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Dong 2013
Dong 2013
art ic l e i nf o a b s t r a c t
Article history: In order to investigate four typical morphologies of α phase, including Platelet α, α case, Equiaxed α, and
Received 7 April 2013 Martensite α, microindentation tests of Ti–6Al–4V under different heat treatment conditions were
Accepted 6 May 2013 performed with various indentation loads from 50 mN to 4900 mN and two loading speeds of
Available online 21 May 2013
9.6841 mN/s and 103.7053 mN/s by a sharp Berkovich indenter. The microhardness H, young's modulus
Keywords: E, initial yield stress sy and strain hardening exponent n were obtained by means of Oliver–Pharr method
Ti–6Al–4V alloy and reverse analysis algorithms. The results show that H of four typical morphologies decreases with the
Alpha phase increase of indentation load. When loads are above around 2000 mN, H of Equiaxed α is the largest.
Morphology However, when loads fall down below 450 mN, H of α case is the largest. This phenomenon can be
Microindentation experiments n
explained by indentation size effects (ISE) and degree of ISE can be indicated by variable hH . E of four
typical morphologies also decreases with the increase of indentation load, which can be explained by
damage during indentation. Among four morphologies, damage could be easily generated and spread
within Equiaxed α. But it is difficult for α case. Moreover, sy and n remain constant with different loads in
four morphologies. The working hardening effect becomes weaker as n becomes larger.
& 2013 Elsevier B.V. All rights reserved.
1. Introduction working [16] have been studied. Although many researchers have
investigated the microstructural and mechanical behaviors of Ti–
Recently, with the development of material producing, the 6Al–4V alloy under different hot working conditions [17–22],
dimensions of new material and device become smaller and it researches on morphology of α phase have been rarely done.
has been found that there are some differences in mechanical It is well known that different microstructures can be obtained
behaviors between micromechanical and macromechanical levels. under different processing technology and subsequent heat treat-
It is difficult for the conventional testing methods to measure the ment. These microstructures are made up of α phase displayed in
micromechanical properties of nano-materials. Therefore, micro- various morphologies and β phase used as matrix. The properties
indentation and nanoindentation tests have been widely used to of α phase and β phase and their volume fraction mainly influ-
probe the micromechanical behavior of various materials at small enced by the chemical compositions and microstructures are
scales, such as CuAlNi shape memory alloy [1], Ti–6Al–4V alloy closely related to mechanical properties [23], so it can be inferred
[2,3], aluminum [4], copper [5], composite [6] and other materials that the morphologies of α phase are important to improve the
[7–10]. The microindentation or nanoindentation test provides properties of Ti–6Al–4V alloy. A clear scientific understanding on
precise measurement and has advantages of celerity, accuracy, and morphology of α phase is necessary.
nondestructiveness [3], which determines and contributes to its This work aims to investigate micromechanical behavior of
increasing popularity in the future. different morphologies of α phase and provide evidence of the
As a two phase alloy, Ti–6Al–4V alloy is one of the most coming study on materials in a smaller scale. Meanwhile, results of
important titanium alloys in aerospace industries, due to its low this study can provide reference to performance design of titanium
density and attractive mechanical and corrosion resistant proper- alloys, organizing computing, and hot working technology as well.
ties [11–13]. Many aspects of Ti–6Al–4V, including the superplastic
deformation ability [14], the influence of α platelet on plastic
flowing [15], and the microstructural mechanisms during hot 2. Experimental procedure
0921-5093/$ - see front matter & 2013 Elsevier B.V. All rights reserved.
http://dx.doi.org/10.1016/j.msea.2013.05.032
106 J. Dong et al. / Materials Science & Engineering A 580 (2013) 105–113
Table 1 According to the Oliver and Pharr's model [26,27], the unload-
Chemical composition of as-received Ti–6Al–4V billet. ing curve can be described as
Main component (wt%) Impurities (wt%) P ¼ B ðh−hf Þm ð2Þ
microstructure of initial specimens consisted of equiaxed primary where β is a indenter constant (1.05 for Berkovich indenter [30]).
α grains (hexagonal close-packed) of about 10 μm average dia- The relationship between En and Young's modulus E is given as
meter and intergranular β grains. Managed as the heat treatment following:
conditions in Table 2, the specimens were carefully ground with −1
1 1−νi 2
sand paper. Then, they were polished with 5 μm and 1 μm E ¼ ð1−ν2 Þ n − ð8Þ
E Ei
diamond to mirror finish. Subsequently, the specimens were
etched with Kroll's Reagent (1HF, 9HCl, and 90H2O) for 5 s to where ν is Poisson's ratio to be taken as 0.33 for Ti–6Al–4V alloy. Ei
reduce the influence of surface hardening and observed by and νi are Young's modulus and Poisson's ratio of the indenter
OLYMPUS PM3 optical microscope. Finally, microindentation whose values are 1141 GPa and 0.07 for diamond indenter,
experiments were performed using the commercial MCT W501 respectively [31].
