Materials Science Forum Submitted: 2015-02-13

ISSN: 1662-9752, Vols. 828-829, pp 194-199 Revised: 2015-05-07

doi:10.4028/www.scientific.net/MSF.828-829.194 Accepted: 2015-05-07
© 2015 Trans Tech Publications, Switzerland Online: 2015-08-26

Effect of Ageing Treatment on the Microstructure and Hardness of the

Ti6Al4V Alloy
MASETE Stephen1,2,a *, MUTOMBO Kalenda1,2,b SIYASIYA Charles2,c
and STUMPF Waldo2,d
1
Materials Science and Manufacturing, Council for Scientific and Industrial Research (CSIR),
Pretoria, South Africa
2
Department of Materials Science and Metallurgical Engineering, University of Pretoria, Pretoria,
South Africa
a
[email protected], [email protected], [email protected],
d
[email protected]

Keywords: Ti6Al4V alloy, solution treatment, ageing, microstructure, hardness.

Abstract. The effects of ageing temperature, time and cooling medium on the microstructure and
hardness of a solution treated Ti6Al4V alloy were investigated. The furnace cooling after ageing for
0.5 hours gave a homogenous structure with higher hardness values than the solution treated and
water quenched Ti6Al4V alloy. Increasing the ageing time to 2 hours reduced the alloy hardness.
Ageing at temperatures between 500 and 7000C, followed by furnace cooling, led to homogenously
distributed α- and β-phases within a fully martensitic matrix leading to improved hardness. A
heterogeneous structure with a high variation in microhardness was revealed when ageing at 800
and 9000C.

Introduction
Ti6Al4V alloys are used mainly in the aerospace industries due to their excellent mechanical
properties, low density and good corrosion resistance [1,2]. The mechanical properties of such
alloys can be optimised during thermo-mechanical processing, which is sensitive to the chemical
composition which may lead to varying microstructural phases and mechanical properties.
Extensive work on the solution heat treatment of the Ti6Al4V alloy at different temperatures and
cooling rates is available [1,2,3,4,5,6], but there is not much data on the effect of ageing
temperature and time on the microstructures and mechanical properties. Most of these authors
[1,3,4] performed solution treatment at temperatures below the beta transus (T. Zeng and Bieler
[2] studied the microstructural evolution of primary alpha (p), secondary alpha (s), beta (,
hexagonal martensite (') and orthorhombic martensite ('')phases in a solution treated and aged
Ti6Al4V wire alloy. These authors showed that metastable phases such as '' and form during
ageing but may transform back to the phase with natural ageing for up to a year. The authors also
indicated that this transformation depends on the temperature and chemical composition of the alloy
but they did not indicate how these phases affect the mechanical properties of the alloy. Youssef et
al. [3] did solution treatments above the  transus temperature but only considered one ageing
temperature and ageing time. These authors found the hardness to increase after solution treatment
and ageing.
Most literature sources suggest that it is costly and time consuming to solution treat and age the
Ti6Al4V alloy. It is preferable to find optimum solution treatment conditions and avoid ageing
treatment [1,4,5] through direct cooling. In most of the cases the ageing treatment is done to
improve the ductility of the alloy after solution treatment and quenching. Solution treated and
quenched Ti6Al4V alloys are mostly high strength alloys as they contain ' martensite which makes
the alloy brittle, hence increasing the need for an ageing treatment to improve the ductility [1,2,3,4].
Reda et al. [4] proposed to solution treat the Ti6Al4V alloy below the -transus temperature of

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 Materials Science Forum Vols. 828-829 195

987 0C to avoid grain coarsening and the formation of a high volume fraction of fine ' martensite
to optimise the strength, elongation and impact strength.
It has also been realised that the resulting microstructural phases of the heat treated alloys from the
literature were not necessarily optimised but resulted simply from heat treatment temperatures
chosen by the authors [1,2,3,4]. Furthermore, none of the authors examined closely the presence
and effect of microstructural phases on the alloy’s mechanical properties.
Understanding how microstructure changes with the ageing treatment, can aid in optimising
microstructural morphology and phases present in Ti6Al4V alloys. This study aims to investigate
the effects of ageing time, temperature and cooling medium on the final microstructure and phases
present in the Ti6Al4V alloy and its effects on the corresponding hardness.

