M A TE RI A L S CH A RACT ER IZ A TI O N 62 ( 20 1 1 ) 2 8 7 –2 9 3

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Investigation of mechanical behavior of quenched Ti–6Al–4V

alloy by microindentation

Jun Cai⁎, Fuguo Li 1 , Taiyin Liu 2 , Bo Chen 2

School of Materials Science and Engineering, Northwestern Polytechnical University, Xi'an, China

AR TIC LE D ATA ABSTR ACT

Article history: This paper investigated the micro mechanical behavior of quenched Ti–6Al–4V alloy,
Received 7 October 2010 microindentation experiments were performed in a wide range of maximum loads: 200, 300,
Received in revised form 500, 700, 1000, 1500, 2000, 3000, 3500 and 4900 mN, and loading speeds: 10, 40 and 103 mN/s.
11 January 2011 The results revealed that loading speed had little influence on measurement of hardness
Accepted 12 January 2011 and Young's modulus. Microindentation hardness experiments showed strong indentation
size effects. Indentation hardness as well as Young's modulus decreased with the increase
Keywords: of indentation load. The decrease of Young's modulus was due to the damage of materials.
Ti–6Al–4V alloy The analysis of plastic behavior revealed that quenching temperatures had little effect on
Microindentation experiments strain hardening exponent n, but had significant influence on yield stress σy.
Quenching temperatures © 2011 Elsevier Inc. All rights reserved.
Mechanical behavior

1. Introduction
Since the early 1990s, microindentation or nanoindentation
hardness tests have been widely used to probe the
mechanical behavior of various materials, such as ductile
metals, brittle ceramics, and so on [1–6]. The main reason
for its ubiquitous use can be attributed to the ease and speed
with which they can be conducted, nondestructiveness, the
ease of testing under special conditions and offering the
possibility of greatly reducing the scale of the tests [7].
Compared with traditional experiments, the advantages of
microindentation test are obvious: firstly, the information
content of the measured data is much more than that of
classical tests; secondly, it is universal concerning materi-
als; and thirdly, the microindentation test can be performed
relatively easy at different temperatures and loading rates
[8,9].
Ti–6Al–4V alloy is one of the most important and widely used
titanium alloys in the aerospace industry, which has low
density and attractive mechanical and corrosion resistant
properties [10–12]. Therefore, great attention has been given in
the scientific literature to the investigation of the deformation
behavior of this alloy [13–19]. However, few investigators have
focused their research on the micro mechanical behavior of Ti–
6Al–4V alloy. This work aims to evaluate the effects of the
quenching temperatures on microindentation of Ti–6Al–4V
alloy. The rest of this paper is organized as follows. The
experimental procedure is introduced in Section 2. This is
followed by the analysis of micro hardness and Young's
modulus of specimens quenched at different temperature. In
Section 3.2, the indentation size effect on hardness and Young's
modulus is investigated. And the plastic behavior of Ti–6Al–4V
alloy using microindentation is developed in Section 3.3. The
paper concludes with a summary in the last section.

⁎ Corresponding author. Tel.: +86 2988474115; fax: +86 2988492642.

E-mail addresses: jeffreycai0116@gmail.com (J. Cai), fuguolx@nwpu.edu.cn (F. Li).
1
Tel.: +8602988474117; fax: +8602988492642.
2
Tel.: +8602988474115; fax: +8602988492642.

1044-5803/$ – see front matter © 2011 Elsevier Inc. All rights reserved.
doi:10.1016/j.matchar.2011.01.011
288 MA TE RI A L S CH A R A CT ER IZ A TI O N 62 ( 20 1 1 ) 2 8 7–2 9 3

using the methods suggested by Oliver and Pharr [20].

2. Experimental Procedure Unloading curve can be expressed by following equation:

Commercial Ti–6Al–4V alloy was used in the present investiga-
m

tion. The initial micrograph of as received Ti–6Al–4V alloy is P = B × h−hf ð1Þ
shown in Fig. 1. The microstructure of alloy consists of equiaxed
primary α grains (hexagonal close-packed) of about 10 um where B and m are fitting parameters, and hf is the residual
average diameter and intergranular β grains (body-centered depth after unloading.
cubic). The main chemical compositions (wt.%) were: 6.02Al, The elastic contact stiffness, S, is obtained by unloading
3.78V, 0.074O, 0.08Fe, 0.007 °C, 0.0082H and the bal. Ti. The slope at maximum indentation depth hm:
specimens were cylindrical, 8 mm diameter and 12 mm height.
The specimens were heated to 900, 925, 950 and 970 °C
respectively, and held for 1 h. Afterward, the samples were S=
dP
dh j h = hm


