Materials Science and Engineering A 489 (2008) 5561

Microstructures and mechanical properties of

Ti45Al8.5Nb(W,B,Y) alloy by SPSHIP route
Y.H. Wang a , J.P. Lin a, , Y.H. He b , Y.L. Wang a , G.L. Chen a
a

State Key Laboratory for Advanced Metals and Materials, University of Science and Technology Beijing, Beijing 100083, PR China
b State Key Laboratory for Powder Metallurgy, Central South University, Changsha 410083, PR China
Received 25 July 2007; received in revised form 28 November 2007; accepted 4 January 2008

Abstract
Microstructures and compression properties of Ti45Al8.5Nb(W,B,Y) alloy consolidated by spark plasma sintering (SPS) and hot isostatic
pressing (HIP) were investigated. The results showed that sintering temperature has a significant effect on microstructure. When the sintering
temperature is 1000 C, the dendritic microstructure of as-SPS alloy is similar to that of the alloying powder. At 1100 C, the interfaces of these
powder particles are still discernible, but near microstructure appear in every particle. A typical fully lamellar (FL) microstructure followed
by two types of microsegregations, such as -segregation and -segregation, is successfully developed at 1200 C. However, FL microstructure
becomes coarser at 1300 C. As-HIP alloy has near lamellar (NL) microstructure along with -segregation. The morphologies of phase in as-HIP
alloy are different from those in as-SPS alloy. The alloy exhibits excellent compression properties at elevated temperatures. When compression
temperature is higher than 1100 C, high quality compressed samples without cracks can be obtained even if engineering compression strain is up
to 80% for the strain rates of 1 101 to 103 S1 .
2008 Elsevier B.V. All rights reserved.
Keywords: TiAl based alloy; Microstructure; Microsegregation; Compression properties

1. Introduction
High Nb containing TiAl alloys are thought to be the potential lightweight high temperature structural materials due to their
low densities, high melting points, good elevated temperature
strengths and environmental resistances [13]. The major problem limiting the practical application of those alloys is their
poor ductility and formability. Those alloys reported so far are
mostly fabricated by ingot metallurgy (IM) [46]. However, IM
process of high Nb containing TiAl alloy is usually difficult due
to their relatively high melting point and the extreme reactivity of Ti. Recently, powder metallurgy (PM) technique appears
to be more attractive since high degrees of chemical homogeneities can be obtained and macrosegregations are avoided.
PM process consists of elemental powder metallurgy (EPM)
and alloying powder metallurgy (APM). EPM TiAl-based alloys
have drawn intensive attention because of its low cost and convenient addition of alloy elements [79]. However, concentrations

Corresponding author. Tel.: +86 10 62332192; fax: +86 10 62332508.

E-mail address: linjunpin@skl.ustb.edu.cn (J.P. Lin).

0921-5093/$ see front matter 2008 Elsevier B.V. All rights reserved.
doi:10.1016/j.msea.2008.01.031

of impurities such as oxygen and carbon are relatively high,

reducing the mechanical properties. Therefore, numerous works
have been conducted on the microstructures and properties of
APM TiAl-based alloys [1012]. In this study, microstructures
and compression properties of high Nb containing TiAl alloys
consolidated in spark plasma sintering (SPS) 1050 furnace and
HIP treatment were investigated in detail.
2. Experimental
Ti45Al8.5Nb(W,B,Y) (at.%) alloying powders were produced by argon atomization process, and then were classified
by Thaler sieve. The mean particle size of the alloying powders adopted in this study was less than 74 m. SPS furnace
was employed to sinter and concurrently consolidate the alloying powders for 10 min under 40 MPa at 1000, 1100, 1200 and
1300 C, respectively. The alloying powders were filled into a
graphite mold with two graphite punches pressed at both ends
and dense compacts of 30 mm 15 mm were obtained. Subsequently, HIP of the alloy sintered at 1200 C was performed at
1200 C/200 MPa/4 h to homogenize microstructure and eliminate porosity.

