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Morphology evolution and orientation characteristics of precipitate of ultra-high strength titanium alloy

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The control of the post-forging cooling rate has been a key issue in the industrial production process of titanium alloys. We investigated texture evolution and variant selection (VS) during β → α transformation through high-temperature compression experiments followed by quantitative control of varying cooling rates. Results show that post-forging cooling rates affect β grains, α variants, and α / β textures. The α precipitation inhibits motions of β static recrystallization (βSRX) grain boundaries and thus leads to grain refining from 0.1°C/s to 0.05°C/s. Further analysis reveals that lamellae grain boundary widmanstatten α (αWGB) keeps growing rapidly within β-grain in an interface instability manner at 0.1-0.05°C/s. Most of α-phase with 50°-60°/<-12-10> is preferentially precipitated at β-medium angle GBs between 30°-45° and strictly follows BOR with the side of of adjacent β-grain with the same or similar {110} or {111}. Moreover, the texture type transforms gradually from RGoss {110} <1-10> to Brass {110} <1-12> from 25°C/s to 1°C/s. βSRX grains exhibit (102) [-201] texture, while the corresponding α has textures of <0001>//Z and <11-20>//Y from 1°C/s to 0.05°C/s. Our findings lay a profound theoretical foundation in microstructure evolution of near-β titanium alloy for industrial production.
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Abstract In titanium alloys, variant selection (VS) of grain boundary α (GBα) at prior β grain boundaries (GBs) during α precipitation has a significant influence on the subsequent transformation pathway and transformation texture development of the α phase, and thus on the final mechanical properties. In this paper, we assess systematically the applicability of all current empirical rules for VS of GBα at prior β GBs using experimental characterization of GB misorientation, boundary plane inclination, and orientation relationships between the GBα and adjacent β grains in Ti-5553. We find that all these VS rules may be violated for a given β grain boundary. Based on the experimental observations, the frequencies of each of these empirical rules being either violated or followed have been assessed, and from this assessment, we analyze theoretically whether the arguments underlying each of these rules are physically sound and why rules are violated, and then discuss when a sound prediction may be made using these empirical VS rules.
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Through three-dimensional phase-field simulations, dislocations are found to exert significant influences on variant selection and subsequent development of transformation texture during α precipitation in α/β titanium alloys. It is found that, for the dislocation configurations considered in the current study, the elastic interaction between α precipitates and dislocations dominates variant selection during the nucleation stage, whereas the habit plane orientations of α precipitates relative to the dislocation lines play an important role in variant selection during the growth stage. In general, edge dislocations exhibit a much more prominent effect than screw dislocations. Various morphological patterns of α precipitates formed by heterogeneous nucleation around dislocations of different configurations are revealed, including clusters of multiple variants and a special “tent” structure that appears as a pyramid with each of its faces composed of a particular α variant. Two types of frequently observed clusters of α variants are found to share either a common <1 1 1>β axis or a common {1 1 0}β plane. The primary tent structure is able to induce the nucleation of secondary α through autocatalysis, reducing the degree of variant selection. The effect of undercooling on variant selection is also investigated in the context of competition between the chemical driving force for α precipitation and the elastic interaction between dislocation and precipitate.
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During β -processing of α /β and β titanium alloys, variant selection (VS) of grain boundary α (GBα) is one of the key factors in determining the final transformation texture and mechanical properties. It has been observed frequently that GBα prefers its 〈0 0 0 1〉α pole to be parallel to a common 〈1 1 0〉β pole of the two adjacent β grains and results in a micro-textured region across the grain boundary (GB) and, as a consequence, slip transmission may take place more easily across that GB. In order to investigate how such a special prior β GB contributes to VS of GBα, we develop a crystallographic model based on the Burgers orientation relationship (BOR) between GBα and one of the two β grains. The model predicts all possible special β grain boundaries at which GBα is able to maintain BOR with both β grains. A new measure for VS of GBα, (βΔJβBOR)(βΔJβBOR), i.e., a measure of the deviation of the actual OR between the GBα and the non-Burgers grain from the BOR, is proposed. For the particular alloy chosen for experimental observations, Ti-5553, it is found that when the misorientation angle θmθm of (βΔJβBOR)(βΔJβBOR) (instead of the closeness between two closet {110}β poles between two β grains widely used in literature) is less than 15°15°, misorientation between the two β grains dominates the VS of GBα and, in particular, the variant with minimum θmθm is always selected for GBα. A possible effect due to grain boundary plane inclination on VS is also discussed.