= m × B hm −hf
m−1
ð2Þ
quenched in water for effective cooling. Fig. 2 illustrates the
microstructure of Ti–6Al–4V alloy after quenching. The globular α
The contact depth hc can be estimated by the relation:
grains can be found in Fig. 2(a), which represents the primary α
phase did not undergo any phase transformation during the heat
Pm
treatment. The microstructure after water quenching from hc = hm −γ ð3Þ
S
925 °C shows a mixture of fine α grains and β phase with α plates
located inside and at β grain boundaries, as shown in Fig. 2(b).
where γ is tip-dependent geometry factor, which is equal to
Examples for almost fully martensitic microstructure with no
0.72 for a conical indenter, 0.75 for a Berkovich indenter and 1
primary α grains can be seen in Figs. 2(c) and (d).
for a flat cylindrical indenter [21]. And the hardness H of the
The sample was ground with sand paper, followed by
specimen can be expressed as:
carefully polishing 5 μm and 1 μm diamond to mirror finish. A
commercial Micro Compression Tester (MCT) type W501
equipped with a diamond Berkovich indenter was employed to Pmax
H= ð4Þ
perform the experiments. Load-displacement curves (P–h curves) A
were recorded with ten maximum loads of 200, 300, 500, 700,
where A is the contact area, which can be expressed as
1000, 1500, 2000, 3000, 3500 and 4900 mN respectively, using
following formula:
three loading speed of 10, 40 and 103 mN/s respectively. Each
test was repeated three times and the average values were
calculated automatically by MCT as the load and displacement. A = Kh2c ð5Þ

where K is a constant, whose value is 24.56 for a Berkovich

3. Results and Discussions indenter [22]. The Young's modulus E can be given by:

3.1. Micro Hardness and Young's Modulus  

 1 1−ν2i −1
E = 1−ν2 − ð6Þ
E* Ei
The typical P–h curves of quenched Ti–6Al–4V alloy (maximum
load of 4900 mN and loading speed of 40 mN/s) are shown in
rffiffiffiffiffiffi
Fig. 3. The hardness and Young's modulus can be obtained π S
E* = × pffiffiffiffi ð7Þ
from the maximum load Pm and the initial unloading slope 2β A

where E* is reduced modulus, β is a correction factor

associated with the indenter shape ranging from 1.0226 to
1.085, about 1.05 for a Berkovich indenter [21], ν is the Poisson's
ratio of the specimen (0.33 for Ti–6Al–4V alloy), Eiand νi are the
Young's modulus and the Poisson's ratios of the indenter,
respectively. Diamond indenter has an elastic modulus of
1141 GPa and Poisson's ratio of 0.07, respectively [23]. Fig. 4
illustrated the variation of micro hardness and Young's
modulus of specimen quenched at 950 °C. It can be seen
from Fig. 4 that the loading speed has little influence on results
of microindentation experiments. Therefore, loading speed
40 um/s was used in the following investigation.

3.2. Size Effect in Microindentation

As shown in Fig. 4, microindentation tests of quenched Ti–

Fig. 1 – Initial microstructure of the as received Ti–6Al–4V alloy. 6Al–4V alloy have shown strong indentation size effects, i.e.,
 M A TE RI A L S CH A RACT ER IZ A TI O N 62 ( 20 1 1 ) 2 8 7 –2 9 3
Fig. 2 – Microstructure of the Ti–6Al–4V alloy after quenching at different temperature (a) 900 °C, (b) 925 °C, (c) 950 °C, and (d) 970 °C.
the decrease of indentation hardness, as well as Young's
modulus, with the increase of indentation load or depth.
Based on the Taylor dislocation model and geometrically
necessary dislocations (GNDs) model underneath an indenter
tip, Nix and Gao [24] established the relation between the
microindentation hardness H and the indentation depth h:
H2 h*
=1+
H20 h
Fig. 3 – P–h curves of quenched Ti–6Al–4V alloy at maximum
load of 4900 mN and loading speed of 40 mN/s.
289
where H0 is the indentation hardness for a large indentation
depth, h* is a characteristic length on the order of microns that
depends on the properties of indented material and the
indenter angle. H0 and h* can be expressed by following
equations [23,24]:
pffiffiffi pffiffiffiffiffi
H0 = 3 3αμb ρs ð9Þ
ð8Þ
 2
81 1 μ
h* = 3
bα2 tan2 θ ð10Þ
2 f H0
where ρs is the density of statistically stored dislocations, μ is
the shear modulus, b is the Burgers vector (0.2388 nm for α
phase and 0.3230 nm for β phase [25,26]), α is a constant to be
taken as 0.3–0.5, f is a scaling factor depending on the material,
ranging from 0 to 3.5, and θ is the angle between the surface of
the indenter and the plane of the specimen surface whose
value is 19.7° for Berkovich indenter.
The influence of quenching temperature on micro hardness
of Ti–6Al–4V alloy is shown Fig. 5. It can be seen from Fig. 5(a)
that the quenching temperature played an important role on the
hardness. The micro hardness of quenched specimens is much
higher than that of unquenched one. This phenomenon is
supposed to be caused by a significantly higher dislocation
density [27], the occasional formation of twins [28], and
formation of martensite arising from rapid cooling [29].It can
290 MA TE RI A L S CH A R A CT ER IZ A TI O N 62 ( 20 1 1 ) 2 8 7–2 9 3