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Y.H. Wang et al. / Materials Science and Engineering A 489 (2008) 5561

The concentrations of gas elements such as oxygen and

nitrogen in the alloying powders and as-SPS alloys were analyzed with the inert gas melting-IR absorption spectrometry. The
concentration of carbon was measured by high frequency-IR
absorption.
The final densities of these alloys were measured through
Archimedes method. X-ray diffraction (XRD) analysis was
conducted using Cu K radiation to examine the phase transformation. Microstructural observation was carried out by scanning
electron microscopy using back scattering electron (BSE) imaging and energy dispersive spectroscopy (EDS). Lamellar spacing
was determined by transmission electron microscopy (TEM).
The lamellar spacing given in this paper was arithmetic average value measured without taking account of types of lamellar
boundaries. TEM foils were prepared by twin jet electropolished in a solution of 60% (vol.%) methanol, 35% butyl
alcohol and 5% perchloric acid at 15 V and 30 C. The
lamellar colony size was determined by the intersection linear
method.
Compression tests were conducted using a hot simulator
modeling Gleeble-1500 at 25, 600, 900, 1000, 1100, 1200 and
1250 C in air and the strain rate of 1 101 to 103 S1 . The

Table 1
Impurities concentrations in adopted alloying powders and as-SPS alloys
Impurities

Alloying powders (ppm)

SPS alloy (ppm)

1150
1170

140
145

24
35

samples were prepared by electric discharge machining in a form

of column with gauge size of 8 mm 12 mm from as-HIP
alloys, and then polished.
3. Results
3.1. Microstructure of as-SPS Ti45Al8.5Nb(W,B,Y)
alloy
Relative densities of >99.5% were achieved in as-SPS samples when sintering temperature is higher than 1100 C. Table 1
shows the impurities concentrations in the alloying powders and
as-SPS alloys. It indicates that the oxygen and nitrogen concentrations slightly increase, but carbon concentration rapidly
increases. This is correlated with the characteristics of SPS pro-

Fig. 1. Microstructures of Ti45Al8.5Nb(W,B,Y) sintered at the different temperatures: (a) 1000 C; (b) 1100 C; (c) 1200 C; (d) 1300 C.

Y.H. Wang et al. / Materials Science and Engineering A 489 (2008) 5561

57

Table 2
EDS analysis in Fig. 2(a)
Phase

Ti

Al

phase
Borides
Y2 O3

58.66
18.79
13.50

29.43
11.22
4.54

Nb
11.79
6.01

W
0.12
0.10

63.88

35.24

46.72

cess, such as the high heating rate, the rapid cooling rate and the
adoption of graphite mould.
The microstructures formed during SPS process were found
to dramatically change with the increase of sintering temperature, as shown in Fig. 1. Alloying powders are deformed
and bonded, but the interfaces of these particles are very evident at 1000 C (Fig. 1a). The sintered alloy has the dendritic
microstructure, which is similar to the microstructure of the
alloying powder [12]. It was also found that a small amount
of pores exist at prior particle boundaries. When sintering
temperature is up to 1100 C, the interfaces of these particles are still discernible, but a near microstructure with
equiaxed grain size of 6 m appears. It also contains small
amounts of 2 and phases, the latter appearing light gray
and white in BSESEM imaging, respectively (Fig. 1b). A
typical FL microstructure containing fine and homogeneous
lamellar colonies 2 / is successfully developed at 1200 C.
The average lamellar colony size is about 27 m and the
width of lamellae and that of lamellae is about 210 and
270 nm, respectively (Fig. 1c). In addition, it can be seen
that there are composition segregations in the FL microstructure from BSESEM micrographs. However, FL microstructure
becomes coarser at 1300 C (Fig. 1d). Therefore, it can be
deduced that the sintering temperature has significant effect on
microstructure, and 1200 C is an appropriate sintering temperature to fabricate high Nb containing TiAl alloys with FL
microstructure consisting of fine and homogeneous 2 / lamellar colonies.
Fig. 2 shows the microsegregations in as-SPS alloys. The
EDS analysis was performed to identify the microsegregations, as shown in Table 2. It suggests that the light reticulate
phases are ; the light particulate or bar phases are borides
and the lightest particles are Y2 O3 . It was found that
phase is the main microsegregation except for B-segregation
(borides) and Y-segregation (Y2 O3 ) in SPS microstructures
(Fig. 2a). However, phase cannot be detected in the XRD
pattern of the ingot because of its lower content (Fig. 3).
High magnification SEMBSE image reveals that phase
can be classified two different types of segregations in fact
[13]. The one is the -segregation at the boundary and triple
junctions among a grain due to the phase transformation of
; the other is the -segregation that forms local lamellar
structure composed of , and plates due to phase transformation of 2 + + . Closer examination of borides
in deeply etched sample reveals that they are needles or rods
smaller than 15 m (Fig. 2b and c). Y2 O3 particles are precipitated at the grain boundary, and their content is considerately
low.