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Evolution of grain boundary α (GB α) in a α + β titanium alloy had been examined by morphology and crystallographic orientation analysis. The results indicate that GB α only retains a Burgers orientation relationship (BOR) with one of the adjacent β grains in most of the prior β/β boundaries. The colony α (single crystallographic variant of parallel α plates) tends to evolve in the adjacent β grain that maintains BOR with GB α, whereas the dendritic α (small protuberances of GB α) tends to grow in the other adjacent β grain that does not maintain BOR with GB α. Additionally, two α colonies developing into two adjacent β grains from GB α keep the same crystallographic orientation as that of GB α when GB α maintain a near BOR with both adjacent β grains in a special prior β/β boundary (60°/〈1 1 0〉). These observations are understood from the perspective of minimum interfacial energy and strain energy.
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In the present work, we investigated the texture evolution as well as the role of the β texture intensity on the α-variant selection and microstructure morphology during the α→β→α phase transformation in Ti60 alloy. Different microstructures and textures were obtained through forging the Ti60 bars into diameters of 45 mm denoted as D45 and 30 mm as D30. Subsequently, small samples with the same size cut from both bars were heat-treated above the β transus followed by furnace cooling and air cooling. We found that the β texture intensity, cooling rate, and variant selection affect both the texture intensity and microstructure morphology of the transformed α phase. The high temperature β phase exhibits stronger (110) parallel to axial direction fiber texture in the β annealed D30 bar than that for the D45 bar. A basketweave microstructure was found in the β annealed D45 bar after air cooling whereas a coarse α colonies populated by fine α lamellae formed in the D30 bar. For furnace cooled samples, the α texture is stronger than that in the air cooled sample in D45 bar whereas the intensities of the textures are very similar to air cooled sample in the D30 bar. The influence of the β texture intensity and variant selection on the α texture evolution were studied by comparing the four experimental results and simulation data. The effect of α variant number in a β grain on α texture intensity, base on variant selection, and the effects of β texture intensity on microstructure morphology are discussed.
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The elastic interactions among α precipitates and their effects on variant selection are investigated. The stress field around a semi-coherent α lath is first calculated using phase field microelasticity theory and then the precipitation process of β→α+β in Ti-6Al-4V is simulated using a 3-D phase field model. The orientations of secondary α variants induced by a primary (pre-existing) α variant obtained from the phase field simulations are consistent with those of variants within commonly observed α clusters in experiments. The formation of α/α orientation relationship of the [112¯0]α/60°-type, [10‾553]α/63.26°-type and [0001]α/10.53°-type frequently observed in experiments could be a direct consequence of autocatalysis during nucleation and growth of α variants. Moreover, the competition among α variants nucleated simultaneously around a primary α lath for limited number of preferred nucleation sites also results in the selection of variants possessing specific crystallographic orientation with respect to the primary α precipitates.
