Microstructural stability on aging of an α + β titanium alloy: ti- 6ai- 1.6zr-3.3mo- 0.30si

The development of the microstructure on aging of an (α + β) type titanium alloy containing 6A1-1.6Zr-3.3Mo-0.3Si (VT9) (in weight percent) has been studied. The β-transus temperature of this alloy is approximately 1243 K. Solution treatment in the β-phase field of the alloy followed by quenching in water at room temperature resulted in the formation of a single-phase martensite struc-ture. The martensitic structure was confirmed to be orthorhombic (α″) using X-ray diffraction. The water-quenched (WQ) specimens were subjected to aging treatments at temperatures of 823, 873, and 973 K for various lengths of time. Aging at 823 K for times between 24 and 100 hours did not bring about any noticeable change in the microstructure. Aging at 823 K for 200 and 300 hours resulted in the heterogeneous precipitation ofs ₂ silicide particles and thin films of β sandwiched between the interplatelet boundaries of martensite. Electron diffraction analysis confirms that the crystal structure of silicide particles is hexagonal with lattice parameters α= 0.70(1) nm andc = 0.36(8) nm. Aging at 873 K for 12 and 24 hours resulted only in the precipitation ofs ₂ silicide particles, while aging at the same temperatures for longer times (48, 100, and 200 hours) and also at 973 K for 6 to 100 hours resulted in the precipitation of silicides and also thin films of β and acicular martensite. The relative sizes of silicide precipitates and width of thin films of β phase increase with increasing aging time. The sites for silicide precipitation are mainly at α′-α′ boundaries, α-β interfaces, and sometimes within regions of transformed β. The kinetics ofs ₂ silicide precipi-tation in this alloy is faster than in commercial near-α titanium alloys. This is attributed to the presence of Mo, a strong β stabilizer. Formerly Reader, Department of Metallurgical Engineering, Centre of Advanced Study, Institute of Technology, Banaras Hindu University, Varanasi-221 005, India     

Effect of silicide precipitation on tensile properties and fracture of alloy Ti-6Al-5Zr-0.5Mo-0.25Si

The effect of silicon in solid solution and in the form of suicides has been studied on the tensile properties and fracture behavior of alloy Ti-6Al-5Zr-0.5Mo-0.25Si (alloy 685). The heat treatment to hold silicon in solid solution consists of solutionizing at 1323 K for 0.5 hour under vacuum (∼10^-5 MPa), followed by water quenching, and the treatment to precipitate suicides involves subsequent aging of the solutionized and water quenched specimens at 1073 K for 24 hours. There is only marginal effect of the aging treatment on strength values; however, the ductility parameters are found to be drastically reduced. There are marked differences in the fracture behavior of the alloy in the as-quenched and the quenched and aged conditions. While the fracture surface of the unaged specimen shows characteristic dimples, there is a large number of facets on the fracture surface of the aged specimen. The facets in the central region are relatively smaller in size than those in the peripheral zone. The central facets show fluted features at higher magnifications; however, the peripheral facets are usually featureless. The faceted fracture in the aged condition is attributed to enhanced tendency for heterogeneous planar slip. The fracture characteristics correlate with the observed differences in the ductility in the two conditions.     

Effect of silicide precipitation on tensile properties and fracture of alloy Ti-6Al-5Zr-0.5Mo-0.25Si

The effect of silicon in solid solution and in the form of suicides has been studied on the tensile properties and fracture behavior of alloy Ti-6Al-5Zr-0.5Mo-0.25Si (alloy 685). The heat treatment to hold silicon in solid solution consists of solutionizing at 1323 K for 0.5 hour under vacuum (∼10^-5 MPa), followed by water quenching, and the treatment to precipitate suicides involves subsequent aging of the solutionized and water quenched specimens at 1073 K for 24 hours. There is only marginal effect of the aging treatment on strength values; however, the ductility parameters are found to be drastically reduced. There are marked differences in the fracture behavior of the alloy in the as-quenched and the quenched and aged conditions. While the fracture surface of the unaged specimen shows characteristic dimples, there is a large number of facets on the fracture surface of the aged specimen. The facets in the central region are relatively smaller in size than those in the peripheral zone. The central facets show fluted features at higher magnifications; however, the peripheral facets are usually featureless. The faceted fracture in the aged condition is attributed to enhanced tendency for heterogeneous planar slip. The fracture characteristics correlate with the observed differences in the ductility in the two conditions.     

