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Procedia Manufacturing 50 (2020) 355–361

18th International Conference Metal Forming 2020 Project

18th InternationalConference
18th International Conference Metal
Metal Forming
Forming 2020 2020
Project
Effect of ball milling speed and sintering temperature on microstructure and
Effect of ball milling speed and sintering temperature on microstructure and
properties of TiAl alloy prepared by powder metallurgy
properties of TiAl alloy prepared by powder metallurgy
Gong Siheng, Dong Xianjuan*, Xiao Xuan, Xu Yong
Gong Siheng, Dong Xianjuan*, Xiao Xuan, Xu Yong
School of Aeronautical Manufacturing Engineering, Nanchang Hangkong University, Nanchang 330063, China
School of Aeronautical Manufacturing Engineering, Nanchang Hangkong University, Nanchang 330063, China
* Corresponding author. Tel.:13397080873. E-mail address: dxj3@163.com
* Corresponding author. Tel.:13397080873. E-mail address: dxj3@163.com

Abstract
Abstract
In order to obtain high-quality composite powder for vacuum hot pressing sintering and TiAl alloy with good microstructure and properties, the
In order
effect of to
ballobtain high-quality
milling speed on thecomposite
morphologypowder for vacuum
of composite hot pressing
powder and thesintering
effect ofand TiAl alloy
sintering with good
temperature microstructure
on the andand
microstructure properties, the
mechanical
effect of ball
properties of milling
the alloyspeed
wereon the morphology
studied. The researchof composite powder
results show and the
that lower effect
ball millof sintering
speed temperature
is beneficial on the the
to achieve microstructure and mechanical
effect of uniform mixing of
propertiesexcessive
powder, of the alloy were speed
rotation studied.of The
ball research
mill willresults
lead toshow that lower and
agglomeration ball cold
mill speed
weldingis beneficial to achieve
of composite powder. theThree
effectsintering
of uniform mixing of
temperatures
powder,
give threeexcessive rotation speed
typical structures of TiAlof alloy,
ball mill
the will lead
matrix to agglomeration
phase content of γ-TiAland cold
and αwelding of composite
2-Ti3Al changes powder.
with the Three
sintering sintering temperatures
temperature, the increase
give
in three typical
sintering structures
temperature makesof TiAl alloy,
the alloy the matrix
structure phase
more content
uniform andoftheγ-TiAl
density α2-Ti
andalso 3Al changes
increases. When with
the the sintering
sintering temperature,
temperature risesthe
to increase
1300Ԩ,
in
thesintering
density of temperature makes the
the alloy reaches alloy structure
4.419g/cm more uniform
3, the hardness value ofand
thethe density also
hot-pressed increases.
alloy Whenisthe
at 2h/1240Ԩ thesintering
highest, temperature
and the valuerises to 1300Ԩ,
of hardness is
the density of the alloy reaches 4.419g/cm3, the hardness value of the hot-pressed alloy at 2h/1240Ԩ is the highest, and the value of hardness is
527.14HV.
527.14HV.
© 2020 The Authors. Published by Elsevier B.V.
© 2020
© 2020
This The
The
is an open Authors.
Authors. Published
accessPublished
article by
the Elsevier
by Elsevier
under B.V. B.V. license (http://creativecommons.org/licenses/by-nc-nd/4.0/)
CC BY-NC-ND
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This is an open
is an open
Peer-review access
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article under
responsibility under the CC
CC BY-NC-ND
of the scientific BY-NC-ND oflicense
license
committee 18th(http://creativecommons.org/licenses/by-nc-nd/4.0/)
(http://creativecommons.org/licenses/by-nc-nd/4.0/)
the International Conference Metal Forming 2020 Project.
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responsibility of of
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committee of 18th
of the the 18th International
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Conference Metal Metal
Forming Forming 2020
2020 Project.
Keywords: Ball milling speed; Ti-44Al-2Cr-4Nb-0.2W-0.2B alloy; Vacuum hot pressing sintering; Sintering temperature
Keywords: Ball milling speed; Ti-44Al-2Cr-4Nb-0.2W-0.2B alloy; Vacuum hot pressing sintering; Sintering temperature

