Characteristics Microstructure and Microhardness of Cast

Ti-6Al-4V ELI for Biomedical Application Submitted to

Solution Treatment

Damisih1,a), I Nyoman Jujur1, Joni Sah1, Agustanhakri1, and Djoko Hadi Prajitno2
1
Center of Technology for Materials, Agency for the Assessment and Application of Technology (BPPT), Puspiptek
Area, 224 Build, Tangerang Selatan, Banten 15314, Indonesia
2
Center for Applied Science and Technology, National Nuclear Energy Agency (BATAN), Jl. Tamansari 71,
Bandung 40132, Indonesia
a)
Corresponding author: damisih@bppt.go.id

Abstract.Ti 6Al-4V ELI (Extra Low Interstitial)alloy containing 6wt% of aluminum, 4wt% of vanadium with controlled
level of iron and oxygen is one of most popular alloy employed in biomedical applications as implant material. Heat
treatment process for titanium alloys becomes important and could be performed by some of different ways in order to
develop microstructure as well as its properties. The objective of this paper is to study the effects of solution treatment
temperature on microstructure and mechanical properties of as-cast Ti-6Al-4V ELI especially microhardness value. The
alloy was melted by single arc melting furnace with a water-cooled copper crucible hearth under argon atmosphere and
then casted. It was heat treated through solution treatment at 3 (three) different temperaturesi.e. 850oC, 950oC and
1050oC in an argon gas atmosphere for around 30 minutes. After solution treatment, samples were water quenched and
then aged at temperature of 500 oC for 4 hours. To investigate its microstructure, the alloy was investigated under optical
microscope and scanning electron microscope (SEM). It was observed Widmanstätten microstructure consisting of
mixture α and β phase with basket-weave pattern. The Vickers microhardness test was performed and the results
exhibited the optimum value was obtained at temperature of 950 oC of solution treatment. From the observation, it
revealed that the heat treatment has substantial effect on microstructural properties where microhardness increased due to
formation of αʹ martensite structure. It was showed also that solution treatment followed by aging could improve
mechanical properties especially microhardness value of Ti-6Al-4V ELI alloy. These results were suggesting the
optimized conditions of heat treatment to obtain the best microstructure properties and microhardness value.

INTRODUCTION
The use of titanium and its alloy have been widely employed in numerous range applications including
aerospace, chemical plants and biomedical industries due to its excellent properties [1]. Some main superior
characteristics of this alloys are high strength-to-weight ratio, high mechanical properties, relatively low elastic
modulus, good corrosion resistance and exceptional biocompatibility mainly when direct contact with tissue or bone
[2]. Especially Ti-6Al-4V ELI (Extra Low Interstitial)alloy where medium strength and good toughness are required
is becoming one of most popular alloy employed in biomedical applications as implant material. Chemical
composition of Ti-6Al-4V ELI alloys contains 6wt% of aluminum, 4wt% of vanadium with controlled level of iron
and oxygen as interstitial elements. Because of lower level of impurities, Ti-6Al-4V ELI alloys have better ductility
and fracture toughness compared with commercial Ti-6Al-4V [3]. In biomedical application, some utilizations of Ti-
6Al-4V ELI consist of hip and knee joints prosthesis, trauma fixation devices and dental implants [2].
Production of titanium casting was recently increased due to cost saving compared to forging as well as
machining method[4]. The use of net-shape or near-net-shape technology like casting receives much attention
considering large cost saving potential in manufacturing part of complex shape of implant. And due to high

Proceedings of the International Seminar on Metallurgy and Materials (ISMM2017)

AIP Conf. Proc. 1964, 020037-1–020037-8; https://doi.org/10.1063/1.5038319
Published by AIP Publishing. 978-0-7354-1669-7/$30.00

