International Journal of Minerals, Metallurgy and Materials V olume 20 , Number 3 , March 2013 , P age 266 DOI: 10.

1007/s12613-013-0722-7

Inuence of semisolid forging ratio on the microstructure and mechanical properties of Ti14 alloy
Yong-nan Chen1,2) , Gang Liu1) , Xue-min Zhang2) , and Yong-qing Zhao3)
1) State Key Laboratory for Mechanical Behavior of Material, Xian Jiaotong University, Xian 710049, China 2) School of Materials Science and Engineering, Changan University, Xian 710064, China 3) Northwest Institute for Nonferrous Metal Research, Xian 710016, China (Received: 19 April 2012; revised: 24 June 2012; accepted: 26 June 2012)

Abstract: The present work is focused on the microstructure and mechanical properties of Ti14 alloy with dierent semisolid deformation ratios during forging tests. The results revealed that the forging ratio had a signicant eect on the precipitation of the alloy. Fewer plate-shaped Ti2 Cu tended to precipitate on grain boundaries with higher forging ratios, and nally the plate-shaped Ti2 Cu formed precipitate-free zones along grain boundaries with a forging ratio of 75%. The precipitation on grain boundaries was found to be controlled by a peritectic reaction. Large forging ratios accelerated the extrusion of liquid and resulted in less liquid along the prior grain boundaries, which reduced the peritectic precipitation in this region and formed precipitate-free zones during re-solidication. In addition, increasing the forging ratio could accelerate dynamic recrystallization, which is favorable for improving the semisolid formability. The tensile ductility increased with increasing forging ratio, and a mixed fracture mode, involving both cleavage and dimple fracture, was observed after forging with a forging ratio of 75%, which is attributed to the presence of precipitate-free zones formed along grain boundaries during semisolid processing. Keywords: titanium alloys; semisolid; forging; microstructure; precipitates; mechanical properties

1. Introduction
Semisolid forming is an eective net-shaped forming process by deforming metals in the semisolid state, which combines elements of both casting and forging and presents many advantages over the conventional process [1]. Compared with conventional forming methods, semisolid forming is characterized by a number of factors including a low deformation resistance, which facilitates the shaping process, a reduced energy input, and lower capital costs, all of which are benecial to productivity [2]. On account of the above advantages, extensive works in the semisolid deformation and processing behavior of Al, Mg, and steel have been carried out by many scientists and engineers. The results showed that the processing parameters, such as forging/rolling temperature or forging/rolling
Corresponding author: Yong-nan Chen

ratio, play a very important role in controlling the microstructural evolution during semi-solid forming (SSF) [3-8]. Generally, the deformation temperature is associated with the volume fraction of the liquid phase present, whereas the deformation ratio is associated primarily with the distribution of the liquid phase in semisolid processing. Therefore, the microstructure and mechanical properties can be improved by controlling the processing parameters [9-11]. During the past 5 years, our group [12-15] has investigated on the deformation and thixoforging behavior of Ti14 alloy in semisolid state and found that temperature has a signicant eect on the ow behaviors of liquid in semisolid state, which result in dierent precipitation characteristics and mechanical properties. However, the inuences of deformation and/or forging ratio, which are con-

E-mail: frank [email protected]

c University of Science and Technology Beijing and Springer-Verlag Berlin Heidelberg 2013

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sidered the other important processing parameters, on the ow behaviors of liquid and microstructure as well as mechanical behavior of Ti14 alloy have not been reported yet. In this work, a comprehensive study of the microstructure evolution, particularly the precipitation behavior on grain boundaries with dierent forging ratios, was carried out to reveal the relationship among forging ratio, microstructure, and mechanical properties.

2. Experimental
2.1. Materials
Ti14 is a new + Ti2 Cu-type burn-resistant Ti alloy [16-17]. There are many Ti2 Cu phases in the alloy. The melting point of Ti2 Cu is 990 C. If the deformation or testing temperature increases above 990 C, Ti14 alloy changes to a semisolid state. During the cooling process, the alloy undergoes both peritectic reaction (990 C) and eutectoid reaction (790 C).

lated using Olympus 3M software and the mean transversal method. SEM studies were carried out to evaluate the microstructure and to determine the distribution of precipitates on grain boundaries. The fracture surface features, after tensile testing, were also examined by SEM. TEM studies were performed to observe the morphology of precipitates in the grain boundary regions. TEM foils were prepared by twin-jet electropolishing in a solution of 95vol% butyl alcohol and 5vol% perchloric acid at 15 V and 30 C.