equipped with a Berkovich diamond indenter at room tempera-
ture under the laboratory environment. Some researchers [24,25] 3.2. Yield stress sy and strain hardening component n
had proved that loading speed exerted little influence on mea-
surement of Young's modulus E and microhardness H. Microin- The behavior of Ti–6Al–4V alloy under room temperature
dentation experiments of this work were only performed with two follows Power law elasto–plastic stress–strain principle:
loading speeds (low loads ( o450 mN) at 9.6841 mN/s and high (
loads at 103.7053 mN/s, respectively). And maximum loads con- Eε; f or s ≤sy
s¼ ð9Þ
ducted on specimens were as following: 50, 100, 150, 200, 250, Rεn ; f or s 4 sy
300, 350, 400, 450, 700, 1000, 1500, 2000, 3000, 3500, 4500, 4600,
where R is a strength coefficient, n is the strain hardening
4700, 4800 and 4900 mN. Notably, each test was conducted five
exponent, sy is the initial yield stress, ε is the strain. The elasto–
times and the average values were calculated in order to eliminate
plastic stress–strain relation equation is shown in Fig. 3.
the errors.
εr is the strain that excesses yield strain εy. So, Eq. (9) can be
rewritten as
(
3. Calculation methods Eε; for s ≤sy
s ¼ s ð1 þ E ε Þn ; for s 4 s ð10Þ
y sy r y
3.1. Young's modulus E and microhardness H
Presently, Cheng and Cheng [33,34] and Tunvisut et al. [35]
A typical P–h curve in instrumented indentation test is shown in proposed dimensional analysis to obtain sy and n. For a Berkovich
Fig. 2. Two important parameters (the maximum indentation depth indenter, the equation of P is [36]:
hm and the maximum load Pmax) can be obtained from P–h curve.
P ¼ Pðh; E; v; Ei ; vi ; sc ; nÞ ð11Þ
According to Kick's law, the loading curve can be expressed as
2 where sc is the representative stress corresponding the represen-
P ¼ Ch ð1Þ
tative strain εc.
where P is the indenter load, h is the indenter displacement and C is a The equation can be simplified by introducing En as
variable depending on the elastic–plastic material properties as well
as indenter geometry. P ¼ Pðh; En ; sc ; nÞ ð12Þ
J. Dong et al. / Materials Science & Engineering A 580 (2013) 105–113 107
Table 2
Heat treatment and corresponding microstructure.
Fig. 4. (a) Platelet α, (b) α case, (c) Equiaxed α and (d) Martensite α (α prime).
4.2.1. Microhardness
It is well known that four different hardening mechanisms
exist in metallic materials and are present in titanium alloys: solid
solution hardening, dislocation hardening, boundary hardening,
and precipitation hardening. In this paper, indentations were
performed exactly within α phase, so only dislocation hardening
mechanism contributes to H. Generally, the nature of plastic
deformation is the movement of dislocation, which can be divided
into two parts: Statistically Stored Dislocations (SSDs) and Geo-
metrically Necessary Dislocations (GNDs). In the micro scales, SSDs
are randomly located and their slip results in even plastic
deformation. While GNDs are arranged periodically and regularly,
causing strong obstacles to slip. Strain gradient plasticity model
believes that a large strain gradient is generated in indentation,
causing large amount of GNDs and inhomogeneous plastic defor-
mation. GNDs have a strengthening effect on hardness and
enhance in duration of material [37]. Indentation size effects
(ISE) caused by GNDs eventually appears.
In order to describe the ISE of materials accurately, Nix and Gao Fig. 5. P–h curves of Equiaxed α.
n
Fig. 8. hH of four typical morphologies.
Fig. 6. H of four typical morphologies.
By plugging Eq. (26) into the Eqs. (24) and (25), they can be
rewritten:
H 0 ¼ 3sref εN
eq ð27Þ
qffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
H ¼ 3sref ε2N
eq þ lη ð28Þ
By plugging Eqs. (21) and (23) into (29), it can be rewritten as:
sffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
H 3l tan 2 θ
Fig. 10. Density of dislocation ρ of four typical morphologies. ¼ 1þ ð30Þ
H0 2hε2N eq
n 3l tan 2 θ
hH ¼ ð31Þ
2ε2N
eq
n
Therefore, it can be concluded that hH can be used to describe
ISE and the hardening effect caused by ISE is more obvious, if value
n
of hH is higher.
Fig. 12. E of four typical morphologies. Fig. 13. Values of E under 50 mN and 4500 mN of four typical morphologies.
5. Conclusions
Acknowledgments
The authors would like to express their sincere thanks for the
research grants supported by the National Natural Science Foun-
dation of China (Grant no. 51275414) and the Aeronautical Science
Foundation of China (Grant no. 2011ZE53059).
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