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reactivity of molten titanium, melting process should be carried out in vacuum condition to minimize oxidation.
However, cast titanium needs post treatment like heat treatmentto reduce some of casting defect, improve
mechanical properties and microstructure. Process parameters in heat treatment that mostly influence the alloy
properties include cooling temperature, cooling rate and cooling medium [5].
Ti-6Al-4V ELI is classified into α-β alloy so that it consists of mixture of α and β phases. The microstructure
showed variations on the morphological development of α and β phase depending on alloy composition, prior work
as well as heat treatment. The microstructure itself considerably affectedon the properties of Ti-6Al-4V alloy. It is
primarily described by the size, arrangement and volume fraction of the two phasesα and β [6].It can be substantially
changed by working and/or heat treating the alloys below or above beta transus temperature. In addition,
compositions, size, and distribution of alloy phase can be manipulated within certain limit. Therefore, the heat
treatment process of this alloy could be performed by some of different ways in order to develop microstructure as
well as properties. The most common used is solution treatment followed by aging. Heat treatment should be carried
out in either an inert gas atmosphere or vacuum to minimize oxidation reaction. Jovanović et al. reported that
annealing temperature have strong effect on the mechanical properties of Ti-6Al-4V as well as Ti-6Al-4V ELI
[7].Types of microstructure that are generally in Ti-6Al-4V including equi-axial, martensitic and Widmanstätten [8].
Ti-6Al-4V ELI alloys when heat-treated above the β transus are in single β phase. On cooling through β transition
temperature, β phase can transform to various equilibrium or non-equilibrium phases. It depends on the cooling rate
and alloying content where rapid cooling of β phase can transform to martensitically to αʹ or αʹʹ [9]. Moreover, β can
transform by nucleation and growth to Widmanstätten pattern of α phase [5].
In this work, the effects of solution treatment on microstructure and microhardness of as-cast Ti-6Al-4V ELI
were studied. Hardness is one of important engineering parameter of materials for implant applications. It is related
to tribological behaviour where the incidence of wear in implant materials decreases as hardness increases.
Furthermore, hardness is also associated with other properties such as toughness, modulus of elasticity and the yield
strength of metals. Because of its simplicity and swiftness operation, hardness test is widely used to characterize
metallic implant especially small size one.

MATERIALS AND METHODS

Ti-6Al-4V ELI rodwith diameter of around 1 cm (Fig. 1a) was used as starting materials subjected to melting
process at vacuum condition. For preparation, rod was cut into tiny pieces adjusting to small size of crucible. The
chemical composition of Ti-6Al-4V ELI could be seen in the Table 1 as follows:
TABLE 1. Chemical composition of the Ti-6AL-4V ELI alloy as starting materials (wt%)
Element Al V C Fe O N H Ti
Standard 5.5-6.5 3.5-4.9 <0.08 <0.25 <0.13 <0.05 0.012 Balance

Raw material 6.377 3.992 - 0.203 - - - 88.711

Single arc melting furnace coupled with water-cooled copper crucible hearth (Fig. 1b) was used to prepare Ti-
6Al-4V ELI ingot at laboratory scale. Using non-consumable electrode, melting was performed under ultra-high
purity (UHP) of argon gas which was kept continuously blowingupon melting process. The melt was led to solidify
at crucible and ingot with button shape was produced.

a b

FIGURE 1. Ti-6Al-4V ELI rod as raw materials was cut into small pieces (a) Single arc melting furnace used in this work (b)

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 After solidified, ingot was divided into three parts subjected to different temperatures of solution treatment for
around 30 minutes. The treatment was accomplished in an inert atmosphere of ultra-high purity argon gas. The
temperature variables of solution treatment were 850oC, 950oC and 1050oC. After solution treatment, samples were
fast cooled in water as quenching medium and then aged at temperature of 500 oC for 4 hours. The schematic
illustration of heat treatment in this work can be shown in Fig. 2 as follows:

FIGURE 2. Schematic illustration of heat treatment condition of Ti-6Al-4V ELI alloy

The samples were observed under optical microscope to investigate its microstructure. It was metallograpically
prepared by grinding, polishing and etching before observation. Samples were etched using Dix-Keller reagent
consisting of a mixture of nitric acid, hydrochloric acid and hydrofluoric acid. Scanning Electron Microscope (SEM,
Hitachi SU3500) was used for more detail observation. Elemental analysis and mapping element were also
performed to know compositional and distribution of each element Ti, Al and V by using Energy Dispersive X-Ray
(EDX, Horiba EMAX) coupled in SEM.The hardness value was determined using Vickers microhardness tester. It
was indented 3 (three) times and taken its average value.

RESULTS AND DISCUSSION

Figure 3 shows microstructure of Ti-6AL-4V ELI alloys in different conditions of solution treatment. It was
observed Widmanstätten microstructure consisting of mixture α and β phase. The α phase is shown by brighterarea
and  phase is demonstrated by darker region. The α phase exhibited lamellar structure and it was respectively
interconnected to form basket-weave. Between α phase lamellae, β phase plates were formed alternating each other.
The α phasecan be formed by the boundaries of the prior β grains and delimit it. This is in accordance with results
by previous researchers [10, 11].
Ti-6Al-4V ELI alloy is characterized by its sensitivity to microstructural change, so that the desired mechanical
properties could be adjusted by controlling microstructure through heat treatment. The properties of this alloy are
developed by relying on the refinement of the grains upon cooling from  region or α+ region and subsequent
aging at low temperature to decompose martensite formed upon quenching [5]. An important point for heat
treatment is -transus temperature since it separated single  phase becoming two phase of α+ [12]. It is described
as temperature when the microstructure is fully  phase which is about 980oC for this alloy.In this work, solution
treatment were performed at various temperature representing different region in phase diagram, above beta transus
temperature (1050oC), between beta transus temperature and martensitic start (Ms) temperature (950oC) and below
martensitic start (Ms) temperature (850oC).
Upon fast cooling, beta may be decomposed by martensite reaction and form Widmanstätten pattern [5]. In this
pattern, αphase is formed along prior βgrain boundaries, and colonies of lath‐type β and α lamellar structure are
present inside prior βgrains. The parallel plates of α delineated by β phase between them and formed microstructural
morphology consisting of these sets of parallel plates. The microstructure in Widmanstätten pattern is formed with a
crystallographic relationship to the phase from which it originated.
The presence of some beta in the structure due to the fact that the temperature for the end of the martensite
transformation (Mf) for this alloy is below room temperature [5]. Rapidly cooling the alloys through quench from β-