3. Results
3.1. Eect of compression ratio on the distribution of liquid phase during compression tests
Microstructures of samples compressed with dierent compression ratios are shown in Fig. 1, in which partial melting mainly occurred in the grain boundary regions, and much less liquid was observed in the center of the compression samples with an increase of compression ratio. The relationship of compression ratio and ow rate can be demonstrated as follows [10]: v V fl (1)

2.2. Compressive deformation tests

The compressive deformation tests were conducted to investigate the distribution of liquid with dierent compressive ratios. Cylindrical specimens with a diameter of 8 mm and a height of 12 mm were cut from the original bar. Specimens were compressed to heights of 6, 5, and 3.5 mm corresponding to compression ratios of 50%, 60%, and 75%, respectively, using a Gleeble-1500 thermal simulator at a deformation temperature of 1050 C.

2.3. Forging tests

The inuence of processing deformation ratio on the microstructure of Ti14 alloy in a semisolid state was studied by forging tests. The Ti14 alloy used in this paper was a 30 kg ingot; after conventional ingot breakup and forging to bars of 40 mm in diameter, the material was reforged to nal diameters of 20, 25, and 30 mm at 1050 C, corresponding to a forging ratio of 45%, 60%, and 75%, respectively.

where v is the ow rate, V is the strain rate, fl is the liquid fraction, and is the compression ratio. The estimated ow rate increases with an increase in compression ratio and more liquid tends to ow to the surface of the samples with a higher ow rate. As a result, much less liquid segregated to grain boundaries with a larger compression ratio during semisolid processing (Figs. 1(a)-1(c)).

3.2. Eect of forging ratio on microstructure

Fig. 2 shows the cross-sectional microstructures of specimens forged at 1050 C with a forging ratio of 45%, 60%, and 75%. It is obvious that the grain size of -Ti is rened with an increase in forging ratio. The grain size of the specimens and the reduction in grain size (compared with the grain size of the as-received specimen, 700 m) are provided in Table 1. For each of the forging ratios, it can be seen that the grain size decreases with an increase in forging ratio, and the grain size is reduced by about 51% with 75% forging compared with that of the as-received sample. This suggests that dynamic recrystallization has occurred during semisolid forging; moreover, higher forging ratios can promote dynamic recrystallization, resulting in significant grain renement. This recrystallization mechanism gradually makes the grains rounder and ner, which plays an important role in improving the semisolid formability. A previous research [12] on the relationship between semisolid forging temperature and microstructure revealed

2.4. Test of mechanical properties

Cylindrical tensile specimens, with a diameter of 4 mm and a gauge length of 45 mm, were cut from the forged billets. The machined specimens were wet grinded using waterproof emery paper down to 1500#. Tensile tests were conducted using an Instron testing machine at room temperature with a nominal strain rate of 4.2103 s1 .

2.5. Analysis of microstructure

Microstructures after compression and forging tests were analyzed by optical microscopy (OM; Olympus GX71), scanning electron microscopy (SEM; JSM-6700), and transmission electron microscopy (TEM; JEM200CX). All samples were cut from the center of the various specimens. The grain size after forging was calcu-

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Fig. 1.

Microstructures of the samples compressed at 1050 C with dierent ratios: (a) 50%; (b) 60%; (c) 70%.

Fig. 2.

Tri-planner micrographs of Ti14 alloy after forging at 1050 C with dierent forging ratios: (a) 45%; (b)

60%; (c) 75%. Grain size of Ti14 alloy forged at 1050 C

Table 1.

Forging ratio / % Grain size / m Reduction in grain size / % 45 418 21 40 60 387 15 45 75 345 15 51

that no -phase was found after forging at 1050 C. In this study, irrespective of the forging ratio, the samples also mainly consisted of an -Ti matrix and Ti2 Cu precipitate phase. Ti2 Cu precipitation occurred both within grains and along grain boundaries in the samples at each

forging ratio (Figs. 2(a)-2(c)). Fig. 3 shows the distribution of precipitates on grain boundaries for the samples after forging with dierent forging ratios. A coarse grain boundary structure consisting of plate-shaped Ti2 Cu precipitates was observed in the sample with a forging ratio of 45% as shown by white arrows in Fig. 3(a), but less plate-shaped Ti2 Cu tended to precipitate on grain boundaries with higher forging ratios (Figs. 3(b) and 3(c)). As a result, a plate-shaped Ti2 Cu precipitate-free zone was formed closed to grain boundaries as shown in Fig. 3(c) with a forging ratio of 75%.

