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钛合金热处理微观组织演变机理

Heat treatment for titanium alloys mainly includes annealing, solid solution and aging. Annealing is to eliminate or reduce internal stress, improve plasticity and structural stability, and obtain better comprehensive mechanical properties. The α/β transformation will cause distortion of the crystal lattice, and a slight increase in volume can be observed macroscopically when the α/β phase transition temperature is passed during the cooling process of titanium. The performance of titanium alloy is directly affected by its microstructure, which is described by the size distribution and arrangement of α phase and β phase. The titanium alloy that obtains sufficient deformation energy through deformation is solid-solution treated at the temperature of the two-phase region to obtain an equiaxed recrystallized structure. The extension of the annealing time will cause the structure to grow and coarsen. The volume fraction of the primary α phase is mainly determined by the solution treatment temperature. When the solid solution temperature is slightly lower than the β phase transition temperature, the titanium alloy can obtain a two-state microstructure, which is characterized by equiaxed α distribution on the layered (α+β) matrix.

针对钛合金热处理主要包括退火、固溶和时效。退火是为了消除或者减少内应力、提高塑性和组织稳定性,以获得较好的综合力学性能α/β转变会使得晶格产生畸变,钛冷却过程中通过α/β相转变温度时可从宏观上观察到体积轻微增加。钛合金的性能直接受其显微组织的影响,显微组织通过α相和β相的尺寸分布及其排列方式来描述。通过变形获得足够的变形能的钛合金在两相区温度内进行固溶处理,能够得到等轴状再结晶组织。退火时间的延长会导致组织长大粗化。初生α相的体积分数主要由固溶处理温度决定。当固溶温度在稍低于β相转变温度时,钛合金能够获得双态显微组织,其特点是等轴状α分布在层状(α+β)基体上。

钛合金热处理机理

文献1(2020):The Microstructural Difference and Its Influence on the Ballistic Impact Behavior of a Near β-Type Ti5.1Al2.5Cr0.5Fe4.5Mo1.1Sn1.8Zr2.9Zn Titanium Alloy(近β型Ti5.1Al2.5Cr0.5Fe4.5Mo1.1Sn1.8Zr2.9Zn钛合金的微观组织差异及其对弹道冲击性能的影响。)

A transmission electron micrograph of prior β grains in the hot-rolled and titanium alloys is shown in Figure 5a. It can be seen that the dislocation tangles occur in most regions of the hot-rolled alloy. Furthermore, these tangles, dislocation network, and dislocation cells (see regions indicated by arrows) form in the α/β interface and lead to a substantial increase in the dislocation concentration. However, in contrast to the hot-rolled alloy, dislocation tangles occur in only a few regions in the heat-treated titanium alloy as shown in Figure 5b, indicating that the dislocation density decreases significantly after the treatment.

Figure 5. Transmission electron micrographs of the (a) hot-rolled specimen and (b) heat-treated specimen.

The cracks formed in the hot-rolled and heat-treated titanium alloy plates after ballistic testing are quantitatively characterized via the industrial CT method as shown in Figure 10. The three-dimensional distributions of the main cracks in both titanium alloys as shown in Figure 10a,c reveal that the crack volume of the hot-rolled alloy is considerably larger than that of the heat-treated alloy (2.55 mm3 and 0.06 mm3 respectively). Magnified views of the main cracks are shown in Figure 10b,d. For the hot-rolled alloy, the maximum crack width (0.22–0.24 mm) occurs in the central region of the bulge. The crack width decreases gradually with the increase of the distance from the central region of bulge, and it varies mainly from 0.10 to 0.17 mm. However, the main crack of the heat-treated titanium alloy undergoes incomplete propagation, and the maximum crack width (0.08 mm) occurs in several separated points. In addition, the crack width ranges mainly from 0.03 to 0.06 mm, which is significantly smaller than that of the hot-rolled alloy.

Figure 10. Three-dimensional distribution of cracks, as determined via industrial computer tomography (CT): (a) crack distribution in the hot-rolled titanium alloy plate, (b) magnified view of the crack in (a), (c) crack distribution in the heat-treated titanium alloy plate, and (d) magnified view of the crack in (c).