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phase leads the formation of hcp martensite and this is not particularly hard. The quantities of retained β phase will
increase as solute concentration increases and Mstemperature decreases.
Sridhar et al.have been studied effect solution treatment at different temperatures also[13]. Their studies revealed
that microstructure consisting equiaxed α and transformed β after solution treatment at 900 oC and 955oC, while a
fully transformed β structure was produced after solution treatment at temperature 1065oC. Water-quenched
specimen also showed martensite structure like as another.

a b

90 µm 90 µm

90 µm

FIGURE3. Microstructuresof Ti-6Al-4V ELI obtained by light optical microscope after heat treated at temperature of (a) 850oC
(b) 950oC (c) 1050oC (500X of magnification, using Dix-Keller reagent for etching)

It was reported that microstructure of as-quenched from 950oC consisted acircular αʹ martensite changed from β
phase with α and retained β [4]. And if followed by aging treatment, primary αʹ martensite transformed into
martensite. Jovanović’s work resulted that water quenching from all annealing temperature (1100oC, 950oC and
900oC) led to the formation of the primary αmartensite structure and its volume fraction decreased with decreasing
temperature. [7]. In addition, Venkatesh et al. described that after water quenching from 955oC and subsequent
aging at temperature of 525oC, the microstructure of Ti-6L-4V ELI consisted of primary α and αʹ+β[2].Meanwhile,
Pinke et al. study resulted microstructure of as-cast Ti-6Al-4V alloy showed structure consisting of equiaxed β
grains and various morphologies of α phase [10].
Youssef et al. performed solution treatment at different temperatures above and below the beta transus
temperature. It was rapidly cooled in water as quench medium and followed by aging. The results showed a fine
lamellar structure was formed when samples were water-quenched from 1050oC, while samples quenched from
800oC showed coarse lamellar structures [14]. Typically, Ti-6Al-4V microstructure contains very fine acicular α,
fine acicular α and β and prior β grain boundaries [11]. Microstructure of cast titanium alloys consists of lamellar
structure ofα and β. However, the morphology of α could change with heat treatment. From the picture in Fig. 3, it
can be seen also that at solution temperature of 950oC showed long and continuous α phase. Needle-like martensite
structure was clearly observed. In addition, at 1050oC, darker region indicating β phase was majorly formed.

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 Microstructures were examined more detail at higher magnification using Scanning Electron Microscope (SEM)
like shown in Fig. 4. Basket-weave structure was clearly observed at 850oC of solution temperature. The structure of
α phase lamellar is mutually connected forming regular network weave of pattern. Between the lamellae of α phase,
there were β phase plates formed alternating each other. SEM analysis was verified the results obtained by optical
microscope. It was also confirmed other researchers finding [5, 15].Meanwhile at 950oC of solution treatment, it is
shown relatively large and long platelet of α phase. It was likely continuous and long stick. At the end of α phase, it
seems that the structure was broken and forked at both of tips. It was slightly different with other researcher results
which mostly lamellar structure or basket-weave arrangement. However, it confirmed that α phase could present in
any different shapes and forms depending on the processing parameter and conditions. At temperature of 1050oC
solution treatment, it is seen lamellar of α phase growing at different orientation with grain boundary as border. By
the boundaries of the prior β grains phase α was formed which ″delimits″ these grains [10]. The lamellar pattern of α
phase was clearly observed in this temperature.

a b

FIGURE 4. Microstructures of Ti-6Al-4V ELI obtained by Scanning Electron Microscope (SEM) after heat treated at
temperature of (a) 850oC (b) 950oC (c) 1050oC (2500X of magnification, using Dix-Keller reagent for etching)

Figure 5 presents mapping image of each element in Ti-6Al-4V ELI for sample heat treatedat 950oC. It is noted
that distribution of aluminum element is denser inα phase at Fig. 5(c). Otherwise, vanadium element has lower
density in this phase. It was due to the fact that aluminum is α phase stabilizer while vanadium is stabilizer for β
phase [5, 6].

