Journal of Materials Processing Technology 78 (1998) 117 – 121 Development of the microstructure and fatigue strength of two phase titanium alloys in the processes of forging and heat treatment K. Kubiak *, J. Sieniawski Department of Materials Science, Rzeszów Uni6ersity of Technology, ul. W.Pola 2, 35 -959 Rzeszów, Poland Abstract The paper reports results of the studies on the influence of deformation degree and temperature in the die forging process and annealing temperature on the fatigue strength of forgings made of two phase martensitic titanium alloys Ti – 6Al –4V and Ti–6Al–2Mo–2Cr. Dilatometric and metallographic studies have been carried out along with X-ray phase analysis and fatigue tests. The influence of the phase composition and microstructure obtained after cooling with different rates on the fatigue strength have been determined. © 1998 Elsevier Science S.A. All rights reserved. Keywords: Two phase titanium alloys; Die forging; Microstructure; Fatigue strength the possibility of using the alloy in structural elements [4,5]. Therefore an effort has been made in this paper to determine the effect of plastic working conditions (strain rate and degree, forging method and temperature) on the fatigue strength of two phase, martensitic titanium alloys, Ti–6Al–4V and Ti–6Al–2Mo–2Cr. 1. Introduction The larger part of the elements made of two phase, martensitic, titanium alloys is fabricated in the process of plastic working. The service life and reliability of these alloys depend on the microstructure obtained after working and heat treatment and on the surface layer condition [1]. Development of different microstructure and phase composition in various regions of the forging is the result of the high sensitivity of two phase titanium alloys to the plastic deformation rate, degree and temperature [2,3]. Proper selection of these parameters allows control of the phase composition of the alloy (as a result of a’, a¦, b, v metastable phases forming and decomposition) and its mechanical properties. Dynamic strength is a basic criterion determining 2. Material and research methodology The material tested was two phase a+ b, martensitic titanium alloys Ti–6Al–4V and Ti–6Al–2Mo–2Cr having the chemical composition presented in Table 1. Dilatometric tests were performed using an absolute dilatometer LS-4. Changes in specimens elongation were measured by means of an inductive converter and Table 1 Chemical composition of the Ti–6Al–4V and Ti–6Al–2Mo– 2Cr alloys Alloy Ti–4Al – 4V Ti–6Al – 2Mo – 2Cr Stability factor Alloying elements and impurities content (%wt.) Kb Al Mo V Cr Fe C Si H N O Ti 0.3 0.6 6.1 6.3 — 2.6 4.3 — — 2.1 0.16 0.40 0.01 0.05 — 0.2 0.015 0.016 0.06 0.016 0.12 0.09 balance balance * Corresponding author. 0924-0136/98/$19.00 © 1998 Elsevier Science S.A. All rights reserved. PII S0924-0136(97)00472-X 118 K. Kubiak, J. Sieniawski / Journal of Materials Processing Technology 78 (1998) 117–121 X –Y recorder (Riken Denshi). Temperature was measured using a Ni–CrNi thermocouple. Rounded specimens 4 mm in diameter and 15 mm long with a ¥ 1.6 ×7.5 hole for the thermocouple were used for the tests. A protective argon atmosphere was used. The start and finish temperature of the a + b ? b phase transformation was determined for a heating rate 6h = 0.08 K s − 1. The specimens were soaked at the b-range temperature for half an hour and cooled at controlled average rate in the range of 6c =48 } 0.004 K s − 1. X-ray phase analysis and lattice constants measurements were carried out using a Philips diffractometer with a copper tube and nickel filter. Characteristic radiation CuKa was applied at a wavelength of l= 0.1542 nm. The microstructure of the specimens was examined using an optical microscope Neophot 2 and a transmission electron