocation structures in disordered and ordered Ni3Fe

Transmission electron microscopy (TEM) methods have been used to examine the dislocation structures in thin foils of Ni₃Fe in four different states, corresponding to disordered and deformed; fully ordered and deformed; deformed when disordered and afterwards fully ordered; and deformed when disordered, afterwards fully ordered and additionally deformed. The study has been carried out on single crystals deformed at room temperature. In the disordered alloy slip is coarse and group motion of dislocations is prevailing, as is confirmed by the abundance of planar dislocation arrays. The dislocation structure of such a disordered deformed crystal remains unchanged after additional ordering by annealing 1000 h at 460°C. No rearrangement of the unit dislocations into superlattice dislocations is observed. The dislocations are preserved and since they are unit dislocations they are sessile. The additional deformation of this disordered deformed and afterwards fully ordered crystal proceeds by the glide of superlattice dislocations. They originate in the high internal stresses of the preserved unit dislocations. Cross slip from (111) onto (11̄1) planes is very frequent, whereas cross slip from (111) onto (010) planes is rather rare. The structure of the superlattice dislocations in fully ordered and deformed specimens consists of dipoles and bundles of dipoles of near edge orientation. Superlattice dislocations of near screw orientation are rarely observed, since they cross slip from (111) onto (11̄1) planes and annihilate in most cases. The experimental results on ordered Ni₃Fe samples differ characteristically from those reported in the literature on other alloys having the L1₂ long range ordered structure (e.g. Ni₃Al, Cu₃Au, Ni₃Ga).     

Grain-boundary precipitation in an Al4.0Cu0.5Mg0.5Ag alloy

Transmission electron microscopy and electron diffraction were used to study grain-boundary precipitation in an Al-4.0Cu-0.5Mg-0.5Ag (wt%) alloy. Low-angle grain-boundaries were found to nucleate Ω precipitates on the {111}_α planes even when the {100}_α habit planes of the competinng θ′ metastable phase were closer to the grain-boundary plane. High-angle grain-boundaries, which were random in nature and had relatively large energy, nucleated Ω precipitates predominantly. A few S precipitates and a θ precipitate (G IV/V orientation) were found to co-exist with Ω in these boundaries. The proximity of the grain-boundary plane to the {111}_α plane on which grain-boundary Ω nucleated was found to be particularly important in both low and high-angle grain-boundaries, similar to results for the θ′ phase in AlCu alloys.     

Effects of cold work on precipitation in Al-Cu-Mg-(Ag) and Al-Cu-Li-(Mg-Ag) alloys

A study has been made of the effects of cold work prior to aging on precipitation hardening in selected Al-Cu-Mg-(Ag) and Al-Cu-Li-(Mg-Ag) alloys. General aging characteristics have been determined by differential scanning calorimetry, and response to hardening has been correlated with microstructure using transmission electron microscopy (TEM), selected area electron dif-fraction (SAED), and quantitative stereology. Particular attention has been given to the phases Ω andT ₁ that form on the {111 }_α planes, although information on the precipitates θ′,S′ (orS), and δ′ is also reported. Although Ω andT ₁, have similar morphologies and habit planes, their response to cold work prior to aging is different. Deformation promotesT ₁ formation at the expense of the δ′ phase in Al-Cu-Li alloys and at the expense of δ′, θ′, andS′ in Al-Cu-Li-Mg-Ag alloys. On the other hand, in Al-Cu-Mg-Ag alloys, deformation assists precipitation of θ′ at the expense of Ω phase, and some decrease is recorded in the hardening response. Prior cold work is also found to reduce the response during natural aging in most alloys. These results are discussed in terms of the role of particular alloying additions. Formerly Research Fellow, Department of Materials Engineering, Monash University     

Microstructure and mechanical properties of a 2091 AlLi alloy—I. Microstructure investigated by SAXS and TEM

The microstructure of the 2091 alloy (AlLiCuMgZr) alloy has been studied and compared to that of two simpler AlLi and AlCuMg alloys. The SAXS, in situ SAXS and TEM techniques have been used for heat treatments at room temperature and at 150°C. The time evolution of the size and of the volume fraction of the δ′ precipitates and of the Cu-rich GPB zones have been determined. The δ′ precipitates are shown to follow a classical Lifschitz-Slyosov-Wagner law. Their interfacial energy has been estimated. S and S′ precipitates have also been characterized, respectively on grain boundaries and on helical dislocations, by TEM.     

Influence of precipitates on the mechanical response and substructure evolution of shock-loaded and quasi-statically deformed Al−Li−Cu alloys

The mechanical response and substructure evolution of two Al−Li−Cu alloys (Al-2.90 wt pct Li-1.00 pct Cu-0.12 pct Zr and Al-2.30 pct Li-2.85 pct Cu-0.12 pct Zr) subjected to shock-loading (strain rate έ> 10⁶ s^-1), Split-Hopkinson-Pressure-Bar compression (έ ~ 5 × 10³ s^-1), and quasi-static compression (έ ~ 1.5 × 10^-3 s^-1) were examined. The strain levels achieved in these three deformation paths were desined to be comparable,i.e., all ∼15 pct. Both alloys were either naturally or artificially aged to yield an underaged or overaged condition. Various precipitates, such as theδ' andT ₁ phase, of different sizes and volume fractions were dispersed in the matrix and at the grain boundaries. The substructure in all of the shock-loaded, Split-Hopkinson-Pressure-Bar, and quasi-static compression samples was characterized by localized slip bands and microbands with the exception of the overaged alloys. The density of dislocations and dislocation loops was higher, independent of the aging condition, in the shock-loaded specimens. Well-defined cell structures were not observed in any of the samples, independent of strain rate. The influence of precipitates, shearable or not, on the substructure development in Al−Li−Cu alloys during shock-loading was seen to be pronounced, even though the size and volume fraction of precipitates was small and low, respectively. Flow stress measurements showed that the shock-loaded samples have flow strengths 3 to 8 pct higher than the quasi-statically deformed samples. This small, but reproducible, strength increment, for alloys deformed to equivalent strains at low and high rates, indicates that the Al−Li alloys studied have a small rate sensitivity. Based upon comparison of the results of the shock-loaded and quasi-static samples, it is concluded that the fundamental deformation mechanisms and substructure evolution in all three loading paths are not drastically different, corroborating previous investigations.     

Precipitate stability in AlCuMgAg alloys aged at high temperatures

A study has been made of the thermal stability of the Ω phase in AlCuMgAg alloys aged at high temperatures (200 to 350°C). This phase, which precipitates as thin plates on the {111}_α planes, has been shown to be replaced by the equilibrium precipitate θ (Al₂Cu) after prolonged ageing (e.g. 2400 h at 250°C). Measurements have been made of the thickening behaviour of the Ω plates and the various orientations and morphologies of the θ phase have been characterised. Whilst there is some evidence for the direct allotropic transformation of Ω to θ, it is concluded that a gradual dissolution/re-precipitation mechanism dominates the changes to microstructure at these high temperatures. Although magnesium and silver are known to segregate to the Ω phase, they were not detected in association with θ. Rather they were found to partition to sites of the S phase (Al₂CuMg) which forms as a minor precipitate under these ageing conditions.