1. Introduction severely restricted [8]. Therefore, in view of the potential

1. Introduction severely
applicationrestricted
background [8]. Therefore,
of TiAl-based in view
alloys,of research
the potential
and
Lightweight high-temperature structural materials have application
developmentbackground
of effective of TiAl-based
preparation andalloys,
forming research and
technology
Lightweight
always been one high-temperature
of the materials ofstructural materials fields
choice in high-tech have development of effective preparation and forming
for this material is the key to its development and application. technology
always
such as been one ofAtthepresent,
aerospace. materials
the of
usechoice in high-tech
temperature fields
of Ni-based forThe
this material is the key to alloy
as-cast TiAl-based its development
prepared by and conventional
application.
such as aerospace.
and Ti-based At present,
superalloys that the usebeen
have temperature of Ni-based
conventionally used The as-cast
methods TiAl-based
has defects alloy structure,
such as coarse prepared internal
by conventional
shrinkage
and Ti-based superalloys that have been conventionally
has basically reached the limit. Therefore, the development used
of methods has defectssegregation,
pores, composition such as coarse andstructure,
inclusions internal shrinkage
[9], and the use
has
newbasically reached the
high-temperature limit. Therefore,
structural materialsthehasdevelopment
become a top of pores, composition
of powder metallurgy segregation,
technologyand to inclusions [9], and the
prepare TiAl-based use
alloys
new high-temperature
priority for the aero-enginestructural materials industry
manufacturing has become a top
[1]. TiAl- of
canpowder metallurgy
effectively improvetechnology to prepare
these problems, it is aTiAl-based alloys
near-net forming
priority for the
based alloys aero-engine
stand out due tomanufacturing industrymechanical
their comprehensive [1]. TiAl- can effectively
technology for improve
effectivelythese problems,
preparing it is a near-net
fine-grained forming
TiAl-based
based alloyssuch
properties standas out
lowdue to theirhigh
density, comprehensive mechanical
elastic modulus, good technology for effectively
alloys. According preparing
to the original fine-grained
powder state, theTiAl-based
method of
properties such as strength
high-temperature low density,
and high elastichigh-temperature
excellent modulus, good alloys.
preparingAccording
TiAl-based to thealloys
original
by powder
powder state, the method
metallurgy can beof
high-temperature
oxidation resistancestrength
[2], and and excellentto high-temperature
are expected replace Ni-based preparing
divided intoTiAl-based
pre-alloyedalloys
powder bymethod
powder andmetallurgy can be
elemental powder
oxidation resistance [2], and are expected
superalloys in turbine engines to achieve weight to replace Ni-based
reduction of divided
method,intoeachpre-alloyed
of the powder method and
two methods has elemental
advantages powder
and
superalloys
20% to 30%in [3], turbine engines toasachieve
recongnized weight
the most reduction
promising of
high- method, each The
disadvantages: of TiAl-based
the two methods has advantages
alloy prepared and
by the pre-alloy
20% to 30%structural
temperature [3], recongnized
material as the most
[4-7]. However,promising
due tohigh-
the disadvantages:
powder methodThe hasTiAl-based
the advantagesalloy prepared by the pre-alloy
of good uniformity, low
temperature
shortcomingsstructural material alloys,
of TiAl-based [4-7]. However,
such as poor due toroomthe powder
oxygen method has the content,
and impurity advantages andof excellent
good uniformity, low
mechanical
shortcomings of TiAl-based
temperature fracture toughness alloys, such low-temperature
and difficult as poor room oxygen and
properties, impurity
however, it iscontent, and expensive
difficult and excellent tomechanical
make raw
temperature fracturethetoughness
plastic processing, practical and difficultoflow-temperature
application this material is properties, however,
materials; the it is difficult
main feature of the and expensive
element powder to method
make raw is
plastic processing, the practical application of this material is materials; the main feature of the element powder method is
2351-9789©©2020
2351-9789 2020
TheThe Authors.
Authors. Published
Published byB.V.
by Elsevier Elsevier B.V.
Thisisisanan
2351-9789
This ©open
2020
open access
The
access article
Authors.
article under
Published
under the theElsevier
by
CC BY-NC-NDCC BY-NC-ND
B.V. license (http://creativecommons.org/licenses/by-nc-nd/4.0/)
license (http://creativecommons.org/licenses/by-nc-nd/4.0/)
Peer-review
This is an open
Peer-review under
access
under responsibility
article under
responsibility of the
CC scientific
BY-NC-ND
of the scientific committee
license
committee of the 18thConference
International Conference
2020 Metal
(http://creativecommons.org/licenses/by-nc-nd/4.0/)
of the 18th International Metal Forming Project.Forming 2020
10.1016/j.promfg.2020.08.066
Peer-review under responsibility of the scientific committee of the 18th International Conference Metal Forming 2020 Project.
356 Gong Siheng et al. / Procedia Manufacturing 50 (2020) 355–361
2 Gong Siheng et al. / Procedia Manufacturing 00 (2019) 000–000
low cost, easy addition of alloy elements and control of alloy
composition, but the high impurity content seriously
deteriorates the performance of TiAl-based alloys [10]. With
the improvement of elemental powder purity and densification