The failure mechanism at adiabatic shear bands of titanium alloy: High-precision survey using precession electron diffraction and geometrically necessary dislocation density calculation

Materials Science & Engineering A 746 (2019) 322–331

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文献2(2019):The failure mechanism at adiabatic shear bands of titanium alloy: High-precision survey using precession electron diffraction and geometrically necessary dislocation density calculation (钛合金绝热剪切带的失效机理:采用旋进电子衍射和几何必须位错密度计算的高精度测量)

A comparison of the textures characterizing each ROI reveals no preferred crystal orientation in the sample prior to shear localization (stage 1). Moreover, during the early stage of shear localization (stage 2), the <0001>directions are, in general, perpendicular to the compression direction in ASB and the surrounding region. Subsequently, when the temperature and amount of deformation are increased, several grain orientations arise in ASB, owing to the formation of many new grains with orientations differing from those of their respective parents (stage 3). The number of grain orientations increases with increasing intensity of the recrystallization (e.g., in the region near the initiation point of microcracks).

Fig.8. Schematic showing the evolution of the crystal orientations. the morphology and corresponding GND density distribution of the α phase in ROI-1, ROI-2, and ROI-3

The distribution of dislocation cells is non-uniform and the GND density of the α phase in ASB is relatively high, especially in the area to be fractured. In fact, the corresponding TEM morphology near several red (i.e., high GND density) regions in ROI-2) reveal the regular arrangement of discontinuous tiny white "voids" along the crack extension line. Compared with that of ROI-2, the GND density associated with the group of ultrafine equiaxed recrystallized grains is low, whereas the adjacent high GND density region consists of many substructures. The positions of this combination of low GND density recrystallized grains and adjacent high GND density regions is basically consistent with that of the aforementioned primary microcracks in the main crack extension line.

The failure mechanism at adiabatic shear bands of titanium alloy: High-precision survey using precession electron diffraction and geometrically necessary dislocation density calculation

Materials Science & Engineering A 746 (2019) 322–331

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文献3(2019):Dynamic compression-induced twins and martensite and their combined effects on the adiabatic shear behavior in a Ti-8.5Cr-1.5Sn alloy(动态压缩诱导孪晶和马氏体及其对Ti-8.5Cr-1.5Sn合金绝热剪切行为的综合影响)

TEM observations of the alloy at strain rate of 1000/s and 1500/s after dynamic compression are also conducted. At strain rate of 1000/s (Fig. 8(a)), the boundary of martensite and the matrix, as well as dislocation accumulation near the boundary can be clearly seen. As strain rate increases to 1500/s (Fig. 8(b)), martensite has lost their original shape, and become fragmented due to severe deformation. The results showed that no ASB is observed at strain rate of 1000/s and 1500/s, and no dynamic recrystallization occurred.

Fig.8. TEM micrographs of the alloy at different strain rates: (a)1000/s; (b) 1500/s.

Fig. 9 ① and ② show SEM images of the areas adjacent to the ASBs in the alloy, while Fig. 9 ③and ④ show regions that are relatively far from the ASBs. Many twins and a large amount of martensite occur in the alloy, but the number of these structures is significantly lower near the ASBs. During ASB initiation and formation, however, the twins and martensite in the vicinity of the ASBs are refined, owing to dislocation motion and dynamic recrystallization, which will absorb energy to some extent. Fig. 9 ① and ③ reveal the bifurcation of ASBs during the dynamic loading process. In fact, the local stress at these locations and the structural fluctuation increase, owing to the twins and martensite in the alloy, and ASB expansion is hindered by ASB interaction with these locations. The expansion is also hindered by the twins and martensite perpendicular to the shear direction, resulting in a bifurcation of the ASBs.

Fig.9. SEM images showing four typical regions of the alloy at a strain rate of 2000/s: ① and ③ show the areas adjacent to the ASBs; ② and ④ show the regions far from the ASBs.

Dynamic compression-induced twins and martensite and their combined effects on the adiabatic shear behavior in a Ti-8.5Cr-1.5Sn alloy

Materials Science & Engineering A 759 (2019) 203–209

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文献4(2017):Microstructural characterization of an α+β type Ti-5.5Mo-7.2Al-4.5Zr-2.6Sn-2.1Cr alloy during recrystallization annealing(再结晶退火过程中α+β型Ti-5.5Mo-7.2Al-4.5Zr-2.6Sn-2.1Cr合金的组织特征)

As the inverse pole figure (IPF) maps (from normal axis) show, increased holding time favors the activation of recrystallization processes, leading to grain size refinement and the formation of equiaxed α grains (Fig. 4(a)-(c)). With the progress of recrystallization, β grains were sub-divided into regions by α grains exhibiting different degrees of refinement (Fig. 4(d)-(f)). The recrystallized region has a random texture, indicating that recrystallization annealing contributes to improved homogeneity of the grain orientation.

Fig.4. IPF maps of the a phase ((a)-(c)) and b phase ((d)-(f)) in samples annealed at 740℃ for 1 h, 2 h, and 5 h.