microscope Tesla BS613. Specimens were ground, polished and etched using etchants having following chemical composition: 50% HNO3 +40% HF+ 10% H2O or 10% HNO3 +2% HF +88% H2O at 270 K. Thin foil specimens were prepared by two-sided mechanical thinning and electrolytic polishing at 230 K in 5%HClO4 +35% C4H9OH +60% CH3OH electrolyte at 15 V at 0.05 A · cm − 2. Dilatometric examination was applied to determine the start and finish temperature of the a +b b phase transformation during alloy heating and cooling. On the basis of the phase transformation temperature the conditions of the plastic working of the alloys were defined. Forging was accomplished in the b-range (1320 K) and in the a +b-range (1170 K). Semifinished products (¥ 65 ×120) were forged on the crank operated power press LKM 4000 and then annealed according to the scheme presented in Table 2. Fatigue behaviour was examined in a rotational bending test according to the PN-76/H-04326 standard on the UMBS-4 machine with a frequency of 50 Hz. From 6 to 10 specimens were tested on each stress level and the terminal number of cycles was set to N =2 · 107. Specimens 7 and 3.5 mm in diameter were made of both as forged and heat treated forgings. Results of the Table 2 Heat treatment of Ti – 6Al–4V and Ti–6Al–2Mo–2Cr alloys forgings Forging temperature (K) Anealing parameters 1170 1320 1170 1320 1170 1320 1170 1320 — — 950 950 1060 1060 1250 1250 K K K K K K 3 3 3 3 1 1 h−1 h−1 h−1 h−1 h−1 h−1 air air air air air air Table 3 The start and finish temperature of the a+bb phase transformation for Ti – 6Al – 4V and Ti – 6Al – 2Mo – 2Cr alloys (6h =6c =0.08 K s−1) Phase transformation temperature (K) Alloy Ti – 6Al--4V Ti – 6Al – 2Mo – 2Cr T ns a+a b T ps a+a b T fa+a b T sa+a b T fa+a b 1090 1170 1260 1220 970 1110 1190 1260 1210 810 ns, Nucleation start; ps, precipitation start; s, start; f, finish. fatigue tests were statistically analysed in order to determine: average life Nav, S.D. s of average life, and confidence intervals for fatigue limit and fatigue strength. 3. Results and their analysis On the basis of the a+b ? b-phase transformation temperature (Table 3) the forging temperature was defined. Dilatometric and metallographic examination and structural analysis of the alloys (Table 4) after continuous cooling from the b-range with a rate in the range of 48–0.004 K s − 1 enabled the determination of model changes in their phase composition and microstructure. That in turn permitted the evaluation of quality of different regions of the forging. It was found that at the cooling rate 6c \ 18 K s − 1 formation of martensitic phases a%(a¦) takes place exclusively in both alloys. The start and finish temperature of the martensitic transformation b a%(a¦) or Table 4 Phase composition of the Ti – 6Al – 4V and Ti – 6Al – 2Mo – 2Cr alloys Cooling rate (K s−1) 48 40 18 9 7 3.5 1.2 0.08 0.04 0.024 0.008 0.004 Phase composition Ti– 6Al– 4V Ti– 6Al– 2Mo –2Cr a%(a¦) a%(a¦) a%(a¦) a+a%(a¦) a+a%(a¦) a+a%(a¦)trace+b a+b a+b a+b a+b a+b a+b a%(a¦) a%(a¦) a%(a¦) a+a%(a¦)+b a+a%(a¦)trace+b a+a%(a¦)trace+b a+b a+b a+b+TiCr2 a+b+TiCr2 a+b+TiCr2 a+b+TiCr2 K. Kubiak, J. Sieniawski / Journal of Materials Processing Technology 78 (1998) 117–121 119 Table 5 Fatigue strength of Ti – 6Al–4V and Ti–6Al–2Mo–2Cr alloys as a function of temperature and degree of deformation and annealing temperature of the forging Alloy Forging temperature (K) Fatigue strength (MPa) Plastic deformation (o1 =0.35) Plastic deformation (o2 =2.0) Annealing temperature (K) Ti–6Al – 2Mo – 2Cr Ti–6Al – 4V 1170 1320 1170 1320 — 950 1250 — 950 1060 1250 546 482 511 426 605 — 558 — — 465 — 417 261 351 262 340 285 372 283 362 232 — 221 — — 326 — 322 b a¦ does not depend on the cooling rate but on the b-stabilizing elements content. The bigger b-stabilizer