Fig. 3.

SEM images of the grain boundaries after forging with forging ratios of 45% (a), 60% (b), and 75% (c).

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It was further conrmed by TEM observations on the morphologies of Ti2 Cu precipitates on grain boundaries with dierent forging ratios (Fig. 4). Ti2 Cu nucleated and grew on grain boundaries with a forging ratio of either 45% or 60% (Figs. 4(a) and 4(b)), and almost no Ti2 Cu precipitated on grain boundaries with a forging ratio of 75% (Fig. 4(c)). The fraction of plate-shaped Ti2 Cu on grain boundaries decreased obviously with increasing forging ratio, indicating that forging ratio has signicant eects on the distribution of precipitates on grain boundaries, with more Ti2 Cu precipitation occurring on grain boundaries under a lower forging ratio.

3.3. Mechanical properties

Table 2 shows the room temperature tensile properties of the semisolid forged alloy. It is notable that the elongation and reduction in area decreased markedly after forging compared with the as-received alloy and increased

with increasing forging ratio. For example, the elongation reduced by 87.5%, 60%, and 20% after forging with forging ratios of 45%, 60%, and 75%, respectively, compared with that of the as-received sample. It can be reasonably explained by referring to the presence of Ti2 Cu precipitation in the grain boundary regions. However, the inuence of forging ratio on the strength is rather weak, and the yield strength increased by 25%, 28%, and 29.5% after forging with the forging ratios of 45%, 60%, and 75%, respectively, compared with that of the as-received material. These results are associated with the dependence of grain size on forging ratio. It is well known that hexagonal close-packed (hcp) metals such as titanium exhibit a strong grain size dependence of strength due to the lack of slip systems [18]. Therefore, the increase in strength of the forged specimens is associated with grain renement induced by dierent forging ratios.

Fig. 4.

TEM morphologies of Ti14 after forging with forging ratios of 45% (a), 60% (b), and 75% (c). Table 2. Room temperature tensile properties of Ti14 alloy with dierent forging ratios UTS / MPa 840 955 970 975 UTS / % 13.6 15.5 16.1 YS / MPa 680 850 870 880 YS / % 25.0 28.0 29.5 El / % 20 2.5 8.0 16.0 El / % 87.5 60.0 20.0 RA / % 40 11.0 17.5 30.5 RA / % 72.5 56.3 23.8

Forging ratio / % As-received 45 60 75

Notes: (1) UTS, tensile strength; YS, yield strength; El, elongation; RA, reduction in area. Elas-recevied 100%; RA = (RAsemisolid RAas-received )/RAas-recevied 100%.

(2) UTS = (UTSsemisolid

UTSas-received )/UTSas-recevied 100%; YS = (YSsemisolid YSas-received )/YSas-recevied 100%; El = (Elsemisolid Elas-received )/

Fig. 5 illustrates the SEM fractographs of the room temperature tensile specimens after SSF with dierent forging ratios. The sample with a forging ratio of 45% displays a brittle fracture mode and a typical intergranular fracture surface (Fig. 5(a)), where the delamination of precipitates and the matrix is the principal mechanism for the nucleation of microcracks. When these microcracks propagate and reach the coarse grain boundaries, cracks are deected and follow the grain boundaries, causing intergranular fracture. Moreover, a mixed mode of failure involving both cleavage and dimple fracture is observed with forging ratios of 60% and 75% (Figs. 5(b) and 5(c)).

Also, the tensile elongation increases dramatically with an increase in forging ratio from 45% to 75% (Table 2). It seems reasonable to assume that the low ductility is related to the amount and distribution of these peritectic-derived Ti2 Cu precipitates on re-solidication of the semisolid processed material.

4. Discussion
4.1. Eect of semisolid forging ratio on precipitation
The results of compression experiments and Eq. (1)

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Fig. 5.