Fig. 2. Microsegregations in as-SPS alloys: (a) -segregation and -segregation;

(b) and (c) rod borides; (d) borides (section image).

3.2. Microstructure of as-HIP Ti45Al8.5Nb(W,B,Y)

alloy
Fig. 4 shows the microstructure of as-HIP
Ti45Al8.5Nb(W,B,Y) alloy. It indicates that as-HIP
alloy has near lamellar (NL) microstructure along with -

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Y.H. Wang et al. / Materials Science and Engineering A 489 (2008) 5561

Fig. 3. XRD patterns of Ti45Al8.5Nb(W,B,Y) alloy sintered at 1200 C.

segregations (Fig. 4a). After HIP treatment, lamellar colonies

sizes slightly increase to 34 m and the length of borides does
not basically change (Fig. 4b). However, a few finer equiaxed
grains, about 5% volume fraction, form at the boundaries
of lamellar colonies. The morphologies of phase in as-HIP
alloy are different from those in as-SPS alloy. Most of phase
(-segregation) is blocky and located at the boundaries of
lamellar colonies, and phase (-segregation) located in the
lamellar colonies are hardly observed.
3.3. Mechanical properties of as-HIP Ti45Al
8.5Nb(W,B,Y) alloy

Fig. 4. Microstructures of Ti45Al8.5Nb(W,B,Y) alloy after HIP treatment:

(a) NL microstructure and -segregations and (b) borides.

The compression experiment was carried out from 25 to

1250 C with three different strain rates. Table 3 is the deformation results of Ti45Al8.5Nb(W,B,Y) alloy. It indicates
that external cracks are found for the samples deformed to
50% engineering compression strain below 1100 C with the
strain rate of 1 101 S1 . It is worth noting that there are
external cracks for one sample and no crack for two samples when the three samples were compressed at 1000 C
with the strain rate of 1 102 S1 . However, external cracks
take place below 1000 C for the strain rate of 1 103 S1 .
Therefore, high quality compressed samples without cracks
can be obtained even if engineering compression strain is up
to 80% at higher temperature (1100 C) for the three strain
rates.

The excellent compression properties at elevated temperatures for Ti45Al8.5Nb(W,B,Y) alloy are followed as Fig. 5.
The flow stress decreases and the shape of the true stress ()true
strain () curves changes with the increase of compression temperature. At 11001250 C, the curves have a characteristic
maximum at the initial stage of the deformation. As the degree
of the deformation increases, the flow stress decreases and a
steady stage of flow takes place. However, the flow stress grows
with increasing compression rate at the same temperature, but
the shape of the curves slightly changes. After the initial
stage, three is no work hardening, showing the alloy has good
hot workability.

Table 3
Deformation results of Ti45Al8.5Nb(W,B,Y) alloy
Temperature ( C)
Strain
rate
(s1 )

1 101

1 102
1 103

Note: (+) with crack; () without crack.

25

600

900

1000

1100

1150

1200

1250

+
+
+

+
+
+

+
+
+

+
+/

Y.H. Wang et al. / Materials Science and Engineering A 489 (2008) 5561

59

Fig. 5. The curves between the true stress and the true strain at different temperatures for alloy: (a) 1 101 S1 ; (b) 1 102 S1 ; (c) 1 103 S1 .

4. Discussion
4.1. Effect of sintering temperature on microstructure
During SPS process, the dendritic structures of alloying powders were removed with increasing the sintering temperature. At
1100 C, a small amount of 2 phase is formed, which is related
with two transformation mechanisms: (i) phase nucleates and
grows at the grain boundaries during the phase transformation of + + 2 and (ii) particles, formed at
grain boundaries in the course of prior powder consolidation,
grow into 2 during SPS treatment. When sintering temperature increases up to 1200 C, FL microstructure similar to
that of ingot forms in terms of
 a strict
 orientation
 relationship: {1 1 1}g //(0 0 0 1)2 and 1 1 0 g // 1 1 2 0 [14], but
2
the lamellar colony size is smaller. The lamellar microstructure
are probably defined by: + 2 + lamellar(2 /)
transformations [15]. However, the effect of SPS temperature
on the lamellar characteristics is not yet clear. It has been
proposed that the eutectoid transformation of 2 + is
diffusion-controlled by the interface reaction that involves uni-

form atomic detachment or a screw dislocation mechanism [15].