Effect of microstructure on fracture characteristics of Ti-6Al-2Sn-2Zr-2Mo-2Cr-Si

The effects of intermetallic compounds of Ti₃Al (α ₂) and silicide separately on fracture characteristics of Ti-6Al-2Sn-4Zr-2Mo-0.1Si (Ti-62222S) alloy were investigated in this study. The alloys with only Ti₃Al and only silicide precipitated were established by aging treatments at temperatures of 913 K followed by air cooling and 1088 K followed by water quenching, respectively. X-ray diffraction analysis results showed that the volume fraction of either Ti₃Al or silicide increases with increasing aging time. Tensile properties, namely, yield stress (0.2 pct proof stress), ultimate tensile strenght, and elongation of as-received alloy are much better than those of the aged alloys. The strength of the alloy with only Ti₃Al is better than that of the alloy with only silicide, while elongation of the alloy with only silicide is better than that of the alloy with only Ti₃Al. Fracture toughness, J _IC, of the alloy with only silicide is better than that of the alloy with only Ti₃Al. The intergranular fracture appears in the alloy with only Ti₃Al. Coarsening of Widmanstätten α structure and increasing ductility of β phase during aging are considered to be effective for increasing fracture toughness.     

Formation of Fine B2/β + O Structure and Enhancement of Hardness in the Aged Ti2AlNb-Based Alloys Prepared by Spark Plasma Sintering

Ti₂AlNb-based alloys synthesized at 1223 K (950 °C) by spark plasma sintering were aged at 973 K, 1023 K, 1073 K, and 1123 K (700 °C, 750 °C, 800 °C, and 850 °C), respectively. Phase composition, microstructure, and microhardness of the aged alloys were investigated in this study. Equiaxed O grains and Widmanstätten B2/β + O laths were formed in the aged alloys, and the microhardness was improved in contrast with the spark plasma-sintered alloy without aging. The microhardness relies largely on the O-phase content, as well as the length and width of the O laths. In particular, complete Widmanstätten B2/β + O laths, with locally finely dispersed β precipitates, were obtained in the alloy aged at 1073 K (800 °C), and the alloy exhibited the best microhardness performance. Such fine structure is due to the temperature-dependent transformations O_equiaxed→O_primary + B2/β _primary, O_primary→O_secondary  + B2/β _secondary, and B2/β _primary→O.

     

Asymmetrical mechanical behavior of a precipitation hardened beta titanium alloy

Precipitation hardened single crystals of a beta (bcc) Ti-40 at. pct V + 1.0 at. pct Si alloy have been deformed in compression at 77 K and 298 K. The dependence of the yield stress upon aging time at 843 K for solution treated crystals shows two maxima which are caused by silicide precipitates. The orientation dependence of the yield stress and of the active macroscopic slip plane have been determined as a function of aging time. The solution treated as well as aged crystals exhibit an asymmetry of both the yield stress and the plane of slip, the degree of asymmetry being larger at 77 K than at 298 K. The asymmetry of slip and yielding is not affected by the presence of precipitation hardening. The results indicate that the effect of the dislocation core structure on dislocation motion is independent of the presence of precipitates.

     

Structure and properties of a near-α titanium alloy after β solution treatment and aging at 625 °

The microstructure, tensile properties, and fractographic features of a near alpha titanium alloy, IMI 829 (Ti-6.lAl-3.2Zr-3.3Sn-lNb-0.5Mo-0.32Si) have been studied after aging at 625 ° for 24 hours following solution treatment in the beta phase field at 1050 ° and cooling at various rates (furnace, air, oil, or water). Transmission electron microscopy studies revealed that aging at 625 ° for 24 hours of this alloy had led to the precipitation of only one kind of silcide with a hexagonal structure (c = 0.36 nm andα = 0.70 nm). The precipitates are ellipsoidal in shape and their size depends on the cooling rate given to the alloy after beta solution treatment. Extremely fine precipitation of Ti₃Al phase has also been observed in the furnace cooled and aged condition. There is a significant improvement in both yield and ultimate tensile strengths after aging of both the oilquenched and water-quenched specimens whereas it is minimal in the case of furnace-cooled and air-cooled specimens. Aging the alloy has also resulted in a drastic reduction in both percentage elongation and percentage reduction in area for all the conditions investigated. While the fracture surfaces of the unaged specimens showed characteristic dimples, a large number of facets appeared in the fractographs of the aged specimens. formerly with Banaras Hindu University, is with the National Metallurgical Laboratory, Jamshedpur, India.     