technology, the preparation of TiAl-based alloys by elemental
powder method has gradually become a development trend
[11].
This experiment uses high-purity Ti, Al, Cr, Nb, W, B
elemental powder as raw materials, using vacuum hot pressing
sintering powder metallurgy technology to prepare Ti-44Al-
2Cr-4Nb-0.2W-0.2B alloy with uniform composition， fine
structure and high density, the effects of ball milling speed and
hot pressing sintering temperature on the microstructure and
properties of the sintered blank were also studied.
2. Materials and methods
In this experiment, high-purity Ti powder (99.7% purity,
300 mesh), Al powder (99.9% purity, 300 mesh), Nb powder
(99.9% purity, 325 mesh), Cr powder (99.5% purity, 325
mesh), W powder (99.9% purity, 325 mesh) and B powder
(99.9% purity, 325 mesh) were used as raw materials.
Preparation of Ti-44Al-2Cr-4Nb-0.2W-0.2B (at%) alloy
powder according to the atomic percentage of the alloy's
nominal composition, then pouring it into a stainless steel ball
mill tank equipped with bearing steel balls. After sealing the
ball mill tank, evacuating and filling it with argon, repeating
the above operation three times to ensure a high degree of
vacuum in the ball mill tank, and using a planetary ball mill to
mill powders under Ar atmosphere. The speed of the ball mill
is 160r/min, 300r/min, 400r/min, the ball milling time is 2h,
and the ball-to-material ratio is 10:1 (stainless steel ball 330g,
powder 33g). The operations of powder loading and powder
extraction are carried out in an argon atmosphere.
The composite powder obtained at the optimal ball milling
speed is selected and filled into a high-strength graphite
sintering mold, and hot-press sintering is carried out in a
ZRYS-2000 multifunctional vacuum hot-press furnace. The
sintering temperature is 1150Ԩ, 1240Ԩ and 1300Ԩ,
respectively, the axial pressure of 40MPa is applied during the
process, and the insulation pressure is maintained for 2h. After
the sintering is completed, the sample is taken out with the
furnace cooling. The sintering process is shown in Figure 1.
The phase composition of the hot-pressed sintered alloy was
analyzed with a D8ADVANCE (Germany Bruker) Da Vinci X-
ray diffractometer. The field emission scanning electron
microscope Nova Nano SEM450 (US FEI) equipped with EDS
system was used to analyze the structure and phase
composition of the hot-pressed sintered alloy. The Archimedes
Drainage Method is used to measure the sample density. The
micro-hardness is measured with a HVS-1000 digital micro-
hardness tester, the load is 1.96 N, the holding time is 15 s, and
each sample is tested with 10 Vickers hardness， and the
average value is taken.
1400 140
1200 —Temperature 120
—Pressure
1000 100
Pressure/Mpa
Temperature/�
800 80
600 60
400 40
200 20
0 0
0 50 100 150 200
Time/min
250 300 350
Fig. 1. Sintering curve.
3. Results and discussion
3.1. Powder morphology analysis
In the process of ball milling, the energy of the powder is
provided by the grinding ball running at high speed, and then
undergoes severe plastic deformation under the impact of the
grinding ball impact and friction. Fig. 2(a) and Fig. 2(b) show
the morphology of the composite powder when the ball milling
speed is 400r/min, due to the different plasticity and strength of
various powders, especially the Al powder with better plasticity
first flattened and firstly adhered to the grinding ball and ball
mill jar, at this speed, the compound powder after ball milling
almost all sticks to the wall of the ball mill tank and the surface
of the grinding ball, and finally a small amount of granular and
disc-shaped substances with metallic luster are obtained, the
average diameter is between 0.7mm～0.8 mm, Li Xuewen [12]
and Zhang Hongzhi [13] had a similar situation when studying
the ball milling process. In the case of 400r/min ball milling,
the reason why the composite powder forms particles with
metallic luster is mainly related to the excessively high milling
speed. The faster the milling speed, the more energy in the ball
milling system, which causes the temperature in the ball
milling tank to increase, the powder softens and the viscosity
increases. When the low melting point Al powder is in a molten
state, as the thickness of the Al layer increases, some Ti powder
and Nb powder are embedded in the Al layer under the action
of the grinding ball and gradually form a Ti/Al/Nb composite
powder layer. The embedded Ti powder and Nb powder cause
the plasticity of the composite layer to decrease, especially
under low temperature environment, Nb has serious brittleness,
and the Ti/Al/Nb composite powder layer falls off under the
effect of surface tension, and finally a small amount of fine
particles and wafers with metallic luster are obtained. Figure
2(c) is the composite powder morphology after the ball milling
speed is 300r/min. Compared with the situation of 400r/min,
the powder morphology and adhesion have been effectively
improved, but cold welding and agglomeration still exist, the
overall appearance is in the shape of gravel, the average size is
around 35μm. Under this ball milling condition, the original
powder was continuously broken and welded during the ball
milling process and thus refined, and the surface energy of the
composite powder increases with the degree of refinement, and
the adsorption is enhanced, in addition, under closed
 Gong Siheng et al. / Procedia Manufacturing 50 (2020) 355–361 357
Gong Siheng et al. / Procedia Manufacturing 00 (2019) 000–000 3