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 FIGURE 5. Mapping image of Ti-6Al-4V ELI obtained by Scanning Electron Microscope (SEM) after solution treated at
temperature of 950oC (a) distribution of mix elements (b) distribution of Ti (c) distribution of Al (d) distribution of V

Venkatesh et al. studied Ti-6Al-4V alloy subjected to water quenching at temperature given followed by aging
exhibited higher value, while as-cast specimen had lowest value of hardness [2]. It indicated that water quenching
somewhat increased hardness value. Similarly, Jovanović et al. reported hardness increased with the increase of
annealing temperature and upon water-quenching showed the highest value compared air as well as furnace cooling
[7].However, hardness reached saturation after 1050oC and formed plateau until 1100oC.
In this work, hardness increased from 386 HVN at 850oC to 452 HV at 950oC of solution treatment temperature
and then slightly decreased to 435 HV at 1050oC. The increase of hardness value was due to formation of αʹ
martensite [16]. It can be concluded here that the optimum value was obtained at temperature of 950 oC of solution
treatment. It was noted that solution treatment through water-quenching followed by aging could improve
mechanical properties of Ti-6Al-4V ELI alloy. These results were suggesting the optimized conditions of heat
treatment to obtain the best microstructure properties and hardness value. And it could be a recommendation to be
used at titanium implant industry. In general, hardness increases as the rate of cooling increases due to the formation
of martensite arising from fast cooling [2]. Unlike the martensite in steel which leads strong distortion to the crystal
lattice and significantly increase hardness and strength, it is known that hardening effect due to martensitic
transformation in Ti-6Al-4V ELI is only moderate [12].Pinke et al. reported significant increase of hardness when it
was rapidly cooled in water for Ti-6Al-4V alloy. It increased again after aging at 550oC for 4 hours which the
highest value obtained was 428 HVN at 1050oC of solution treatment temperature [10].
The increase of hardness also might be due to formation of α case layer that was formed at surface but not
significant because samples were prepared by grinding and polishing. Hardness value could be likewise related with
Al-equivalent. There is Al-equivalent value which indicates the capacity of alloy to obtain a given hardness [6]. At

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higher temperature of solution treatment of 950oC, aluminum content would be more dissolved if compared to the
lower solution of 850oC. Then, dissolved aluminum precipitated at α phase as it was considering as α stabilizer.
Consequently, it led the increase of hardness value due to high amount of α precipitate. However, it reached
optimum point and got saturated so that hardness slightly decreased at 1050oC of solution temperature.

500 TABLE 2. Vickers hardness value of Ti-6Al-4V ELI

Vickers Hardness (HVN)

after heat treated at different temperature of solution

treatment
450

Temperature of
400 Solution 850oC 950oC 1050oC
Treatment

350

300 Vickers Hardness

800 850 900 950 1000 1050 1100 386 452 435
(HVN)
Solution Temperature (oC)

FIGURE 6. Graph of Vickers hardness of Ti-6Al-4V

ELI after heat treated at different temperature of solution
treatment

Hardness is included to one of prime important properties of materials for biomedical application[17]. It is
related with surface tribological properties and used to find suitability of clinical use of biomaterials. Hardness
measurement was subtantial particularly when combining various materials for bearing or wear conditions. For
biomaterials application, it is desirable that Ti-6Al-4V ELI hardness is similar to bone hardness. However, the
fundamental disadvantages of titanium and its alloys include poor fretting fatigue resistance and poor tribological
properties due to its low hardness [18]. Some developments have been done to improve hardness such as surface
treatment, thermo-mechanical process and heat treatment. From the results of this works, it was suggested that
solution heat treatment and then water quenched followed by aging is beneficial for increasing hardness of Ti-6Al-
4V ELI and expecting to enhance its wear resistance.

CONCLUSIONS
The microstructure observation by optical microscope, SEM analysis and microhardness testingwas performed
on Ti-6Al-4V ELI alloy under different temperatures of solution treatment. And the results were concluded as
follows:
 The microstructure observed by optical microscope and SEM indicated different microstructure at different
temperatures of solution treatment. It was observed Widmanstättenmicrostructure consisting of mixture α and β
phase with basket-weave pattern.
 Elemental mapping distribution showed that the distribution of aluminum element was denser in α phase but
vanadium has lower density due to the fact aluminum is α stabilizer.
 Vickers microhardness value increased as temperature of solution treatment increaseddue to formation of αʹ
martensiteuntil reach optimized condition.
 The optimum value of microhardness was obtained at solution treatment temperature of 950oC which was 452
HVN.
These results suggested the optimized conditions of heat treatment to obtain the best microstructure properties
and hardness value. And it could be a recommendation to be used at titanium implant industry.

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