Kinetics and Equilibrium of Age-Induced Precipitation in Cu-4 At. Pct Ti Binary Alloy

Transformation kinetics and phase equilibrium of metastable and stable precipitates in age-hardenable Cu-4 at. pct Ti binary alloy have been investigated by monitoring the microstructural evolution during isothermal aging at temperatures between 693 K (420 °C) and 973 K (700 °C). The microstructure of the supersaturated solid solution evolves in four stages: compositional modulation due to spinodal decomposition, continuous precipitation of the needle-shaped metastable β′-Cu₄Ti with a tetragonal structure, discontinuous precipitation of cellular components containing stable β-Cu₄Ti lamellae with an orthorhombic structure, and eventually precipitation saturation at equilibrium. In specimens aged below 923 K (650 °C), the stable β-Cu₄Ti phase is produced only due to the cellular reaction, whereas it can be also directly obtained from the intergranular needle-shaped β′-Cu₄Ti precipitates in specimens aged at 973 K (700 °C). The precipitation kinetics and phase equilibrium observed for the specimens aged between 693 K (420 °C) and 973 K (700 °C) were characterized in accordance with a time–temperature–transformation (TTT) diagram and a Cu-Ti partial phase diagram, which were utilized to determine the alloy microstructure, strength, and electrical conductivity.

     

Precipitation in a Cu-30 Pct Ni-1 Pct Nb alloy

Decomposition of a Cu-30 pct Ni-1 pct Nb alloy on aging in the range of 866 K (600°C) to 1073 K (800°C) was investigated. The initial decomposition, concomitant with age hardening, occurred through the precipitation of body centered tetragonal metastable Ni₃Nb-γ” precipitates on the 100 matrix planes. Equilibrium orthorhombicβ phase formed either through a grain boundary cellular reaction at low temperature (≤973 K (700°C)) or as Widmanstaettenplatelets on the 1ll planes at higher temperatures (≥1073 K (800°C)) with the following crystallographic relationship: (0l0)_β//111_γ [100]β//[1•11]_γ. Based on the observations, a schematic transformation sequence is presented.     

High-Performance dispersion-strengthened Cu-8 Cr-4 Nb alloy

A new high-temperature-strength, high-conductivity Cu-Cr-Nb alloy with a Cr:Nb ratio of 2:1 was developed to achieve improved performance and durability. The Cu-8 Cr-4 Nb alloy studied has demonstrated remarkable thermal and microstructural stability after long exposures at temperatures up to 0.98 T_m. This stability was mainly attributed to the slow coarsening kinetics of the Cr₂Nb precipitates present in the alloy. At all temperatures, the microstructure consists of a bimodal and sometimes trimodal distribution of strengthening Cr₂Nb precipitates, depending on precipitation condition, i.e., from liquid or solid solution, and cooling rates. These precipitates remain in the same size range, i.e., large precipitates of approximately 1 μm and small precipitates less than 300 nm, and effectively pin the grain boundaries, thus retaining a fine grain size of 2.7 μm after 100 hours at 1323 K. This grain-boundary pinning and sluggish coarsening of Cr₂Nb particles explain the retention of good mechanical properties after prolonged holding at very high temperatures, e.g., twothirds of the original yield strength after aging for 100 hours at 1273 K. The main sources of strengthening are the Hall-Petch and Orowan mechanisms due mostly to small particles. The coarsening kinetics of the large precipitates are most likely governed by grain-boundary diffusion and, to a lesser extent, volume diffusion mechanisms.     