FL microstructure coarsening happens at 1300 C, which is not
favorable to controlling microstructure and leads to the difficulty
in the grain boundary gliding and dislocation movement.
The formation of 2 / lamellar structures in as-SPS alloys
is different from that in ingot. Generally, it is a solidification
process for the ingot. However, the microstructural evolution in
as-SPS alloys is a diffusion-controlled phase transformations,
i.e. + 2 + lamellar(2 /). In other words, the
eutectoid transformation 2 + followed by the precipitation from 2 phase takes place, which leads to the formation of
2 / lamellar structure. It must be noted that the transformation
2 + will proceed if the sintering temperature is higher
than 1100 C. It can be deduced that the ordering transformation of to 2 is incomplete when the sintering temperature is
up to 1200 C because of the rapid heating rate of SPS process.
Thus, the transformation will be complete if the holding time
at the highest sintering temperature is extended. The decomposition of 2 2 + , later forms lamellar structure, completes
during cooling from sintering temperature. During subsequent
cooling, the growths of lamellar colonies are restrained each

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Y.H. Wang et al. / Materials Science and Engineering A 489 (2008) 5561

other owing to their excessive number. As a result, the lamellar

colony size is finer when the holding time is 10 min. Moreover,
the ordering transformation of also improves the homogenous
precipitation and distribution of phase.
For SPS process, the lamellar colony forms when sintering
temperature increases to 1200 C. At the same time, the interdendritic regions containing the higher Al content in alloying
powders were melted due to SPS characteristics. As well known
that SPS process is an activating sintering by discharging effect
between particles. The interior temperature is approximately
200 C higher than the programmed, as the temperature of the
mold was controlled [15,16]. During solidification, phase (segregation) as the first solidified phase becomes richer in Nb
and W. However, the volume fraction of phase is small due
to the lower concentrations of Nb and W in the interdendritic
region. Subsequently, phase transforms to . However, the
transformation of to , which later transformed to lamellar
colony, is incomplete because the cooling rate is often too rapid
to completely eliminate differences in composition by diffusion.
During further cooling, very fine phase (-segregation) precipitates from 2 and locates in the lamellar colonies. Lamellar
colonies and phase simultaneously grow up, but the growth
rate of lamellar colonies is faster than that of phase due to the
low diffusivities of Nb and W. Finally, lamellar colonies except
for -segregation and -segregation are formed.
As is well known that B addition is beneficial to refining grain
for TiAl-based alloys [17,18]. It can be seen that the length of
borides is less than 15 m when the alloy was sintered with
1200 C/40 MPa/10 min. It has been reported by other investigators, that borides exist in different morphologies in TiAl-based
alloys, and their crystal structures mainly depend on the boron
contents [18,19]. For the studied alloy, the crystal structure of
the flakes is not known yet, but from the quasi-hexagonal sections of the borides it is concluded that the boride phase is TiB2
[19]. In addition, Y2 O3 particles cannot be eliminated through
SPS process.
4.2. Effect of HIP on microstructure
It is well known that HIP treatment is more efficient to homogenize microstructure and eliminate pores. According to TiAl
quasi-phase diagram, the formation of NL microstructure is not
difficult to understand because HIP temperature is in the ( + )
phase regions (Fig. 6). Similarly, it can be deduced that the
SPS microstructure is unstable due to the shorter sintering time.
When as-SPS alloy was HIPped at 1200 C, phase dissolves
and transforms to phase. The dissolving rate of phase (segregation) located in the lamellar colonies is faster than that
located at the boundaries of lamellar colonies, which maybe
the diffusion distances of Nb and W elements is shorter in the
colonies. Therefore, most of -segregation disappears after HIP
treatment. However, -segregation cannot completely dissolve
during the holding due to the lower HIP temperature. During
subsequent cooling, diffusion takes place, which allows for the
growths of lamellar colony and the remanent phase. Lamellar colonies size does not evidently increase after HIP treatment
due to the restricting effect of grains and phase located at

Fig. 6. 8Nb (at.%) containing TiAl quasi-phase diagram.