conditions, the system heat is not sufficiently dissipated, which
causes the fine powder particles to agglomerate to form
secondary large particles, as a result, the shape of the ball mill
powder is irregular and the size becomes larger, and the powder
extraction rate is low, thereby affecting the density of the
sintered block. Figure 2(d) is the composite powder
morphology after the ball milling speed is 160r/min. Under this
condition, the composite powder after ball milling is nearly
spherical, with an average particle size of 13 μ m, which
basically remains unchanged from the original powder
morphology, the energy provided by the low-speed ball mill is
insufficient to make the composite powder achieve
agglomeration and cold welding, and can only achieve uniform
mixing of the composite powder.

(a) (b)

(c) (d)

Fig. 2. Evolution of morphology of Ti-44Al-2Cr-4Nb-0.2W-0.2B composite powder at different ball milling speeds

(a) 400r/min (b) 400r/min macro powder morphology (c) 300r/min (d) 160r/min.

3.2. Composite powder phase and grain size analysis

Figure 3 is the X-ray diffraction pattern of the composite
powder at different ball milling speeds. It can be seen from the
figure that the composite powder still has only Ti, Al, Nb
diffraction peaks after ball milling at different speeds, because
the amount of Cr, W, B added is too small, their diffraction
peaks are not detected, but EDS is applied to the sintered block
analysis can detect their presence. No new phase is formed
during the ball milling process, which is consistent with what
is reported in the literature [14,15], that is, during ball milling,
no matter how the ball milling conditions are changed, TiAl
metal compounds will not be generated. With the increase of
the ball milling speed, the diffraction peaks of the three
elements gradually decrease and broaden, especially under
400r/min, the diffraction peak changes most significantly. The
composite powder is plastically deformed by the impact of the
grinding ball at a speed of 400r/min, internal stress and strain
are generated inside the powder particles, a large number of
dislocations generated within the crystal are entangled or
concentrated at the position of the grain boundary, which is
typical of work hardening. In the final state, dislocation cells
are formed in the crystal grains, which induces lattice distortion
of Ti and Al, thereby refining the crystal grains, this is
358 Gong Siheng et al. / Procedia Manufacturing 50 (2020) 355–361
4 Gong Siheng et al. / Procedia Manufacturing 00 (2019) 000–000