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The effects of cooling rate following the β or α/β heat treatment on microstructure and phase transformation are investigated for BT25y alloy. For this purpose, BT25y alloy is soaked at 1000 °C, 980 °C, 960 °C, 940 °C or 920 °C for 10 min, and then control cooled at rate of either 0.15 °C/s, 1.5 °C/s, 15 °C/s, 45 °C/s, 90 °C/s or 150 °C/s to room temperature. Microstructure observations indicate that the microstructure of BT25y alloy is significantly influenced by the cooling rate. When material is cooled from the β phase field at the lower rate, the αGB and αWGB phases are precipitated, and this transformation process can be divided into the four stages: (a) the formation of αGB, (b) the connection of adjacent αGB, (c) the precipitation of αWGB, (d) the growth of αWGB. However, the increasing of the cooling rate will greatly restrain the precipitations of αGB and αWGB phases. In this case, the acicular martensite α′ is precipitated inside β grain. The primary equiaxed-α is retained when material is cooled down from the α/β phase field. The content and size of equiaxed-α decrease with the increasing of solution temperature, but is independent on the cooling rate. At the lower cooling rate, the lamellar α is precipitated and its thickness increases with the increasing of solution temperature. But the increasing cooling rate will weaken the precipitation capacity of the lamellar α. Instead, the martensite α′ phase is precipitated and gradually takes the place of the lamellar α with the increase of cooling rate. In conclusion, whether material cools down from β single phase field or α/β two-phase field, a phase transformation law is summarized for BT25y alloy. The lamellar α is the only precipitated phase when the cooling rate ≤15 °C/s. The precipitated phase consists of the lamellar α and martensite α′ phase when the cooling rate is 15 °C/s ∼90 °C/s. The only martensite α′ phase is precipitated when the cooling rate ≥90 °C/s.
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Morphology and variant selection (VS) of grain boundary (GB) allotriomorphs and Widmanstätten side-plates of α phase in an α/β titanium alloy, Ti-6Al-4V (wt%), are investigated using a three-dimensional phase field model. The structures of low-angle GBs (misorientation θm ≤ 10°) are modeled as discrete dislocation networks using Frank-Bilby theory. It is shown that α allotriomorphs and side-plates compete with each other during precipitation and the final morphology and selected α variants exhibit a strong correlation with the GB dislocation structures. While the side-plate morphology is more preferred by a symmetrical tilt GB with θm ∼ 10°, it can also be induced by a pure twist GB with θm ≤ 5°. Quantitative analysis indicates that precipitate morphology and VS are determined by the interplay among (i) elastic interaction between a nucleating α precipitate and the GB dislocation networks, (ii) growth anisotropy determined by the relative inclination of the habit plane with respect to the GB dislocations, (iii) density of nucleation sites for the same variant and coalescence during growth, and (iv) spatial confinement from simultaneously nucleated neighboring α variants of dissimilar types.
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The intergranular lattice strains in the near-β titanium alloy Ti-β21S have been measured in the longitudinal and transverse directions during tensile loading using neutron diffraction. The obtained results have been modelled and explained using a two-phase elasto-plastic self-consistent model. We first identified the best set of the main model parameters (single crystal elastic constants, critical resolved shear stresses) and investigated the influence of these parameters on the behaviour of both the polycrystal and the diffracting volume. Good agreement between the experimental results and those predicted by the model was found for the macroscopic stress-strain dependencies and lattice strain developments of Ti-β21S.
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The influence of transformation temperature on microtexture development associated with α precipitation at β/β grain boundaries (GB) in the near-β Ti17 alloy was studied using electron backscatter diffraction and considering isothermal treatments. For the alloy studied and the temperature range considered, decreasing the transformation temperature decreased the local microtexture strength within each prior β grain because of a larger number of αWGB colonies (standing for α Widmanstätten GB) formed per β grain, each colony increasing by one the number of α orientations inside each prior β grain. This larger number of αWGB colonies was a consequence of faster formation along β/β GB of their precursors, the allotriomorphic αGB grains (standing for α-GB) at lower transformation temperatures, as evidenced by detailed examination of the first stages of αGB formation. αGB crystallographic orientations frequently followed a variant selection (VS) criterion based on the alignment of (0 1 1)β//(0 0 0 1)αGB//(0 1 1)β. From a statistically relevant number of observations, VS was found to be more frequent at a lower transformation duration and a lower temperature, but the effect was not significant enough to influence the final α microtexture, considered at the scale of one prior β grain. αGB grains that followed the VS criterion emitted two αWGB colonies on either side of the β/β GB more frequently than those with no particular orientation.