A 7×7×7μm3 volume of interest was used to represent the 3D morphology of the sample. Fig. 5(a) shows the IPF map of the α phase and the band contrast (BC) map of the β phase; Fig. 5(b) is the inverse of (a). The BC (Kikuchi image quality index), which reflects the degree of lattice distortion, of the α phase is larger than that of the β phase. This indicates that the retained strain energy of the a phase is larger than that of the β phase. The α grains shown in Fig. 5(c) and (d) have mean misorientations of 11.05° and 7.68°, respectively, whereas the β matrix grain (Fig. 5(e)) has a mean misorientation of 4.58°. The schematic hexagons and cubes, which showed the mean crystallographic orientation of these grains, were superimposed on the maps. The 3D observations revealed that large α grains were further refined to globular and equiaxed sub-grains during recrystallization annealing and the β grains were divided into sub-regions (i.e., large matrix grains with small misorientation). This suggests that the spatial microstructure is composed of a highly globular, homogeneous, and equiaxed α phase dispersed in a sub-structured β matrix.

Fig.5. (a) IPF map of the a phase and BC map of the b phase; (b) IPF map of the b phase and BC map of the a phase; 3D microstructure of (c) and (d) a grains; (e) a b matrix grain.

Microstructural characterization of an α+β type Ti-5.5Mo-7.2Al-4.5Zr-2.6Sn-2.1Cr alloy during recrystallization annealing

Journal of Alloys and Compounds 705 (2017) 183-187

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文献5(2012): 微观组织对Ti-6Al-4V-4Zr-1.5Mo 合金绝热剪切敏感性的影响(Effects of Microstructure on the Adiabatic Shear Banding Sensitivity of Ti-6Al-4V-4Zr-1.5Mo Alloy)

钛合金经过3种热处理后的1#、2#和3#显微组织如图3所示。其中图3a为低温退火后形成的1#等轴组织,其晶粒尺寸大约为10um,晶粒较细,a相分布较均匀;图3b为双重退火后形成的2#双态组织,即在网篮基体上分布着等轴状初生a相;图3c为β退火后形成的3#网篮组织,B相薄片分布在浅色a相层片。

图3 3种热处理组织形貌

微观组织对Ti-6Al-4V-4Zr-1.5Mo合金绝热剪切敏感性的影响非常明显。图5为3种组织在同一应变率(2300 s-1)条件下产生的剪切带的微观形貌,从图中可以看出:通过β退火得到的是纵横交错的网篮状组织,因此剪切带在扩展的过程中需要不断改变方向冲破更多的晶界的阻碍,同时在片状组织中运动方向的改变比在球状组织中更频繁,裂纹容易分叉形成次生裂纹,这些过程的结果使裂纹的总长度增加, 需要对更多的金属体积塑性变形做功,从而具有更高的断裂韧性。

图5 同一应变率下3种组织剪切带形貌

微观组织对Ti-6Al-4V-4Zr-1.5Mo 合金绝热剪切敏感性的影响

稀有金属材料与工程, 2012(01):45-48.

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文献6(2012):TC6 钛合金加热和冷却过程中的相转变研究(Phase Transformation in TC6 Titanium Alloy during Heating and Cooling)

图2为随炉升温至700, 750, 800, 850, 900 ℃,并在该温度保温15 min后水冷保留的高温状态下显微组织,其中αP、αS和β分别表示初生α相、次生α相和β相。由图2a~2e可知,随着保温温度升高,β基体内次生α相的相比例逐渐降低,β相相比例逐渐升高;在两相区较低温度(850℃及以下),如图2a、2b、2c和2d所示,初生α相相比例基本不变,而在两相区较高温度900 ℃时,如图2e所示,β基体内已经没有次生α相,初生α相颗粒细化,初生α相相比例显著降低;这说明在升温阶段,α相的固溶分为两个阶段,在较低温度段,β基体内次生α相优先固溶,等轴状初生α相在较高温度段才会固溶。

图2 不同保温温度水冷的显微组织

由图5 所示,次生α相析出前自900 ℃冷却至800 ℃的过程中,初生α 相的长大速度较快,相比例显著增加,图中虚线表示未析出次生α 相时初生α 相相比例的增加趋势;次生α 相析出后自750 ℃冷却至650 ℃的过程中,初生α 相的长大速度降低,相比例增加速率明显降低。次生α 相的析出会抑制初生α 相的长大,这主要是因为次生α相的析出会显著降低β 基体中溶质原子的过饱和度从而降低初生α 相的长大速度,而且β 基体中析出的次生α 相会阻塞初生α 相的长大。

图5 次生α相析出对初生α相长大速度的影响

TC6钛合金加热和冷却过程中的相转变研究

稀有金属材料与工程, 2012(12):2123-2126.