confirmed by the broadening of the diffraction peaks of Ti and 50 0.6

Al
Al and the reduction of the peak intensity. At 400r/min, some 45
0.5
Al particles form amorphous, which may be caused by the 40

extreme refinement of the grains and the continuous increase 35 Ti 0.4

of microscopic defects such as vacancies and microcracks in

Grain size(nm)
30
the grains, and the two-element atoms at the Ti/Al interface

Strain(%)
25 0.3
diffuse together under the thermal excitation of the ball mill Ti
20
system. 0.2
15 Al

 10
○ 0.1
72 5

● Ti
○ Al 54 0 0.0

Intensity/a.u.
 Nb 100 200 300 400
Milling speed(r/min)
36
Fig. 4. Effect of ball milling speed on powder grain size and microscopic strain.
 18
○
  ○
  ○ 3.3 Effect of sintering temperature on alloy phase

160r/min composition and microstructure

300r/min Although increasing the ball milling speed is beneficial to

refine the grain size of the powder, it is accompanied by
400r/min unfavorable factors such as an increase in the size of the
powder morphology and a low powder extraction rate.
10 20 30 40
2θ/(0)
50 60 70 80
Considering that these unfavorable factors will affect the
Fig. 3. X-ray diffraction pattern of composite powder at different ball milling diffusion reaction of the powder during the sintering process,
speeds. therefore, in order to ensure the compactness and uniformity of
the sintered body, the uniformly mixed composite powder
Figure 4 shows the variation of the grain size of Ti and Al
obtained at the speed of 160r/min is selected for hot-press
in Ti-44Al-2Cr-4Nb-0.2W-0.2B composite powder and the
sintering . The phase analysis of the alloy blocks obtained at
microscopic strain in the grains of Ti and Al with the ball
different sintering temperatures is shown in Fig 5. According
milling speed, calculated according to a single wavelength.
to the mechanism of the reaction synthesis of Ti and Al element
With the increase of the speed of the ball mill, the grain size of
powders, it can be seen that Ti and Al have undergone a
Ti and Al has decreased significantly. At the speed of 160r/min
complex reaction and phase transformation process during
～300r/min, the trend of the grain size decline is slow, but
vacuum hot-press sintering. After hot-press sintering at 1240Ԩ
during the process of 300r/min～400r/min, the grain size of the
and 1300Ԩ, the metastable phases TiAl3 and TiAl2 synthesized
two powders decreases sharply, especially for Al powder, the
by the reaction of Ti and Al disappeared completely, and finally
grain size decreases to 19.2nm at a speed of 400r/min, the
only the matrix phases of γ-TiAl and α2-Ti3Al stabilized by
broadening of the Al diffraction peak also clearly illustrates
TiAl-based alloys were formed. The difference is that the XRD
this. The decrease in grain size is related to the violent plastic
detection of the 1150Ԩ sintered block not only contains γ-TiAl
deformation of the powder during the ball milling process, as
and α2-Ti3Al high-temperature stable phases, but also finds the
the grain size of the powder decreases, the microscopic strain
existence of TiAl3 phase, this may be because the temperature
also increases accordingly, the lattice distortion induced by
is too low and the TiAl3 phase has not been exhausted. At the
large plastic deformation and the dislocations accumulated in
same time, no characteristic peak of Nb element was found in
the grains gradually form substructures, resulting in a large
the XRD pattern, indicating that the Nb element has fully
number of new grain boundaries, and the grains are refined. It
diffused or solid dissolved into each phase. According to the
is also found from Fig. 4 that the grain refinement rate of Ti is
RIR value of each phase, adiabatic method is used to calculate
lower than that of Al, this may be due to the fact that the
the content of each phase of alloy block under different
hardness of Al is lower than that of Ti during ball milling, under
temperature sintering. As shown in Fig 6, it can be seen from
the high-speed rotating grinding ball, Ti particles are rolled into
Fig. 6 that the higher the sintering temperature, the γ phase
the form of embedding into the Al layer on the surface of the
content of the sintered alloy increases and the α2 phase content
ball, and the degree of deformation is naturally lower than that
decreases, this point can also be known from the peak intensity
of Al, the degree of dislocation accumulation and lattice
ratio of γ-TiAl and α2-Ti3Al at various temperature in Fig. 5.
distortion are also relatively low, so the rate of decrease of Ti
grain size is slower than that of Al.
 Gong Siheng et al. / Procedia Manufacturing 50 (2020) 355–361 359
Gong Siheng et al. / Procedia Manufacturing 00 (2019) 000–000 5