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The mechanism of nucleation and growth of α-lamellae when a TA15 Ti alloy with an equiaxed structure is cooled from an α + β phase field were studied by end quenching experiments and thermal simulation tests using a Gleeble-3500. The results showed that for the Ti alloy TA15 the nucleation and growth of α-lamellae involved four steps, including nucleation of αGB, growth of αGB, nucleation of αWGB, and growth of αWGB. Widmanstätten α, αWGB, grew faster than grain boundary α, αGB, and equiaxed α in common cases. It was found for the first time that the mode of nucleation of αWGB for alloy TA15 was interface instability, i.e. αWGB nucleated through surface instability and the protuberance of αGB and equiaxed α, and the αWGB nucleus did not have an independent and complete surface. A new model of the nucleation of αWGB and phase transformation is proposed. The growth of αWGB in the TA15 alloy started from a small protuberance and spread into a β grain with a sectorial morphology, to become lamellar instead of spiculate or oblate cuboid in shape. The nucleation rate of αWGB determined the thickness of αWG, with, to some extent, an inverse relation between the nucleation rate and thickness of αWGB.
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The crystallography of alpha(hcp) precipitates formed on the beta(bcc) matrix grain boundaries has been studied with transmission electron microscopy (TEM) in a Ti-15V-3Cr-3Sn-3Al alloy. The alpha precipitates have a near-Burgers orientation relationship with respect to at least one of the adjacent beta grains. Among the possible 12 variants in this orientation relationship, the variant that [11•20]alpha is parallel to the beta closest to the grain boundary plane tends to be preferred by the alpha precipitates. Additionally, further variant selections are made so as to minimize the deviation of orientation relationship with respect to the ``opposite`` beta grain from the Burgers one. Such rules in variant selection often result in the formation of precipitates with a single variant at a planar grain boundary. Prior small deformation of beta matrix changes the variant of alpha precipitates at the deformed portion of grain boundary. It is considered that the stress field of dislocations in the slip bands intersecting with the boundary strongly affects the variants of alpha precipitates. Discussion of these results is based upon a classical nucleation theory.
Article
In the present study, the texture evolution and the role of β grain growth on variant selection during β→α phase transformation have been investigated in Ti-6Al-4V with and without 0.4wt% yttrium addition. The aim of adding yttrium was to control α grain growth above the β transus by pinning grain boundaries with yttria. Both materials were first thermomechanically processed to generate similar starting microstructures and crystallographic textures. Subsequently, both materials were solution heat treated above the β transus followed by slow cooling to promote growth of the α lath structure from grain boundary α. Additional interrupted slow cooling experiments were carried out to identify the α lamellae that nucleate first from β grain boundaries. Detailed EBSD analysis was carried out and it was found that the β heat treatment did not generate new texture components although the intensities of the individual components changed dramatically depending on the alloy/β grain size. Variant selection was assessed by comparing measured α texture components with predicted α texture components based on the high temperature β texture assuming equal variant selection. It was found that with increasing β grain size variant selection intensified favouring the {φ1, Φ, φ2} {90°, 30°, 0°} texture component. Interrupted cooling experiments revealed that α nucleates first on β grain boundaries that are formed by two β grains having a common (110) normal and that these α lamellae display almost exclusively a {φ1, Φ, φ2} {90°, 30°, 0°} orientation. Consequently, the dominance of this variant with increasing β grain size can be related to the relative free growth of this particular α texture component into an “empty” β grain.
Article
The microtexture of secondary α plates in Ti–4.5Fe–6.8Mo–1.5Al has been investigated by electron backscatter diffraction (EBSD) to obtain more insight in the nucleation and variant selection of these α plates. A statistical analysis of the EBSD data shows that for most β grain boundaries the variant selection of the α plates is in agreement with a commonly used variant selection criterion yielding that the α-{0001} pole is nearly parallel to the closest β-{110} poles of the two adjacent β grains. For a small angle between the β-{110} poles nucleation is predominantly observed at both sides of the grain boundary, while with increasing angle some β grain boundaries exhibit nucleation of α plates at only one side. In the β grain interior many so-called Type 2 α–α grain boundaries are observed which are thought to originate from autocatalytic nucleation when a new α plate is formed at an existing α–β interface.