Structure-property relations in a metastable β Ti alloy containing Si

The hardness response, tensile behavior, and phase transformations occurring in a quenched and aged metastable β phase Ti-30 at. pct V-l at. pct Si alloy have been inves-tigated. Upon aging at 570°C, as-quenched samples show a broad hardness peak which is associated with the formation of rod-like, hexagonal (Ti,V)_xSi_y transition phase precipi-tates. The equilibrium silicide is observed upon aging at 570°C in the form of faceted, tetragonal particles. A loss of tensile ductility and a transition to intergranular fracture occurs after extended aging at 570°C and is related to Si segregation to the grain bound-aries. Comparing the behavior of Ti-30V to that of Ti-30V-lSi shows that the presence of Si strongly retards α-phase formation. However, a substantial age hardening re-sponse still occurs upon aging at 450°C, especially after prior cold work (the yield strength increases from 635 to 982 MPa). This hardening response is combined with a retention of a ductile, transgranular fracture even after extended aging at 450°C. Aging first at 570°C followed by aging at 450°C results in an increase in the volume fraction of α-phase formed but a subsequent decrease in ductility and hardness response upon aging at 450°C. These results are discussed in terms of the structure/property relationships which result from the influence of Si on the formation of, a) (Ti.V)_xSi_y precipitates, b) the equilibrium silicide, and c) the α-phase.     

The influence of Si on precipitation phenomena and age hardening of a beta Ti alloy

The phase transformations occurring in a quenched and aged β-phase (bcc) Ti-40 at. pct V+1 at. pct Si alloy have been investigated using transmission electron microscopy. Upon aging at 570°C, the most probable precipitation sequence is the following: bcc super-saturated solid solution»bcc zones»(Ti, V)_xSi_y (hexagonal)»(Ti, V)₃Si (tetragonal). The bcc precipitates may be considered Si-rich GP zones which are homogeneously nucleated and coherent with the matrix. The (Ti, V)_xSi_y particles are a rod-shaped transition phase aligned along the <100> matrix directions. The precipitation reaction causes two peaks in the dependence of the yield stress or hardness upon aging time. The particle diameter and interparticle spacings of the hexagonal silicides indicate that these precipitates are responsible for the second hardness peak. The bcc zones evidently cause the first hardness peak at short aging times at 570°C.     

Coercive force and microstructure in a Zr-permalloy

An alloy containing 80.0 pct Ni, 12.65 pct Fe, 6.74 pct Mo, 0.36 pct Zr, and 0.25 pct Mn by weight was cast, homogenized, and successively cold rolled into thin strips with area reductions of 0, 50, 75, and 90 pct. Annealed samples were studied by optical and electron microscopy, electron diffraction, and magnetic testing to determine the effects of cold work and annealing upon the microstructure and magnetic properties of the alloy. Cold work produced a high initial hardness together with high coercive force. Recrystallization of the cold worked structures occurred upon annealing at 600°C (873 K) and above and caused significant and parallel decreases in hardness and coercive force. The activation energy for recrystallization was found to be 80.5 kcal/g mole (337.0 kJ/g mole) for the 50, 75, and 90 pct cold worked specimens. After annealing at 600°C (873 K), a small number of spherical Ni₄Mo particles were observed, but the particles produced little change in magnetic properties apparently because of their relatively coarse size and large spacing. Beginning at 700°C (973 K) ribbon-shaped particles of a Ni₅Zr intermetallic compound also precipitated out of solid solution. Both the Ni₄Mo and Ni₅Zr precipitates were the result of a homogeneous continuous precipitation reaction within the grains. A peak in coercive force at 800°C (1073 K) is attributed to domain wall pinning associated with the fine distribution of rodlike Ni₅Zr particles. Cold working 90 pct and aging at 800°C (1073 K) was found to increase coercive force by almost 60 pct from the minimum produced by complete recrystallization. Annealing, however, decreased hysteresis and improved squareness.     

The precipitation behavior of a Zr-2.5 wt pct Nb alloy

The morphology, crystallography, and nature of precipitates in a quenched and aged Zr-2.5 wt pct Nb alloy has been studied by transmission electron microscopy. The needle-shaped matrix precipitates and equiaxed twin boundary nucleated precipitates produced by aging at 500 °C were the equilibrium Nb-rich β₂ phase. On aging at 600 °C, the matrix precipitation was a mixture of β₂ needles and coarse metastable Zr-rich β₁ particles, while only β₁ particles were found at twin boundaries. The growth direction of the needle-shaped particles, 6.6 deg to 8.2 deg from (1-100)_h, and their orientation relationship can be predicted by an invariant line strain model. The β₁ precipitates have the Burgers orientation relationship. The formation of metastable β₁ and stable β₂ particles is considered from the free energy approach of Menon, Banerjee, and Krishnan.     