Fig. 4 – Influence of loading speed on (a) micro hardness and Fig. 5 – Influence of quenching temperature on hardness (a) H−h
(b) Young's modulus. and (b) H2 −h−1.

be found that the specimen shows the highest hardness at the where E0 is defined as initial Young's modulus of virgin material.
quenching temperature of 925 °C, followed by 950 °C. And If the damage variable D = 0, the material was free of damage, if
specimen quenched at 900 °C as well as 970 °C exhibit the D = 1, the material was broken [32]. Therefore, the measured
similar hardness. The corresponding microstructure to the Young's modulus E during the microindentation test at higher
highest hardness consists fully of aged β phase with very fine loads is lower than the nominal one. Lee and Welsch [34]
precipitations of α grains (Fig. 2(b), similar to the result of Ti–6Al– reported that the dynamic Young's modulus of Ti–6Al–4V alloy
4V ELI alloy by Venkatesh [30]), which cause the strengthening was a function of quenching temperature: the Young's modulus
effect, as report by Mayer [28]. However, other specimens show increased with the increasing of quenching temperature (above
course α phase (Fig. 2(a)) or few α phase (Fig. 2(c) and (d) 800 °C). However, the values of the Young's modulus at 900 °C
respectively) which led to the lower hardness. Meanwhile, Eq. (8) and 1000 °C were 110 GPa and 112 GPa respectively, which
predicts a linear relation between H2 and h−1, as shown in indicated that the quenching temperature had no significant
Fig. 5(b). The values of H0 and h* can be easily obtained from Fig. 5 influence on the Young's modulus. This report is in accordance
(b), shown in Table 1. with the results obtained by Fan [35], and in accordance with the
Fig. 6 showed the influence of quenching temperature on microindentation results at lower load (as illustrated in Fig. 6). It
Young's modulus. As shown in Fig. 4(b) and Fig. 6(a), the Young's
modulus E decreases rapidly with increasing of indentation
depth h. The variation of Young's modulus can be induced by
damage evolution, and the decrease of Young's modulus
Table 1 – Variation of H 0 and h* with quenching
denoted an increasing damage during the experiments [31,32]. temperature.
According to continuum damage mechanics (CDM), the damage
Quenching temperature H0(GPa) h*(um)
variable (D), characterizing the deterioration of the mechanical
properties of materials, can be described by Young's modulus 900 °C 3.8031 1.2036
[33]: 925 °C 4.0149 1.7122
950 °C 3.9506 1.2905
970 °C 3.9108 0.8579
D = 1− E= E0 ð11Þ
 M A TE RI A L S CH A RACT ER IZ A TI O N 62 ( 20 1 1 ) 2 8 7 –2 9 3 291

indenter loads, shown in Fig. 7. The stress–strain relation is

assumed to be the following formula:

8
< Eε;forσ ≤ σy 
n
σ= E ð13Þ
: σy 1 + εp ; forσ ≥ σy
σy

where n is the strain hardening exponent, σy is the initial yield

stress and εp is the nonlinear part of the total effective strain
accumulated beyond the yield strain.
A number of dimensionless material parameter set (E, ν, σy
and n) or (E, ν, σr and n) can be used to describe the constitutive
behavior, where σr is representative stress (defined at εp = εr,
where εr is a representative strain) [41]. For a Berkovich
indenter, the load P can be written as:

P = Pðh; E; v; Ei ; vi ; σr ; nÞ ð14Þ

This equation can be simplified to:

P = Pðh; E*; σ r ; nÞ ð15Þ

According to dimensional analysis, Eq. (14) can be changed

into:
 