 lamellar structure composed of most lamellar layers (L(α2/γ))
500  TiAl
 Ti3Al
and a small amount of equiaxed γ grains is obtained, the
 TiAl3 lamellar layer is larger than the double-structured lamellar
400
layer obtained by sintering at 1240°C, the lamellar size is
1300�   between 75μm～80μm, this is because the reduction of γ
   
  grains limits the growth of the lamellar layer. The bright white
Intensity/a.u.

300      

area in the figure is the Nb-rich area, it can be seen that as the
200 sintering temperature increases, the bright white area gradually
decreases, indicating that the more fully the Nb element is
100 1240�
diffused, the more evenly distributed in the matrix structure.
From Figures 7(b) and (c), it is found that the lamellar structure
1150�  is mostly present in the Nb-rich region, Chen et al. [16] have
0
20 30 40 50 60 70 80
shown that the presence of high Nb content reduces the Tα value
2θ/( )
0
of the alloy. Therefore, the enrichment of the Nb element has
Fig. 5. X-ray diffraction pattern of alloy blocks at different sintering conducive to the formation and growth of sheet tissue.
temperatures.
90
TiAl (a)
80 78.4 Ti3Al
74.8
TiAl3
70

60
Phase content%

50

39.7
40
35.1
30
25.2 25.2
21.6
20

10

0
1300� 1240� 1150�
Fig. 6. The phase content of alloys with different sintering temperatures.

Figure 7 is a secondary electron image of Ti-44Al-2Cr-4Nb- (b)

0.2W-0.2B alloy under different hot pressing temperatures.
Obviously, the microstructure morphology of the alloy changes
significantly with the increase of temperature. 1150Ԩ is close
to the eutectic point (Te), the α2 phase grain nucleation and
growth are restricted, in the subsequent cooling process, a large
number of fine γ equiaxed crystals and a small amount of α2
phase near γ structure are formed, and the grain size is between
10μm～15μm; 1240°C is in the middle of the α+γ two-phase
region, higher than the eutectoid temperature Te, there will be
more γ-phase transformation to α-phase, that is the α+γ two-
phase region is transformed into α-phase by high-temperature
disordered transformation, duo to the residence time of the α+γ
two-phase region is too long, the γ phase will nucleate in the α
phase and evolve toward the γ/α sheet structure, in the
subsequent cooling process, when the cooling temperature
reaches the Te point, the α phase undergoes an eutectoid
reaction to orderly transform and decomposes into the γ phase
and the α2 phase along the lamellar direction, the two compete
with each other for growth, which limits the growth of the
lamella thickness and forms a more stable and fine α2/γ
lamellae structure. Finally, a dual structure composed of
equiaxed γ grains and α2/γ lamellar clusters is obtained, the
lamellar size is between 30μm～35μm; 1300Ԩ is slightly
lower than the α transition temperature (Tα), at this temperature,
the sintered alloy is mainly composed of a large amount of
massive α phase and a small amount of γ, after cooling, a near
360 Gong Siheng et al. / Procedia Manufacturing 50 (2020) 355–361
6 Gong Siheng et al. / Procedia Manufacturing 00 (2019) 000–000