Article
The present study has examined for α/β-Ti alloys the relationship between the morphology and crystallography of Widmanstätten plates of α-Ti in colonies within a prior grain of β-Ti. Thus, optical metallography, scanning electron microscopy and transmission electron microscopy have been used to characterize the morphological features of the microstructure, whereas orientation-imaging microscopy (OM) and transmission electron microscopy (TEM) have been employed to reveal crystallographic information. It has been discovered that within a prior β-Ti grain, although the growth direction of the Widmanstätten plates in given colonies may differ by large angles from α-plates in other colonies, they may exhibit very close crystallographic relationships. For example, inclined α-plates may share common basal planes and be related by a rotation of ~10.5° about the c-axis of the crystals. This phenomenon has been interpreted on the basis of variant selection of the Burgers orientation relationship commonly adopted between the α and β phases in these alloys. Similar relationships have been observed in α-colonies growing either side of a given prior β grain boundary. These latter observations have been used to draw conclusions concerning the precipitation of α on prior β grain boundaries.
Article
The role of starting texture in variant selection has been studied during α → β → α transformation in Ti–6Al–4V. By hot rolling at different temperatures followed by recrystallization, material with either a strong basal texture or a strong transverse texture was generated. Subsequently, both conditions were heat-treated above the β transus followed by slow cooling. The degree of variant selection was assessed by comparing the strength of the measured and predicted α texture from high temperature β texture, assuming equal occurrence of all possible variants during β → α transformation. It was found that, even though the material rolled originally at 800 °C displayed a stronger α texture after β heat treatment, it was the material rolled originally at 950 °C that showed greater variant selection. The variant selection mechanism is discussed in terms of the generated β texture and common 〈1 1 0〉 poles in neighbouring β grains selecting a similar α variant on both sides of the prior β grain boundary. Predictions of possible 〈1 1 0〉 pole misorientation distributions for the two investigated β textures showed that the combination of texture components generated during rolling Ti–6Al–4V at 950 °C increases the likelihood of having β grain pairs with closely aligned (1 1 0) planes compared to rolling at 800 °C. Therefore, it can be proposed that avoiding the generation of certain combinations of β texture components during thermomechanical processing has the potential for reducing variant selection during subsequent β heat treatment.
Article
The evolution of texture in a cold rolled Ti–5Ta–1.8Nb alloy sheet, during the α → β → α transformation has been studied using EBSD and XRD techniques, for different cooling rates. The sheet exhibited a basal plane type texture upon cold rolling, and a sharp ‘{1 1 −2 0}||rolling plane’ transformation texture was inherited after the heat treatment. The microtexture analysis of the lamellar α/β structure, suggested that this transformation texture arises from the {1 1 1}〈1 1 0〉 type of high temperature β texture, obeying the Burgers orientation relationship. The strength of the transformation texture was found to sharply increase with decrease in cooling rates, denoting variant selection. Two types of parent β orientations with [1 1 0] parallel to either rolling directions are possible, and among their α product variants, 3 of them are common, and can be preferentially formed at the prior-β grain boundaries. The role of grain boundary-α in influencing variant selection and the transformation texture for different cooling rates is described in this paper.
Article
The solid-state β→β + α transformation in titanium alloys leads to complex microstructures with feature spanning across a range of length scales. In order to develop a better understanding of the microstructural evolution process, a detailed characterization of the crystallography of α laths formed from the β phase in a candidate α/β Ti alloy, Timetal 550, has been carried out. Specifically, the influence of the orientation relationship (OR) between the grain boundary α (GB α) and the adjacent β grains on the microstructural evolution has been investigated in this alloy employing orientation imaging microscopy (OIM) studies in a high-resolution SEM. The results indicate that the colony microstructure (clustering of α laths belonging to the same variant) tends to develop in the β grain that exhibits the Burgers OR with the GB α allotriomorph, whereas the basketweave microstructure (clustering of multiple variants) develops in the adjacent β grain. Additionally, the multiple variants of α laths forming the basketweave microstructure appear to be related by certain selection criteria.