Experimental procedure
Ti6Al4V specimens were solution treated at 10500C for 30 minutes in air in a Naber N150
muffle furnace and quenched in water (WQ) or air cooled (AC) or furnace cooled (FC) to room
temperature. Samples were cut from the solution treated specimens for ageing experiments at 500,
600, 700, 800 and 900 0C. Ageing times of 0.5 and 2 hours were used, and samples were furnace
cooled (FC) or water quenched (WQ). Aged samples were sectioned to remove the alpha-case and
hot mounted. They were then ground, polished and etched using Kroll’s reagent.
A Leica DMI5000M inverted optical microscope equipped with image analysis software (Image
Pro Plus) was used to investigate the microstructural changes after the solution and ageing
treatment. The automatic Vickers micro-hardness tester FM-700 equipped with Future–Tech
software was used to measure the hardness change and microstructural homogeneity. Each sample
was loaded at 500 gram force for 10 seconds and was indented on four separate parallel lines. The
indents were 250 m apart and lines 1.5 mm apart.

Results and discussions

The samples of Ti6Al4V solution treated and water quenched produced a fully martensitic
microstructure as shown in Fig. 1(a). The martensite was identified by fine acicular' phases seen
as needle-like shapes. The grain boundaries consisted entirely of a dark  phase. The Ti6Al4V
solution treated and air cooled produced a partially martensitic microstructure shown in Fig. 1(b).
The microstructure was identified by the partial transformation of  to  phase on grain boundaries
and shown as a light-coloured phase. The grain boundaries are a mixture of dark ( phase) and
light-coloured phases ( phase). Fine and  lamellar structures are visible within the grains. A
colony of a lamellar microstructure, shown in Fig. 1(c), was produced by solution treatment and
furnace cooling. This microstructure has  phase on the grain boundaries resulting from complete
transformation of to  on the grain boundary. The grains consist of colonies of / lamellar
structures. The  laths are parallel plate-like structures having thin dark  regions sandwiched
between them. The  laths are thicker in the lamellar microstructure and thinner in a partially
transformed martensitic microstructure.

a) b) c)
Fig. 1. Optical micrographs of the Ti6Al4V alloy solution treated at 10500C for 30 minutes and
(a) water quenched (b) air cooled (c) furnace cooled.
196 Light Metals Technology 2015

The effect of solution treatment and cooling medium on the hardness of Ti6Al4V is shown in
Fig. 2. The fully martensite structure showed a higher hardness than a partially transformed
martensite (Ti6Al4V, AC) and a lamellar structure (Ti6Al4V4, FC).

Fig. 2. Micro-hardness (HV0.5) values of all samples solution treated for 30 minutes and water
quenched or air cooled or furnace cooled.
Fig. 3 (a), (b) and (c) show hardness indentations of the solution treated Ti6Al4V alloy cooled at
different rates after heat treatment. The fully martensitic sample (Fig. 3(a)) showed high hardness
values due to the presence of fine martensitic needles. The lamellar sample shown in Fig. 3(c)
showed the lowest hardness values due to the presence of thicker  laths. The partial martensitic
microstructure (Fig. 3 (b)) showed intermediate hardness values as the  laths are thinner than in
the lamellar microstructure.

a) b) c)
Fig. 3. Optical micrograph of microhardness indentations of Ti6Al4V alloy solution treated at
10500C for 30 minutes and (a) water quenched, (b) air cooled or (c) furnace cooled.

Ageing experiments were done on solution treated and water quenched samples due to the
consistent hardness values, i.e. the homogeneous structure that had been produced. Water
quenching from the solution treatment provides more degrees of freedom in optimising the
microstructure and mechanical properties than air cooling or furnace cooling during ageing
treatment [6]. This is because the water quenched microstructure can consist of ''' and
phases which would respond better during ageing [7]. The presence of fine martensitic needles in
solution treated and water quenched samples is desirable for a high ductility, high ultimate tensile
strength, and consistency in the microstructure as well as providing maximum response during
ageing [8].
The ageing at 500 to 7000C for 0.5 hours to 2 hours did not alter the microstructural morphology
of solution treated samples. Ageing by cooling medium of either water quenching or furnace
cooling left the microstructural morphology unchanged. The fully martensitic morphology
remained unchanged as shown in Fig. 4 (a).
 Materials Science Forum Vols. 828-829 197

a) b)
Fig. 4. Optical micrograph of the Ti6Al4V alloy solution treated at 10500C for 30 minutes, water
quenched, and aged at a) 7000C, b) 9000C for 30 minutes and furnace cooled

The ageing treatment at 800 to 9000C for 0.5 to 2 hours changed the microstructural morphology of
solution treated samples. The changed microstructure of aged Ti6Al4V at 9000C is shown in Fig.
4(b). The microstructure changed from fully martensitic to partial martensitic. At these
temperatures, which are close to the  transus temperature, phase transformation into  phase
would occur during the ageing heating cycle. Furnace cooling from the ageing temperature of
9000C would have the phase transforming back to the phase, leading to a partial martensitic
structure.