4.5 550
(c) Density
Hardness 527.14 4.419
525
4.4

4.308 500
4.3

Density(g/cm 3 )

Hardness(HV)
480
475
4.223
460.86
4.2
450

4.1
425

Fig. 7. Secondary electron micromorphology of sintered alloy at different hot
pressing temperatures: (a)1150Ԩ/2h；(b)1240Ԩ/2h；(c)1300Ԩ/2h.
3.4 Effect of sintering temperature on alloy properties
Figure 8 shows the relationship between alloy density and
hardness at different sintering temperatures. It can be seen from
Fig. 8 that during the temperature increase, the alloy density
increases from 4.223 g/cm3 at 1150°C to 4.308 g/cm3 at
1240°C, and finally to 4.419 g/cm3 at 1300°C. It can be seen
that as the sintering temperature increases, the density of the
alloy also increases, due to the softening of the powder during
the heating process, under the action of pressure, the higher the
sintering temperature, the more sintered body is more likely to
undergo plastic deformation, and the powder is crushed and
rearranged, the diffusion and migration speed of atoms is
accelerated, at this time, the increase in temperature also makes
the sintering neck grow faster between powders, the faster the
pore shrinkage, the higher the density of the alloy, so the
greater the density of the alloy.
In contrast, the hardness values of the three sintered alloys
at different temperatures have changed, as the sintering
temperature increases, it shows a trend of increasing firstly and
then decreasing. This is mainly caused by different structures
obtained from different sintering temperatures, in theory, the
finer the structure, the better the overall mechanical properties
of the alloy. Although the near γ structure obtained at 1150Ԩ
is mainly composed of fine γ grains, the sintering temperature
is too low, the resulting structure is not uniform, and the density
is low, the sintered alloy is in a low density state, and the
residual pores cause the intergranular bonding force to weaken,
so the hardness is low; when the sintering temperature rises to
1240Ԩ, the equiaxed γ phase transforms to a more stable α2/γ
layer platelet cluster, the α2 phase has a higher hardness than
the γ phase at room temperature [17,18]. The dual structure has
excellent strength, so the hardness has increased; when
sintering at 1300Ԩ, the reaction is more sufficient, the lamellar
structure grows, and the properties of the formed large-sized
lamellar are oriented [19], resulting in uneven hardness
distribution, so the hardness shows a downward trend.
4.0 400
1150� 1240� 1300�
Fig. 8. The relationship between alloy density and hardness at different
sintering temperatures.
4. Conclusions
(1) Increase of ball milling speed is beneficial to refine the
grain size of the powder, but it will increase the degree of
agglomeration and cold welding of the composite powder. The
large particle size powder has a small contact area and a long
diffusion distance, which is not conducive to the hot press
sintering reaction. The preparation of uniformly mixed and fine
composite powder should be carried out at low ball mill speed
as much as possible.
(2)There are three typical structures of TiAl alloys obtained
at three different sintering temperatures, the structure obtained
by sintering at 1150°C is near-gamma structure, the structure
obtained by sintering at 1240°C is bimorphic, and the structure
obtained by sintering at 1300°C is near-lamellar structure.
Compared with the as-cast structure reported, the grain size
refinement is at least one order of magnitude or more. The alloy
after hot pressing sintering mainly consists of γ-TiAl and α2-
Ti3Al matrix phases. With the sintering temperature increasing,
the content of γ phase increases, and the content of α2 phase
decreases. The Nb element will also diffuse more uniformly as
the sintering temperature increasing.
(3) The sintering temperature has a significant effect on the
structure and properties of the prepared TiAl alloy. The density
gradually increases with the increase of the sintering
temperature, and the hardness increases firstly and then
decreases. The hardness value of the hot-pressed sintered alloy
at 2h/1240Ԩ is the highest, which is 527.14HV. Ti-44Al-2Cr-
4Nb-0.2W-0.2B alloy sintered at 1240Ԩ has better
comprehensive mechanical properties.
Acknowledgements
The authors would like to thank financial supports of
foundation of National Defense Key Discipline Laboratory of
Light Alloy Processing Science and Technology (201903175),
Jiangxi University Science and Technology Plan Project
(NO.GJJ180535).
References

