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Grain refinement of / phase Ti-6Al-4V alloy by thermomechanical treatment

Pakawadee Sirilar1 and Panya Srichandr2 Division of Materials Technology, School of Energy and Materials King Mongkuts University of Technology Thonburi, Bangkok 10140 Phone 0-2470-8643, Fax 0-2427-9062, E-Mail: paka_wd@hotmail.com Abstract This paper summarizes the experiment on grain refinement of two phase Ti-6Al-4V alloy by thermomechanical treatment (TMT) methods. The hot rolling was conducted on alloy with starting equiaxed-, 20 micron grain size, at temperature range of 850-950C and reduction per pass of 16 and 64% plus air cooling. It was found that the 950C deformation with 64 % reduction per pass produces the 8 micron refined equiaxed-. Grain refinement at the temperature of / phase equilibrium below transus temperature with large reduction percentage is resulted by dynamic recrystallization (DRX). However, hot rolling with 16% reduction per pass produces very large flow structure which can be refined by globularization during annealing. The annealed structure at 950C for 4 hours shows globularized- which grain-aspect-ratio is 1.2. 1. Introduction Thermomechanical treatment methods of / phase Ti-6Al-4V alloy usually involves a series of hot rolling and heat treatment steps which ultimate objective is to produce a uniform, fine, globularized- grain [1]. The mechanical properties of Ti-6Al-4V are strongly influenced by the grain size and the well-known Hall-Petch equation [2] with a decrease in grain size ( d ). Annealing time and temperature affect the conversion of microstructures by globularization [5]. The objective of this paper is to analyze the grain refinement of Ti-6Al-4V alloy during TMT methods by microstructural observation and tensile property measurements. 2. Experimental procedures Ti-6Al-4V from Verkhnaya Salda Metallurgical Production Association : VSMPO, USSR having the follow composition (wt%) was used in this paper: 6.3Al, 4V, 0.008C, 0.18F, 0.168O, 0.007N, 0.004H and balance Ti. The transus temperature for this materials is about 990C. As received bar stocks of 15 mm diameter in the mill annealed condition were used for testing and the starting microstructure consisted of equiaxed- grain and small amount of intergranular-. The specimens were cut of 80 mm in height for two pieces, solution treatment at 950C for 1 hour was followed plus furnace cooling. After that, the first piece was hot rolled at 950C with 64% reduction per pass (Ti-64) and with 16% reduction per pass, total 64%, for the second piece (Ti-16) then both pieces were cooled by air cooling. The T-16 was divided into three pieces and were annealed at 950C for 1,2 and 4 hours respectively, follow by furnace cooling. Microstructures were observed by optical microscope (OM) and scanning electron microscope (SEM) and grain size was measured by image analyzer in ASTM standard E1382[7]. 3. Results and discussion 3.1 Influence of hot rolling on microstructures Starting microstructure of Ti-6Al-4V, after solution treatment, consist an equiaxed- with 20 micron mean grain size as shown in Fig. 3.1 X2000 grain (black)

y =o +

K d

(1)

Ti-6Al-4V alloy has two different phases: phase with HCP crystal structure, stable at lower temperature and phase with BCC crystal structure, stable at higher temperature. The transformation temperature from to is called transus temperature [3]. The alloy may be heat treated to obtain a variety of microstructures ranging from transformed- to equiaxed- [4]. Hot rolling below transus temperature with large reduction per pass produces fine and equiaxed- grain. Early studies of Seshasharyulu et al. [5] on the hot working of Ti-6Al-4V with an equiaxed - microstructure indicated that the DRX only occurred below transus temperature. Elagina et al. [6] suggested that the hot rolling with 10, 20, 30 and 40% reduction per pass at 950C produces structure of refined-. Increases in reduction percentage is important from a viewpoint.

-intergranular (white)

10 m

Fig. 3.1 Starting microstructure of Ti-6Al-4V, SEM

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X10

(a)

50 m

The primary- grain is produced after globularization for 1 hour annealed as shown in Fig. 3.3 (b) and the amount of globularization increases when annealing time is increased, in Fig. 3.3 (c) for 2 hours and in Fig. 3.3 (d) for 4 hours. Because of different dislocation density along the flow structure, higher at the edges and lower at the middle, primary- grain was nucleated on the edges before other sites as shown in Fig. 3.3 (b).