Microstructural characterisation of near-α titanium alloy Ti-6Al-4Sn-4Zr-0.70Nb-0.50Mo-0.40Si

Microstructural stability in the near-α titanium alloy (alloy 834) containing Ti-6Al-4Sn-4Zr-0.70Nb-0.50Mo-0.40Si (in weight percent), in the β and(α + β) solution-treated and quenched conditions, has been investigated. The β transus for this alloy is approximately 1333 K. Solution treatment in the β phase field at 1353 K followed by quenching in water at room temperature resulted in the formation of α′ martensite platelets with high dislocation density and stacking faults. Thin films of β are found to be sandwiched between interface phases, which, in turn, are sandwiched at the interplatelet boundaries of lath martensite. The interface phase is a subject of much controversy in the literature. Solution treatment at 1303 K in the(α + β) phase field followed by quenching in water at room temperature resulted in the near-equiaxed primary α and transformed β. Both the β and(α + β) solution-treated specimens were aged in the temperature range of 873 to 973 K. While aging the —treated specimen at 973 K,(α + β)-treated specimen, even at a lower temperature of 873 K for 24 hours, caused precipitation of suicides predominantly at the interplatelet boundaries of martensite laths. Electron diffraction analysis confirmed them to be hexagonal suicide S₂ witha = 0.70₂ nm andc = 0.36₈ nm. The above difference in the precipitation could be attributed to the partitioning of a higher amount of β- stabilizing elements as well as silicide-forming elements to the transformed β in the(α + β) solution-treated condition. However, ordering of theα′ phase was observed under all of the aging conditions studied. The ordered domains were due to the longer aging times, which cause local increases in the level of theα-stabilizing elements. Formerly Research Associate, Department of Metallurgical Engineering, Baranas Hindu University.     

Study of Aging-Induced Degradation of Fracture Resistance of Alloy 617 Toward High-Temperature Applications

For the Alloy 617, the effect of aging on the fracture energy degradation has been investigated after aging for different time periods at 1023 K (750 °C). A sharp reduction in impact energy (by ~55 pct vis-à-vis the as-received material) after 1000 hours of aging, as evaluated from room-temperature Charpy impact tests, has been observed. Further aging up to 10,000 hours has led to a degradation of fracture energy up to ~78 pct. Fractographic examinations using scanning electron microscopy (SEM) have revealed a change in fracture mode from fibrous-ductile for the un-aged material to intergranular mode for the aged one. The extent of intergranular fracture increases with the increasing aging time, indicating a tendency of the material to undergo grain boundary embrittlement over long-term aging. Analysis of the transmission electron microscopy (TEM) micrographs along with selected area diffraction (SAD) patterns for the samples aged at 10,000 hours revealed finely dispersed γ′ precipitates of size 30 to 40 nm, rich in Al and Ti, along with extensive precipitation of M₂₃C₆ at the grain boundaries. In addition, the presence of Ni₃Si of size in the range of 110 to 120 nm also has been noticed. The extensive precipitation of M₂₃C₆ at the grain boundaries have been considered as a major reason for aging-induced embrittlement of this material.     

Phase equilibria and transformations in a Ti-Zr-Si system

The phase equilibria in the titanium-zirconium rich region of the ternary Ti-Zr-Si system have been studied in the temperature range from 1473 to 1323 K, together with microstructures pres-ent in the as-cast state. DTA, microscopy, X-ray diffraction (XRD), and chemical analysis by X-ray energy-dispersive spectroscopy have been employed. Whereas Ti₅Si₃ nucleates hetero-geneously and grows rapidly in titanium matrices, Ti₃Si exhibits very slow precipitation kinetics. It also is displaced by (Ti, Zr)₅Si₃ and a ternary silicide in ternary and more complex systems, explaining its absence in commercial alloys. Zirconium exhibits substantial solid solubility in Ti₅Si₃in ternary alloys, while Ti exhibits only limited solubility in Zr₂Si, Zr₃Si, and Zr₅Si₃. Additionally, a new silicide of general formula (Ti, Zr)₂Si is formed in ternary alloys with a Ti:Zr ratio ranging from 2.26 to 0.68. Isothermal sections for the Ti-Zr-Si system are presented for temperatures of 1473 and 1323 K.     