The effect of ageing temperature and time on the hardness of aged Ti6Al4V4 is shown in Fig. 5
while Fig. 6 shows the effect of ageing followed by different cooling media on the alloy’s hardness.

Fig. 5. Micro hardness (HV0.5) values of all samples solution treated for 30 minutes and water
quenched, and aged at different temperatures and times.
198 Light Metals Technology 2015

Fig. 6. Micro hardness (HV0.5) values of all samples solution treated for 30 minutes and water
quenched, as well as aged at different temperatures followed by different cooling media.

The general trend showed that the hardness increased during ageing at 6000C as shown in Figs. 5
and 6. The increase is shown relative to the hardness of solution treated Ti6Al4V alloy. The drop in
hardness starts to occur at an ageing temperature of 7000C and a time of 2 hours. This finding is
consistent with reports by Lütjering et al. [6], Mutombo et al. [7] and Lee et al. [9]. The authors
[6,7,9] report that fine crystals of Ti3Al or 2 form inside the  phase in Ti6Al4V alloy during
ageing up to 6250C. The 2 promote increased hardness values due to precipitation or an age
hardening mechanism. Above 6250C,  starts to convert to  until the  transus is reached where
the alloy is completely . Mutombo et al. [7] report the disappearance of the 2 phase above 6500C.
Ageing at temperatures of about 800 and 9000C gave lower hardness values. This was due to the
amount of martensite decreasing as the ageing temperature increased leading to a drop in hardness.
Martensite transforms to  and 2 phases as the temperature increases. At ageing temperatures of
800 to 9000C, the 2 phase is also no longer present and the volume fraction of martensite needles
has reduced, hence the hardness dropped.
Furnace cooling after ageing gave higher hardness values than water quenching at temperatures
of 500 to 8000C. Faster cooling after ageing such as a water quenching, does not provide sufficient
time for continuous 2 phase transformation to occur below 625oC, and formation of α-phase below
the β-transus causes age hardening. Donachie et al. [8] report that Ti3Al forms easier with furnace
cooling than air cooling which can explain why furnace cooling gave higher hardness values than
water quenching. The effect of ageing in the cooling medium was only investigated after ageing for
0.5 hours. At an ageing temperature of 9000C, water quenching after ageing gave higher hardness
values. Martensite forms during water quenching as some  phase has already formed at 9000C.
For all ageing temperatures, ageing times of 2 hours led to a drop in the hardness values. This
was due to the amount of martensite decreasing as the ageing time increased, leading to a drop in
hardness. The metastable  phase converts to a stable  phase which is known to have lower
hardness values. With longer ageing times, the volume fraction of martensite reduces and more 
forms, hence a reduction in hardness.

Conclusions
Furnace cooling after ageing of solution treated and water quenched Ti6Al4V, was found to
result in higher hardness values than water quenching. Lower ageing temperatures of 500 and
600 0C resulted in high hardness values above 370 HV0.5. Ageing at higher temperatures of
800 0C and 900 0C resulted in lower hardness values of below 370 HV0.5. At these temperatures,
which are close to the  transus temperature of Ti6Al4V alloy of 970 0C, the microstructural
 Materials Science Forum Vols. 828-829 199

morphology can change depending on the post-ageing cooling medium. Any further ageing
optimisation should be done at temperatures where the morphology does not change. These
temperatures were found to be between 500 and 700 0C. As ageing time increased from 0.5 to 2
hours, hardness decreased.

Acknowledgements
The authors would like to acknowledge the financial support of the South African Department of
Science and Technology (DST) as well as permission to publish from both the University of
Pretoria and the Council for Scientific and Industrial Research (CSIR).