X10
X10 kinking

X10

(b)

(a)

50 m

50 m 50 m

Fig. 3.2 Microstructure of Ti-6Al-4V (a) before TMT and (b) after 950C hot rolling with 64% reduction, T-64, OM The as-rolled microstructures of the T-64 and T-16 are summarized in Fig. 3.2 and in Fig. 3.3 respectively. The T-64 material gave rise to refine equaxed- grain, Fig. 3.2 (b) shows the refined- grain of 8 micron. Because of a critical dislocation density, nucleation usually generates on pre-existing grain boundary or other high energy defects inside grains. The dynamically recrystallized grains are equiaxed and the mean grain size remains constant, grain growth does not occur during deformation. This process is called DRX [8]. In contrast, in the T-16 material gave rise to much obvious kinking is shown in Fig. 3.3 (a). The kinking of flow structure (black arrow) is occurred because of flow softening at low strain [9], dislocation substructure change and dynamic globularization have been eliminated. This kinking may increase dislocation density especially at the edge of the flow structure. 3.2 Influence of annealing on microstructures After 950C hot rolling with 16% reduction per pass, T-16 was divided into three pieces and were reheated at 950C for 1,2 and 4 hours respectively, follow by furnace cooling. Micrographs of specimens annealed at 950C and different annealing time are shown in Fig. 3.3 (b)-(d), which exhibit globularization of the kinking structure.

X10

(b)

globularized grain
50 m

X10

(c)

50 m

X10 X10

(d)

50 m

Fig. 3.3 Microstructure of T-16 (a) after 950C hot rolling with 16% reduction and after 950C annealed for (b) 1, (c) 2 and (d) 4 hours, grain-aspect-ratio of 1.2, OM

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After 4 hours annealing, the grain conversion was completed and near equiaxed- grain was occurred with grain-aspect-ratio is 1.2.
80 70 60 frequency 50 40 30 20 10 0 0 5 10 15 20 25 30 35 grain size (micron) after TMT
before TMT

for martensite structure. The differences are resulted by dislocation density and grain orientation change [10]. 4. Conclusion 1. The two processes for grain refinement by TMT are dynamic recrystallization and globularization. 2. Dynamic recrystallization was occurred during hot rolling below transus temperature, the temperature of / phase equilibrium, with higher reduction per pass. The dynamically recrystallized grain were equiaxed and refined. 3. Globularization was occurred after annealing below transus temperature, the material was hot rolled with lower reduction per pass. The primary- grain was produced at the edge, kinking, of flow structure. 4. The tensile properties of Ti-6Al-4V are strongly influenced by the grain size and shape, because of the difference in dislocation density and grain orientation. 5. Acknowledgement Division of Materials Technology, School of Energy and Materials, King Mongkuts University of Technology Thonburi and National Metal and Materials Technology Center (MTEC).

Fig. 3.4 grain distribution of Ti-6Al-4V before TMT with 20 micron mean grain size and after TMT (T-64) with 8 micron mean grain size

2000 1800 1600 1400 1200 1000 800 600 400 200 0
mic ron Wi dm ans tatt en Ma rten site cie ved mic ron

18 16 14 12 10 8 6 4 2 0

tensile/yield strength (MPa)

elongation (%)

6. References [1] Ari-Gur, P., Semiatin, S. L., Materials Science and Engineering A, A257 (1998) 118. [2] Humphreys, F. J, Prangnell, B. P., Priestner, R., Solid State and Materials Science, 5 (2001) 15. [3] American Society for Metal, Metal Handbook Vol.9, Ninth Ed, ASM, 1989. [4] Boyer, R., Welsch, G., Collings, E. W., Materials Properties Handbook : Titanium Alloys, ASM International, 1994. [5] Seshasharyulu, T., Medeiros, S.C., Frazier, W.G., Prasad, Y.V.R.K., Materials Science and Engineering A, A325 (2002) 113, 117. [6] Elagina, L. A., Gorgienko, A. I., Evmenov, O. P., Titanium and Titanium Alloys, 2 (1989) 1789. [7] Leica Microsystems Imaging Solutions, Cambridge, United Kingdom, 2001. [8] Ding, R., Guo, Z.X., Computational Materials Science, 23 (2002) 209. [9] Miller, R.M., Bieler, T.R., Semiatin, S.L, Scripta Materialia, 40 (1999) 1392. [10] Nishimura, T., Tsumori, Y., Shimizu, K., Titanium and Titanium Alloys, 2 (1987) 1987.

As -re

Eq uia x

Eq uia x

tensile strength

ed, 20

ed, 8

grain shape, size yield strength elongation

Fig. 3.5 tensile properties of Ti-6Al-4V 3.3 Influence of microstructures on tensile properties The tensile properties of Ti-6Al-4V were depended on microstructures. Tensile and yield strength increase with decrease in grain size, from Hall-Petch equation (1). Fig. 3.5 indicated the increase of tensile strength from 957.38 to 989.85 MPa and yield strength from 918.18 to 942.12 MPa with decrease of grain size from 20 to 8 micron. However, the different grain shapes may affect the different properties. Tensile and yield strength are 1604.20 and 1543.82 MPa respectively for Widmanstten structure, and are 1741.56 and 1704.10 MPa respectively