[1] Fu Yongming, Liu Wei, Zong Wei, et al. Effects of ball milling time and
hot pressing temperature on microstructure and mechanical properties of
 Gong Siheng et al. / Procedia Manufacturing 50 (2020) 355–361
Gong Siheng et al. / Procedia Manufacturing 00 (2019) 000–000
powder metallurgy Nb-16Si-22Ti-2Al-2Hf-2Cr alloy at room temperature.
Rare Metal Materials and Engineering 2013;02:184-8.
[2] Gerling R, Clemens H, Schimansky FP. Powder Metallurgical Processing
of Intermetallic Gamma Titanium Aluminides. Adv Eng Mater
2004;6(12):23-38.
[3] Chen G, Jiang Y. Preparation and Application of TiAl Intermetallic Alloys
for the Key Parts of Automobile Engine. Sichuan Nonferrous Metals; 2014.
[4] Dimiduk DM. Gamma titanium aluminide alloys—an assessment within
the competition of aerospace structural materials. Mater Sci Eng A
1999;263(2):281-8.
[5] Loria EA. Gamma titanium aluminides as prospective structural materials.
Intermetallics 2000;8(9):1339-45.
[6] Zhang Ji, Zhong Zengyong. Research and Progress of TiAl Intermetallics
Engineering Practicality. Progress in Chinese Materials 2010;29(2):9-13.
[7] Zhang WJ, Reddy BV, Deevi SC. Physical properties of TiAl-base alloys.
Scripta Mater 2001;45(6):645-51.
[8] Kabir MR, Chernova L, Bartsch M. Numerical investigation of room-
temperature deformation behavior of a duplex type γTiAl alloy using a
multi-scale modeling approach. Acta Mater 2010;58(17):5834-47.
[9] Tetsui T. Manufacturing technology for gamma-TiAl alloy in current and
future applications. Rare Metals 2011;30(1):294-9.
[10]Wang Erde, Li Xiaoqiang, Hu Lianxi. Preparation of TiAl-based alloy by
powder metallurgy. Powder Metall Tech 2002;20(5):287-93.
[11]Lin Junpin, Zhang Laiqi, Song Xiping, et al. Research progress of light-
weight γ-TiAl intermetallic compounds. Progress in Chinese Materials
2010;29(2):1-8.
361
7
[12]Li Xuewen. Powder metallurgy preparation and microstructure properties
of Ti-45Al-10Nb alloy Harbin Institute of Technology; 2015.
[13]Zhang Hongzhi. Preparation of Ti/Al/Nb composite powder and hot-press
sintering. Harbin Institute of Technology; 2018.
[14]Li Xiaoqiang, Hu Lianxi, Wilde, et al. Preparation of TiAl-based alloy by
mechanical ball milling and reaction sintering. Powder Metall Tech
2001;19(3):131-5.
[15]Bhattacharya P, Bellon P, Averback RS, et al. Nanocrystalline TiAl
powders synthesized by high-energy ball milling: effects of milling
parameters on yield and contamination. J Alloy Compd 2004;368(1-2):187-
96.
[16]Chen GL, Wang J, Ni X, et al. A new intermetallic compound in TiAl+Nb
composition area of the Ti–Al–Nb ternary system. Intermetallics
2005;13(3):329-36.
[17]Gebhard S, Pyczak F, Goeken M. Microstructural and micromechanical
characterisation of TiAl alloys using atomic force microscopy and
nanoindentation. Mater Sci Eng 2009;523(1-2):235-41.
[18]Schloffer M, Iqbal F, Gabrisch H, et al. Microstructure development and
hardness of a powder metallurgical multi phase γ-TiAl based alloy.
Intermetallics 2012;22:231-40.
[19]Zhang Peng. Preparation of Ti-45Al-5Nb alloy by powder metallurgy and
its microstructure and properties. Harbin Institute of Technology; 2013.