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文献7(2011):Effects of electric pulse heat treatment on microstructures and dynamic deformation behaviors of Ti6441 alloys(电脉冲热处理对Ti6441合金组织和动态变形行为的影响)

The SEM micrographs of the L0 and LP microstructures are shown in Fig. 4(a) and (b), respectively. Fig. 4(c) and (d) are local magnified SEM micrographs of the center regions of the prior beta grains, which show the microstructure details of alpha plates more clearly. As presented in Fig. 4(a) and (c), in the L0 microstructure without undergoing EPH treatment, nuclei of alpha phases form preferentially at the prior beta grain boundaries and the alpha phases grow fast into the grain interior from the grain boundaries along certain atomic planes. As a result, an alpha colony is developed. At the same time, nucleation occurs at the inside of the prior beta grain and then alpha colonies with different orientation are produced.

Fig.4. SEM micrographs of the lamellar (a), (c) L0 and (b), (d) LP microstructures, before and after EPH treatment, respectively. (c), (d) are the magnified images of partial region within (a) and (b), respectively.

As shown in Fig. 6, although the dynamic strength retains nearly the same high level, the LP microstructure undergoing EPH treatment performs much outstanding dynamic ductility with 29% in the fracture strain, in contrast with the L0 microstructure having the fracture strain of 23%, at the 3600 s-1 strain rate. This means that at the same strain rate, the LP microstructure can absorb much more energy due to the augment of fracture strain during the dynamic compression deformation process, showing the increase of load bearing time in contrast with L0 microstructure. As prior beta grains, alpha colonies, alpha plates and fine acicular alpha precipitates are refined, the significant increase of alpha/beta phase interfaces in LP lamellar microstructures has an advantageous effect on avoiding the stress concentration at the boundary of alpha/beta phase, because each alpha/beta interface is assigned to less stress. Hence, the LP microstructure can bear much longer time before fracture failure than the L0 one at the strain rate of 3600 s-1, showing the better dynamic ductility.

Fig.6. Stress–strain curves obtained from the dynamic compression test and SEM fractography of the dynamically fractured specimens for the (a) L0 and (b) LP microstructures, respectively.

Effects of electric pulse heat treatment on microstructures and dynamic deformation behaviors of Ti6441 alloys

Materials Science and Engineering A 530 (2011) 161–167

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文献8(2010):锻造工艺对 Ti-6Al-4V-4Zr-Mo 合金绝热剪切敏感性的影响(Effects of Forging Processing on Adiabatic Shearing Sensitivity of Ti-6Al-4V-4Zr-Mo Alloy)

钛合金经过α+β 锻造与β 锻造后的显微组织如图3 所示。从图3a 中可以看出,α+β 锻造得到了等轴状组织,为均匀分布的混合组织,其中有初生α 相和(α+β)混合体,晶粒尺寸为5 μm 左右。形成这种组织的主要原因是:在α+β 锻造过程中同时发生α 与β 晶粒形状的变化,β 晶粒被压扁,并沿着金属流动的方向被拉长、破碎,在一定温度与变形程度下开始发生再结晶现象,再结晶后的α 晶粒呈现扁球状,而一些未能完全进行再结晶的α 晶粒呈纤维状或杆状。从图3b 中可以看出,β 锻造得到的显微组织为网篮状组织,其晶粒尺寸较大,并有部分原始β 晶界残留,晶界不完整、不清晰。这是由于β 锻造的温度高于该合金的相变点,因此最后形成的显微组织为网篮组织。由于变形温度较高,导致了晶粒不断长大。另外,已被打碎的晶粒有重结晶现象发生,因此最终形成晶粒尺寸较大、组织不均匀的网篮状微观组织。

图3 不同锻造工艺处理后的微观组织

图4 分别为2种试样在应变率为1800,2250,2750s-1时动态剪切的时间-电压曲线。从图4a 可看出,在应变率1800 s-1条件下2 种试样均承受了80μs 而未出现应力塌陷,即二者均未发生绝热剪切破坏;当应变率升高到2250 s-1 时,如图4b 所示,β锻造后的试样的承载时间为57.6μs,即在57.6μs 时出现了应力塌陷,发生了剪切破坏,而α+β锻造后的试样仍能完整承载80μs,即没有剪切现象出现;如图4c 所示,当应变率达到2750 s-1时,2 种试样均出现了应力塌陷,但α+β锻造后的试样承载时间较β锻长。

图 4 2种试样在同一应变率下动态剪切的电压-时间曲线

锻造工艺对Ti-6Al-4V-4Zr-Mo合金绝热剪切敏感性的影响

稀有金属材料与工程, 2010, 39(S1):60-63.

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