the boundaries of lamellar colonies. It is noted that the volume

fraction of phase decreases from 7% to 5% after HIP treatment
even if the remanent phase grows up.
It was also found that the sizes of borides in the studied alloy
after HIP treatment almost does not change, which is consistent
with previously observed results [20]. It reveals that the borides
can hardly eliminated by HIP or heat treatment due to lower
solubility in both and 2 phases. Moreover, borides can act as
grain growth inhibitors by pinning grain boundaries during HIP.
4.3. Effect of microstructure on the mechanical properties
For as-HIP Ti45Al8.5Nb(W,B,Y) alloy, the compression
strength is higher, but its ductile is equal to that of as-cast alloys
reported previously [20]. Under compressive loading, as-HIP
alloy generally exhibits higher strength because of its grain
refinement and high impurity content. For the NL structure of asHIP alloy, the grain sizes can be as small as 35 m, whereas cast
alloys have lamellar grains being normally 100500 m [6,21].
According to Hall-Petchs Law, a material with fine microstructure possesses high yield strength. The other reason may be due
to the existence of higher oxygen content.
Microsegregations in NL microstructure play important roles
in the mechanical properties. The deformation incompatibility
between phase and matrix will induce microcracks in their
interfaces and reduce the ductility of the alloy as well [22]. The
effect of boron addition on mechanical properties is contradictory. On the one hand, boron addition is beneficial to improve
strength and ductility by refining grain. On the other hand, lager
boride precipitation is detrimental to the mechanical properties.
Few yttrium oxide (Y2 O3 ) can improve mechanical properties
due to its precipitation strengthening at the grain boundary.
It was also found that the effect of the strain rate on deformation behavior is significant. With the increasing of the strain
rate, the compression temperature increases if the high quality compressed samples without cracks can be obtained. As

Y.H. Wang et al. / Materials Science and Engineering A 489 (2008) 5561

well known that the compression deformation is complied with

ZenerHollomon parameter Z, i.e. Z = exp(Q/RT), where , T
are the test strain rate and temperature, respectively, Q is the
apparent activation energy for hot deformation [23]. It indicates that the alloy has lower deformation resistance at higher
temperature (1100 C) and lower strain rate (1 102 S1 ).
The shape of the curves reflects the change of the
microstructure during compression deformation. The decrease
of the flow stress at a certain stage of deformation is owing
to a great deal of dynamic recrystallization and breakup of the
lamellar microstructure. Under the test conditions, the plasticity of phase is increased and relatively large strain can be
realized by the propagation of dislocation and twins. The available information on the deformation behavior of the 2 and
phases in TiAl-based alloys with NL microstructure is limited,
but the effect of phase on the deformation behavior can be
ignored because of its low content for the studied alloy. Therefore, dynamic recrystallization and globalization of the lamella
is responsible for the microstructure evolution. It has been found
that the globalization of the 2 phases is slower than that of the
phase in the 2 / lamella structure [24]. The latter globalization
depends on lamellar orientation and strain. The lamella oriented
along and perpendicular to the compression axis are the more
favorable for dynamic recrystallization development. Intensive
cross twinning at the beginning of the loading and activation of
rotation modes of deformation promote the dynamic recrystallization for lamellar colonies. At the same time, when lamellar
boundaries are relatively inclined to the compression axis, the
stability of the lamellar structure is the highest. As a result, the
dynamic recrystallization process is very slow. When the stress
levels off, dynamic recrystallization process is completed.
5. Conclusions
(1) The sintering temperature has a significant effect on the
microstructures. When the sintering temperature is 1000 C,
the dendritic microstructure of as-SPS alloy is similar to
that of the alloying powder. At 1100 C, the interfaces of
these particles are still discernible, but near microstructure appear in every particle. A typical FL microstructure
followed by two types of microsegregations is successfully
developed at 1200 C. However, FL microstructure becomes
coarser at 1300 C.
(2) As-HIP alloy has NL microstructure along with segregation. The morphologies of phase in as-HIP alloy
are different from those in as-SPS alloy because most of
phase in the form of block are located at the boundaries of
lamellar colonies.
(3) The alloy exhibits excellent compression properties at
elevated temperatures. When compression temperature is
higher than 1100 C, high quality compressed samples with-

61

out cracks can be obtained even if engineering compression

strain is up to 80% for the strain rates of 1 101 to
103 S1 .
Acknowledgements
This research was performed under the auspices of the
Hi-Tech Research and Development Program of China (No.
2006AA03Z511), the Key Grant Project of Chinese Ministry
of Education (No. 704008) and the program from New Century
Excellent Talents in University (No. NCET0401017).
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