Microstructural and analytical characterization of TiNχ precipitation in N+ implanted equiatomic NiTi alloys

In order to explain the improved tribological properties obtained on NiTi alloys after N⁺ implantation, complementary surface sensitive techniques (TEM, SIMS and XPS) are used to characterize an initially martensitic NiTi alloy. When the nitrogen ions are implanted at 293 K, the affected zone is fully amorphous with embedded fine disoriented TiNx (x ≈ 0.8) precipitates. At 473 K the implanted region consists of an amorphized layer and an underneath crystalline austenitic layer both containing TiN_χ precipitates. These precipitates are in epitaxy with the austenitic matrix. After implantations at 573 K and above, the implanted zone is fully austenitic with epitaxial TiNx precipitates. Post implantation annealings under 823 K do not sensibly affect the implanted element distribution but favor the evolution of TiN_χ precipitates towards the stoichiometric compound TiN. Beyond 823 K the amorphous layer crystallizes.     

Effect of Aging on Microstructure and Shape Memory Properties of a Ni-48Ti-25Pd (At. Pct) Alloy

The microstructure and properties of a precipitation-hardenable Ni-48Ti-25Pd (at. pct) shape memory alloy have been investigated as a function of various aging conditions. Both the hardness and martensitic transformation temperatures increased with increasing aging time up to 100 hours at 673 K (400 °C), while no discernable differences were observed after heat treatment at 823 K (550 °C), except for a slight decrease in hardness. For aging at 673 K (400 °C), these effects were attributed to the formation of nano-scale precipitates, while precipitation was absent in the 823 K (550 °C) heat-treated specimens. The precipitation-strengthened alloy exhibited stable pseudoelastic behavior and load-biased-shape memory response with little or no residual strains. The precipitates had a monoclinic base-centered structure, which is the same structure as the P-phase recently reported in Ni(Pt)-rich NiTiPt alloys. 3D atom probe analysis revealed that the precipitates were slightly enriched in Ni and deficient in Pd and Ti as compared with the bulk alloy. The increase in martensitic transformation temperatures and the superior dimensional stability during shape memory and pseudoelastic testing are attributed to the fine precipitate phase and its effect on matrix chemistry, local stress state because of the coherent interface, and the ability to effectively strengthen the alloy against slip.     

Microstructural study of the titanium alloy Ti-15Mo-2.7Nb-3Al-0.2Si (TIMETAL 21S)

A relatively new titanium alloy, TIMETAL 21S (Ti-15Mo-2.7Nb-3Al-0.2Si-0.15O (in wt pct)), is a potential matrix material for advanced titanium matrix composites for elevated temperature use. In order to develop a perspective on the microstructural stability of this alloy, the influence of several commonly used heat treatments on the microstructure of TIMETAL 21S was studied using optical and transmission electron microscopy (TEM). Depending on the specific thermal treatment, a number of phases, includingα,ω- type, and silicide, can form in this alloy. It was found that both recrystallized and nonrecrystallized areas could be present in the microstructure of an annealed bulk alloy, but the microstructure of annealed sheet alloy was fully recrystallized. The mixed structure of the bulk alloy, developed as a result of inhomogeneous deformation, could not be removed by heat treatment alone at 900 °C. Athermalω-type phase formed in this alloy upon quenching from the solution treatment temperature (900 °C). Silicide precipitates were also found in the quenched sample. Thermal analysis was used to determine theβ transus and silicide solvus as close to 815 °C and 1025 °C, respectively. In solution-treated and quenched samples, a high-temperature aging at 600 °C resulted in the precipitation ofα phase. The precipitation reaction was slower in the recrystallized regions compared to the nonrecrystallized regions. During low-temperature aging (350 °C), the ellipsoidalω-type phase persisted in the recrystallized areas even after 100 hours, whereas a high density ofα precipitates developed in the nonrecrystallized areas within only 3 hours. The observed behavior in precipitation may be related to the influence of substructure in the nonrecrystallized areas, providing for an enhanced kinetics during aging. Theα precipitates (formed during continuous cooling from the solution treatment temperature, low-temperature aging, and high-temperature aging) always obeyed the Burgers orientation relationship. With respect to the microstructure, TIMETAL 21S is similar to other solute-lean, metastableβ titanium alloys.