E*
P = σr h2 Π1 ;n ð16Þ
σr

where Π1 is a dimensionless function. When εr=0.033 an

explicit functional form of Π1, independent of strain harden-
Fig. 6 – Influence of quenching temperature on Young's
ing exponent n, can be expressed as [41]:
modulus (b) lnE − lnh.
    3 "  #
E* E* E* 2
Π1 = −1:131 ln + 13:635
σ0:033 σ0:033 σ0:033
ð17Þ
 
can be seen in Fig. 6(a) that variation of Young's modulus versus E*
−30:594 + 29:267
the indenter distance is influenced by quenching temperature. σ0:033
When the indenter loads are higher than 500 mN (about 2.3 um
of the indenter displacement), the Young's modulus of speci- Similarly, the unloading slope can be written as:
men quenched at 970 °C is much lower than others, while the
variation of Young's modulus of specimens quenched at 900,
dPu dPu
925 and 950 °C are very similar. The data on variation on Young's = ðh; E*; σr ; nÞ ð18Þ
dh dh
modulus of quenched Ti–6Al–4V alloy during the compression
process are rather limited. Possibly, the localized deformation
[36–38] and shear bands [39,40] underneath the indenter cause
the difference of Young's modulus between 970 °C and other
quenching temperature. Further research needs to be done to
draw the firm conclusion. Meanwhile, lnE and lnh illustrate an
approximately linear relationship at the constant temperature,
as shown in Fig. 6(b).

3.3. Plastic Behavior

The loading curves are generally considered to follow Kick's

Law:

P = Ch2 ð12Þ

where C is the loading curvature which depends on material

properties. The C values decrease with the increase maximum Fig. 7 – Variable of C with maximum indenter loads.
292 MA TE RI A L S CH A R A CT ER IZ A TI O N 62 ( 20 1 1 ) 2 8 7–2 9 3

Dimensionless function at h = hm is:

 
dPu
dh j h = hm = S = E*hΠ2
E*
σr
;n ð19Þ

And Π2 can be written by [41]:

 
E* S
Π2 ;n = = ð−1:40557n3 + 0:77526n2 + 0:15830n−0:06831Þ
σr E*hm
  3
E*
 ln + ð17:93006n3 −9:22091n2 −2:37733n + 0:86295Þ
σ0:033
 2
E
 ln * + ð−79:99715n3 + 40:55620n2 + 9:00157n−2:54543Þ
σ0:033
  
E*

 ln + 122:65069n3 −63:88418n2 −9:58936n + 6:20045
σ0:033 Fig. 9 – Influence of quenching temperature with n and σy.
ð20Þ

Substituted values of C (obtained in Section 3.3), E *and S/hm

(obtained in Section 3.1) into Eqs. (17), (20) and (13), the values
of n and σy can be calculated. As shown in Fig. 8, the calculated
values of n and σy of specimen quenched at 900 °C remain
constants with the variation of indenter displacement,
denoting the values of n and σy calculated by Eqs. (20) and
(13) are correct. Therefore, the mean values at different loads
are taken as values of n and σy. Fig. 9 exhibits the variation of n
as well as σy with the quenching temperature. As shown in
Fig. 9, the n-values, ranging from 0.2618 (975 °C) to 0.2750
(900 °C), have no significant change with the quenching
temperature. However, the values of σy are seriously influ-
enced by quenching temperature. The water quenching heat
treatment leads to much higher yield strength because of the
formation of martensite arising from rapid cooling (about
825 MPa for water unquenched Ti–6Al–4V alloy [42]) [43–45].
Again, the highest value of σy subjected to quenching
temperature of 925 °C corresponds to the highest hardness
(as shown in Fig. 5), and this trend is also in agreement with
the results obtained by Zhang [29] and Venkatesh [30].
Meanwhile, the values of σy at 900 and 950 °C are in good
accordance with the compress test results of Meyer at the
strain rate of 0.01 s−1(1.12 GPa and 1.24 GPa respectively) [28].
4. Conclusions
Microindentation tests were performed on specimens of Ti–
6Al–4V alloy quenched at various temperatures using a
Berkovich indenter. Following are the conclusions:
(1) Variations of micro hardness and Young's modulus
were measured in this study. Loading speed has little
influence on measurement of hardness and Young's
modulus in microindentation experiments.
(2) Hardness as well as Young's modulus showed strong
indentation size effects during experiment. Quenching
temperature plays an important role on the hardness,
and the specimen had the highest hardness at the
quenched temperature of 925 °C. The Young's modulus
decreased rapidly with increasing of indentation depth,
which is due to the increasing damage of materials.
(3) The influence of quenching temperatures on strain
hardening exponent n was not obviously, while initial
yield stress σy was seriously affected by quenching
temperatures.

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