Room temperature tensile fractograghs of Ti14 alloy after forging with forging ratios of 45% (a), 60% (b),

and 75% (c).

indicated that the compression ratio has great eect on the distribution of liquid on grain boundaries for Ti14 alloy. A larger compression ratio causes a higher liquid ow rate, and this accelerates liquid ow from the center to the surface of the sample by grain boundaries and nally results in less liquid segregates at grain boundaries. A similar trend was obtained during the forging test, more liquid segregates to the surface of the forging bar via grain boundaries with increasing forging ratio, and this leads to less liquid distributed at grain boundaries in the center of the forging bar. It is well accepted that the volume fraction and distribution of liquid are associated with temperature and deformation ratio, respectively. In the present work, the volume fraction and distribution of the liquid phase has a signicant inuence on the amount of precipitation of Ti2 Cu on grain boundaries during the re-solidication. The re-solidication and phase transformation pathway for

the alloy studied in our tests are described as follows: L + Ti2 Cu (peritectic) + + Ti2 Cu (eutectoid) + Ti2 Cu (peritectic). The liquid phase forms a thin lm on the grain boundary during the forging, and the transformation of L + Ti2 Cu (990 C) occurs where the liquid is present at the /L interface via a peritectic reaction. The distribution and amount of peritectic Ti2 Cu signicantly depend on the distribution and the volume fraction of liquid present during semisolid processing. In this study, more liquid segregates to the surface of the forging bar via grain boundaries, leaving less liquid in the grain boundary regions in the center of the forged bar with increasing forging ratio, and this results in the formation of less peritectic Ti2 Cu precipitates, as schematically shown in Fig. 6. This is the main reason for the formation of precipitatefree zones along grain boundaries for forging ratios of 75% and greater.

Fig. 6.

Simulated diagrams of Ti2 Cu precipitation on grain boundaries with increasing forging ratio.

4.2. Eect of semisolid forging ratio on tensile properties

The dierences in properties for the as-received alloy

and the hot forged one can be explained by the microstructure change resulting from semisolid forging. Grain renement caused by forging suggests that dynamic recrystallization occurs during forging. All the semisolid forged materials showed a higher strength and lower ductility than

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that of the as-received alloy at room temperature. The increase in strength is due to the ner grain size caused by dynamic recrystallization. The decreased ductility is believed to be associated with the precipitation of Ti2 Cu phase in the grain boundary regions [19]. Forging ratio has a weak eect on the strength due to the fact that the grain size is not altered greatly with increasing forging ratio, at least over the range investigated, which can be clearly seen in Table 1. However, forging ratio has a signicant inuence on the ductility due to the precipitation at grain boundaries. It is found that the distribution of Ti2 Cu precipitates on grain boundaries caused by peritectic reaction is the main reason for the dierence in ductility of samples with dierent forging ratios. More Ti2 Cu tended to nucleate and grow on grain boundaries via peritectic reaction under low forging ratios, which resulted in a coarse structure in the grain boundary regions. The coarse structure is considered to be the main principal mechanism for the nucleation of microcracks and subsequent intergranular fracture. The increase in ductility with increasing forging ratio suggests that increasing the forging ratio reduces the amount of liquid undergoing the peritectic reaction and therefore produces less Ti2 Cu precipitates, resulting in the improvement in ductility. In general, the above experimental results and discussion indicate that the method of semisolid forging can be employed to improve the tensile properties of Ti14 alloy, especially on ductility, by controlling forging ratio. In addition, within the test regions, the increase of forging ratio can facilitate dynamic recrystallization, which is favorable to formability during semisolid processing.

a signicant reduction in ductility at room temperature and causes intergranular fracture.

Acknowledgements
This work was nancially supported by the Major State Basic Research Development Program of China (No. 2007CB613807), the State Key Laboratory for Mechanical Behavior of Materials (No. 0111201), and the National Natural Science Foundation of China (No. 51201019).

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5. Conclusions
The eect of semisolid forging ratio on the microstructure and mechanical properties of Ti14 alloy was investigated by forging tests with the ratios ranging from 45% to 75%. The conclusions are as follows. (1) Forging ratio aects the distribution of Ti2 Cu precipitates in the grain boundary regions. As the forging ratio increases, much less Ti2 Cu tends to precipitate on and near grain boundaries via the peritectic reaction during post-forging solidication, which can lead to precipitatefree zones along grain boundaries for large forging ratios (i.e., 75%). (2) High strengths are obtained for all forged alloys, which are attributed to grain renement caused by dynamic recrystallization. (3) The dierences in ductility are associated with the distribution of Ti2 Cu precipitates resulting from dierent forging ratios. The extensive formation of precipitates in the grain boundary regions with low forging ratio leads to

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