Article
The phase transformations of Ti-5Al-2Sn-4Zr-4Mo-2Cr-1Fe (β-CEZ) have been studied during continuous cooling after β-solution treatment. For this purpose, electrical resistivity measurements and metallographical examinations have been carried out, and the continuous cooling transformation (CCT) diagram of β-CEZ alloy has been plotted. The different kinds of β-phase decomposition schemes in β-CEZ alloy during continuous cooling have been investigated in detail. Two main morphological features of the α/β structure are involved, depending on the cooling rate: the basket-weave and the colony structures are observed for high and low cooling rates, respectively. For the intermediate cooling rates, the two morphologies coexist. Finally, a generalized scheme of the β → β + α transformation sequences during continuous cooling is presented.
Article
In heterogeneous nucleation on lattice defects in the matrix during diffusional phase transformation and precipitation reactions, the variant of product phase with the specific orientation relationship is strongly selected by the nature of the defects. For dislocations, effective accommodation of the transformation strain by the strain field of dislocations occurs, leading to the variant selection in which the direction of the maximum misfit is nearly parallel to the Burgers vector of the dislocations. For high-angle grain boundaries and subgrain boundaries, precipitates tend to select the variant with a low-energy interface (often the parallel close packed planes) inclined at the smallest angle to the grain boundary plane. On the other hand, precipitates that nucleate on the incoherent inclusions embedded in the matrix do not hold any specific orientation relationship with respect to the matrix. It is important to produce many variants locally for the effective refinement of microstructures that improves the mechanical properties of steel and titanium alloys.
Article
The variant selection occurring in the β-α phase transformation of Ti-64 material after rolling in the β-field was investigated by using texture transformation modelings. In a previous work published in this journal, we observed that the variant selection was very sensitive to the deformation degree imposed at high temperature prior to the transformation. In this contribution, we assumed that crystal defects formed during glides on the 110〈111〉 and 112〈111〉 β slip systems could favor the growth of plates corresponding to specific variants. Moreover, a detailed study of the β → α phase transformation suggested a link between the selected variants and the slip systems activated at high temperature. Therefore, we developed a texture transformation modeling, assuming that a variant is selected if its corresponding slip system was sufficiently activated in the last step of the hot deformation. The activity of the slip systems was evaluated by a rate sensitive Taylor model. The modeling was applied to a Ti-64 material 75% rolled at 1050°C and the simulated texture was in good agreement with the experimental one.
Article
A three-dimensional (3D) continuum stochastic field kinetic model of martensitic transformations which explicitly takes into account the transformation-induced elastic strain is developed. The model is able to predict the major structural characteristics of martensite during the entire transformation including nucleation, growth and eventually formation of internally twinned plates which are in thermoelastic equilibrium with the parent phase. No a priori constraints are made on the possible configurations and sequences of structural patterns formed by orientation variants of the martensite. 3D computer simulations are performed for a generic cubic → tetragonal martensitic transformation in a prototype crystal which is elastically isotropic and elastically homogeneous. The simulations predict that (i) nucleation of martensite in a perfect crystal occurs collectively to accommodate the coherency strain, e.g. the critical nuclei are formed by two internally twinned orientation variants; (ii) the ultimate structure consists of plate-like martensite and retaining parent phase. The martensitic plates consist of twin-related platelets of two orientation variants and the habits of the plates meet the invariant plane requirement. These simulation results are in good agreement with experimental observations.
Article
This study presents in situ observations of the hcp (α) to bcc (β) phase transformation in commercially pure titanium at 882 °C using SEM imaging concurrent with crystal orientation determination using EBSD. Direct observations of the onset of the phase transformation are presented showing the early stages of the growth of β plates within α grains and allotriomorphic β along α–α grain boundaries. Intragranular β plates have a Burgers orientation relationship (OR) with the parent α grain and are lenticular in shape. These plates also have a tent surface relief and surface-traces consistent with habit planes predicted by the phenomenological theory of martensitic crystallography for pure titanium. These features suggest a military component to the growth mechanism. The β allotriomorphs have a Burgers OR with one of the α grains abutting at the boundary, but do not have surface relief characteristic of a military transformation. These are likely to grow by a civilian mechanism. The final stage of the transformation is a process of competitive growth of the two β forms, with the allotriomorphic β dominating by virtue of its faster moving α–β interfaces. Grain growth in the β stability field is more than an order of magnitude faster than that in the α field at temperatures near the phase transformation.