References
[1] J. Cai, F. Li, T. Liu, B. Chen.. Investigation of mechanical behaviour of quenched Ti-6Al-4V
alloy by micro indentation, Journal of Materials Characterisation. 62 (2011) 287-293.
[2] L. Zeng, T.R. Bieler, Effects of working, heat treatment and ageing on microstructural evolution
and crystallographic texture of ''' and  phases in Ti-6Al-4V wire, Journal of Materials
Science and Engineering A. 392 (2005) 403-414.
[3] S.S. Youssef, K.M. Ibrahim, M.A Karim, Effect of heat treatment process on tribological
behaviour of Ti-6Al-4V alloy, Journal of Mechanical Engineering and Robotics Research. Vol. 2,
No 4 (2013) 385-394.
[4] R. Reda, A.A. Nofal, A.H.A. Hussein, Effect of quenching temperature on the mechanical
properties of cast Ti-6Al-4V alloy, Journal of Metallurgical Engineering. 2 (1) (2013) 48-54.
[5] M. Benedetti, V. Fontari, The role of bimodal and lamellar microstructures of Ti-6Al-4V on the
behaviour of fatigue cracks emanating from edge notches, Journal of Fatigue and Fracture of
Engineering Materials Structures. 27 (11) (2004) 1073-1089.
[6] G. Lütjering, J. Williams and A. Gysler, Microstructure and mechanical properties of titanium
alloys, Microstructure and Properties of Materials. 2 (2000) 1-74.
[7] K. Mutombo, C. Siyasiya, W. E. Stumpf, Dynamic globularization of phase in Ti6Al4V alloy
during hot compression, Materials Science forums. 783-786 (2014) 584-590.
[8] J. Donachie, J. Matthew, Titanium: A Technical Guide, 2nd Edition, ASM International, USA
(2000) 56-63.
[9] D. G. Lee, S. Lee, Effects of nano-sized 2(Ti3Al) particles on quasi-static and dynamic
deformation behavior of Ti-6Al-4V alloy with bimodal microstructure, Journal of Materials
Science. 40 (2005) 4077-4084.
Light Metals Technology 2015
10.4028/www.scientific.net/MSF.828-829

Effect of Ageing Treatment on the Microstructure and Hardness of the Ti6Al4V Alloy
10.4028/www.scientific.net/MSF.828-829.194

DOI References
[1] J. Cai, F. Li, T. Liu, B. Chen. Investigation of mechanical behaviour of quenched Ti-6Al-4V alloy by
micro indentation, Journal of Materials Characterisation. 62 (2011) 287-293.
10.1016/j.matchar.2011.01.011
[2] L. Zeng, T.R. Bieler, Effects of working, heat treatment and ageing on microstructural evolution and
crystallographic texture of ', and phases in Ti-6Al-4V wire, Journal of Materials Science and Engineering A.
392 (2005) 403-414.
10.1016/j.msea.2004.09.072
[3] S.S. Youssef, K.M. Ibrahim, M. A Karim, Effect of heat treatment process on tribological behaviour of
Ti-6Al-4V alloy, Journal of Mechanical Engineering and Robotics Research. Vol. 2, No 4 (2013) 385-394.
10.5897/jmer11.090
[4] R. Reda, A.A. Nofal, A.H.A. Hussein, Effect of quenching temperature on the mechanical properties of
cast Ti-6Al-4V alloy, Journal of Metallurgical Engineering. 2 (1) (2013) 48-54.
10.1007/s13632-013-0103-7
[5] M. Benedetti, V. Fontari, The role of bimodal and lamellar microstructures of Ti-6Al-4V on the behaviour
of fatigue cracks emanating from edge notches, Journal of Fatigue and Fracture of Engineering Materials
Structures. 27 (11) (2004) 1073-1089.
10.1111/j.1460-2695.2004.00825.x
[6] G. Lütjering, J. Williams and A. Gysler, Microstructure and mechanical properties of titanium alloys,
Microstructure and Properties of Materials. 2 (2000) 1-74.
10.1142/9789812793959_0001
[7] K. Mutombo, C. Siyasiya, W. E. Stumpf, Dynamic globularization of phase in Ti6Al4V alloy during hot
compression, Materials Science forums. 783-786 (2014) 584-590.
10.4028/www.scientific.net/msf.783-786.584
[8] J. Donachie, J. Matthew, Titanium: A Technical Guide, 2nd Edition, ASM International, USA (2000) 56-
63.
10.1002/9781118985960.meh105
[9] D. G. Lee, S. Lee, Effects of nano-sized 2(Ti3Al) particles on quasi-static and dynamic deformation
behavior of Ti-6Al-4V alloy with bimodal microstructure, Journal of Materials Science. 40 (2005) 4077-
4084.
10.1007/s10853-005-1914-y