content (Kb ) the smaller start and finish temperature of martensitic transformation. At the cooling rate in the range 6c =9 – 7 K s − 1 diffusion transformation ba and martensitic transformation b a¦ take place in the Ti – 6Al – 4V alloy resulting in the formation of a, a¦ and b phase mixtures [3]. Cooling of the alloy at the rate 6c B1.2 K s − 1 leads to the development of stable a and b phases in the shape of colonies of parallel a-phase lamellae in primary b-phase grains. However in the Ti – 6Al – 2Mo– 2Cr alloy at the cooling rate 6c \3.5 K s − 1 martensitic transformation b a%(a¦) was observed. Cooling of this alloy at the rate 6c B 0.024 K s − 1 results in eutectoid decomposition of the part of b-phase: b a +TiCr2. The forging temperature, the degree of deformation and the annealing temperature of the Ti – 6Al – 4V and Ti – 6Al–2Mo–2Cr alloys have very pronounced effect on the fatigue strength of the alloys studied (Table 5). It applies especially to Ti – 6Al – 2Mo – 2Cr alloy as the presence of chromium raises its susceptibility to phase composition changes (martensitic transformation b a‘‘). Metallographic examination revealed the significant effect of the forging temperature on the microstructure of Ti–6Al–4V and Ti – 6Al – 2Mo – 2Cr alloys (Figs. 1 – 4). After forging in the a +b-range (1170 K) a globular microstructure was formed with grain deformation depending on the degree of plastic strain. A characteristic feature of that microstructure was significant irregularity, i.e. various distortions of the a-phase grains (Fig. 1). Microstructure irregularity is related to the strain degree. The strain degree was calculated by numeric simulation using FORGE – 2 software [6,7]. The higher deformation degree the lower microstructure irregularity and the larger the a-phase grains distortion. Forging in the b-range (1320 K) generated lamellar microstructure (Fig. 2). Parallel lamellae of a-phase formed colonies in primary b-phase grains. Forging in the b-range leads to a primary b-phase grain refinement that follows the dynamic recrystallization processes. The annealing temperature of the forgings after plastic working has an influence on the fatigue strength. The maximum fatigue strength of the Ti–6Al–4V and Ti–6Al–2Mo–2Cr alloys was obtained after annealing at 950 K for 3 h. Increase in fatigue strength after annealing (950 K for 3 h) compared with the strength in as forged condition was: Ti–6Al–4V alloy forging temperature 1170K 9% forging temperature 1320 K 4% Ti–6Al–2Mo–2Cr alloy forging temperature 1170K 10% forging temperature 1320 K 6% Examination of the microstructure revealed that a recovery process took place in the alloys during annealing at 950 K for 3 h. A much lower dislocation density was observed in the a-grains and lamellae (Fig. 3). Annealing at 1250 K for 1 h led to a decrease in the fatigue strength comparing with the alloys both in as forged condition and annealed at 950 K for 3 h. For Fig. 1. Microstructure of the Ti – 6Al – 2Mo – 2Cr alloy after forging at 1170 K. 120 K. Kubiak, J. Sieniawski / Journal of Materials Processing Technology 78 (1998) 117–121 Fig. 2. Microstructure of the Ti–6Al–2Mo–2Cr alloy after forging at 1320 K. Fig. 4. Microstructure of the Ti – 6Al – 2Mo – 2Cr alloy after forging at 1170 K and annealing at 1250 K for 1 h. forging temperature 1320 K reduction in fatigue strength was: Ti –6Al–4V alloy strain degree o1 =0.35 2% strain degree o2 =2.0 5% Ti –6Al–2Mo–2Cr alloy strain degree o1 =0.35 4% strain degree o2 =2.0 8% Decrease in the fatigue strength is related to the volume fraction of the recrystallized microstructure which depends on the degree of deformation. Hardness measurements of the alloys forged at 1170 and 1320 K showed that the annealing temperature is a critical factor in considering the fraction of recrystallized microstructure and yet the degree of deformation has a minor effect (Table 6). Annealing of Ti – 6Al – 4V and Ti – 6Al–2Mo–2Cr alloys at 1250 K for 1 h promoted the formation of new recrystallized grains and lamellae of the a-phase and an increase in the fraction of recrystallized regions in the microstructure to 66 and 67% respectively. This was also confirmed by micro- scopic examination. Annealing at 1250 K resulted in the formation of new recrystallized grains and lamellae of the a-phase (Fig. 4) 4. Summary Analysis of the results of the Ti–6Al–4V and Ti– 6Al–2Mo–2Cr titanium alloys examined allowed us to determine: (1) the effect of the forging conditions, i.e. temperature, amount of deformation and cooling rate after forging on the phase composition, microstructure and fatigue strength of the alloys studied; (2) the effect of the heat treatment on the forgings, i.e. annealing temperature on their fatigue strength. Continuous cooling of the Ti–6Al–4V and Ti–6Al– 2Mo–2Cr alloys from the b-range produces a microstructure in the shape of colonies of parallel a-phase lamellae in primary b-phase grains with various phase compositions (a+ a%(a¦), a+ a%(a¦)+ b, a+ b, a+ b+ TiCr2). As a result of the increased chromium content (Kb = 0.6) the volume fraction of martensitic a%-phase grows in the Ti–6Al–2Mo–2Cr alloy. Table 6 Recrystallized microstructure fraction for Ti – 6Al – 4V and Ti–6Al– 2Mo – 2Cr alloys for various deformation conditions and heat treatment Alloy Recrystallized microstructure fraction (%) Deformation degree and heat treatment Fig. 3. Microstructure of the Ti–6Al–2Mo–2Cr alloy after forging at 1170 K and annealing at 950 K for 3 h. Ti– 6Al– 4V Ti – 6Al – 2Mo – 2Cr o =2.0 950°C 3 h−1 o= 2.0 1250°C 1 h−1 o =0.35 950°C 3 h−1 o =0.35 1250°C 1 h−1 34 36 66 67 26 27 63 60 K. Kubiak, J. Sieniawski / Journal of Materials Processing Technology 78 (1998) 117–121 Forging of two phase titanium alloys at the b a+ b transformation temperature develops a globular microstructure. Lamellar microstructure is formed during forging in the primary b-phase temperature range. The fatigue strength of the alloys studied depends on the forging temperature, which controls the type of microstructure, and plastic deformation degree. The maximum fatigue strength was obtained by forging at 1170 K (Ti–6Al–2Mo – 2Cr, 546 MPa; Ti – 6Al–4V, 511 MPa). Forging at 1320 K leads to a decrease in fatigue strength (Ti – 6Al – 2Mo – 2Cr, 482 MPa; Ti– 6Al –4V, 426 MPa). Increased plastic deformation degree lowers the fatigue strength. Decrease in the fatigue strength is smaller in the case of forging in the b-range than in the a+ b-range. The fatigue strength of the alloys depends also on the heat treatment of the forgings. During annealing microstructure recovery and recrystallization processes take place and result in fatigue strength changes. For example during annealing at 950 K for 3 h a recovery process took place and the maximum fatigue strength was obtained (Ti–6Al – 2Mo – 2Cr, 605 MPa; Ti –6Al– . 121 4V, 558 MPa). After annealing at 1250 K for 1 h the recrystallized microstructure fraction was found to be as high as 67% which led to a decrease in the fatigue strength. Acknowledgements This work was supported by the KBN under Grant 708A03809. References [1] I.J. Polmear, Light Alloys, Arnold, London, 1995. [2] J. Sieniawski, Zeszyty Naukowe Politechniki Rzeszowskiej, Mechanika 10 (1985). [3] J. Sieniawski, Inz; . Materiałowa, 2 – 3 (1993) 64. [4] H. Inagaki, Z. Metall. 6 (1990) 324. [5] R.V. Miner, Fatigue of Superalloys, Wiley, New York, 1987. [6] A. Piela, Arch. Metall. 1 (1993) 101. [7] Program FORGE – 2, CMFM, Ecole Nationale Soperieure des Mines, de Paris rue C. Daunesse, Sophia Antipolis, 06560 Valbonne cedex, France.