1-An Investigation of Ti-43Al-9VTi-6Al-4V Interface by Diffusion

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Intermetallics 36 (2013) 127e132

Contents lists available at SciVerse ScienceDirect

Intermetallics
journal homepage: www.elsevier.com/locate/intermet

An investigation of Ti-43Al-9V/Ti-6Al-4V interface by diffusion


bonding
X.R. Wang, Y.Q. Yang*, X. Luo, W. Zhang, G.M. Zhao, B. Huang
State Key Lab of Solidification Processing, Northwestern Polytechnical University, Friendship Western Road No. 127, Xi’an, Shanxi 710072, China

a r t i c l e i n f o a b s t r a c t

Article history: Ti-43Al-9V/Ti-6Al-4V joints were fabricated by vacuum hot pressing under 920  C/45 MPa/2 h. After
Received 6 August 2012 fabrication the joints were thermally exposed in vacuum at 920  C for 5 h and 17 h, and at 1100  C for 1 h.
Received in revised form The interfaces of both the as-prepared and the thermally exposed joints were analyzed by means of
24 December 2012
optical microscope, scanning electron microscope, electron backscatter diffraction system and energy
Accepted 28 December 2012
dispersive spectrometer. The results indicate that sound joints can be achieved under 920  C/45 MPa/2 h,
Available online 16 February 2013
and the interfacial phase sequence of the as-prepared joints was identified as Ti-43Al-9V/g(TiAl)/B2 (the
ordered form of b-Ti phase)/a2(Ti3Al)/a(Ti)/Ti-6Al-4V. The thickness of the interfacial zone increased
Keywords:
A. Titanium aluminides, based on TiAl
with the duration of thermal exposure at 920  C. Furthermore, the interfacial zone thickened rapidly
C. Joining when the joints were thermally exposed at temperature above the phase transformation point
D. Microstructure (a-Ti / b-Ti) of Ti-6Al-4V. In this paper, the interface growth way was also discussed based on the
B. Thermal stability locations of the refractory phase YAl2 and microvoids. The analysis of the thermally exposed joints
E. Phase stability, prediction confirmed the correctness of the interface growth way. Moreover, elemental diffusion mechanism was
discussed in this paper.
Ó 2013 Elsevier Ltd. All rights reserved.

1. Introduction phase, respectively). However, tensile and fracture properties have


no obvious distinction between the joints and g-TiAl IHI alloy.
g-TiAl intermetallics are winning more attention because of Wang et al. [2] successfully joined Ti-46.5Al-2.5V-2Cr-1.5Nb and
their low density, high elastic modulus, better oxidation resistance Ti64 via hot isostatic pressing under different parameters. They
and good creep properties at elevated temperature [1e3]. Simul- found that sound joints can be obtained at 800e900  C/100 MPa/
taneously, the welding performance of g-TiAl alloy must be studied 2 h. Their tensile results indicated that the joints fabricated under
before their extensive application in aerospace field. For the 880  C/100 MPa/2 h have the highest fracture strength. G. Çam et al.
welding between Ti-6Al-4V (called as Ti64 hereafter) and TiAl alloy, studied the microstructural and mechanical characterization of
the welding technologies used in previous studies mainly belong to diffusion bonded hybrid TiAl/Ti64 joints [7]. According to the
fusion welding [4,5]. However, fusion welding can affect the measured shear strength values of the joints, the optimum pressure
structure of base materials, and it can lead to voids and hot crack- and bonding temperature are 850  C and 5 MPa, respectively. They
ing. Diffusion bonding can effectively avoid these defects and needs thought that the formed interfacial product Ti3Al is detrimental to
not to melt base materials [6e8]. the bond strength of the joints, which can be concluded by the
Many studies have been carried out concerning g-TiAl/Ti64 joint results of the shear strength test of the produced joints. Kong et al.
by diffusion bonding. Holmquist et al. studied the interfacial also studied the interfacial microstructure and shear strength of
microstructure, the distribution of elements and tensile property of Ti64/Ti-43Al-9V laminate composite sheet fabricated by hot packed
Ti64/TiAl joint which was achieved by hot isostatic pressing [1]. rolling [8]. Combining the results of energy dispersive spectrometer
According to their results, sound joints can be achieved under (EDS), X-ray diffraction (XRD) and transmission electron micro-
900  C/200 MPa/1 h. The interfacial thickness increased with the scope (TEM) analysis, they thought that the structure of the inter-
increase of temperature, and the interfacial phase sequence is g- facial region was TiAl/g þ B2/a2/Ti64 (in which B2 is the ordered
TiAl/g þ a2/a2 þ a/Ti64 (in which g, a2 and a are TiAl, Ti3Al and a-Ti form of b-Ti). The average shear strength of the produced joints was
335.7 MPa, and one of the reasons for this value is that the strength
of the formed a2 is better than that of the g-TiAl intermetallic
* Corresponding author. Tel./fax: þ86 29 88460499. compound. Several other investigations have also been done by
E-mail address: [email protected] (Y.Q. Yang). researchers [9e12]. Although the compositions and statuses of the

0966-9795/$ e see front matter Ó 2013 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.intermet.2012.12.018
128 X.R. Wang et al. / Intermetallics 36 (2013) 127e132

Fig. 1. OM photographs of the as-prepared joint with a lower magnification in (a) and a higher magnification in (b).

intermetallic alloys based on TieAl system are different in these room temperature through 3 h. The pressure, 45 MPa, was kept 2 h
studies, similar promising results have been achieved. And the at 920  C. The cooling process took 5 h to room temperature. During
previous studies mainly focused on the processing and mechanical the hot pressing process, the vacuum pressure in the furnace was
property of the joints. However, the interface growth way has not kept below 3.5  102 Pa.
been addressed, and the element diffusion behavior has not been By vacuum seal welding machine, part of the as-prepared joints
deeply studied, either. Therefore, the interfacial microstructure of was sealed in the stainless steel tubes which supply a vacuum at-
the Ti-43Al-9V/Ti64 joint, the interface growth way and element mosphere (<5  103 Pa). Then these sealed joints were thermally
diffusion behavior will be studied in this work. exposed under 920  C/5 h, 920  C/17 h and 1100  C/1 h in a box type
In this study, Ti-43Al-9V/Ti64 joints were fabricated via vacuum resistance furnace, respectively.
hot pressing under 920  C/45 MPa/2 h. Part of the as-prepared Both the as-prepared and the thermally exposed joints were cut
joints was then thermally exposed at 920  C for 5 h (written as perpendicular to the bonding interface with a low speed diamond
920  C/5 h hereafter), 920  C/17 h and 1100  C/1 h, respectively. saw. Then metallographic specimens were prepared by conven-
Then the interfacial microstructure and element distribution tional preparation methods of metallographic sample. After that
characteristic were analyzed by means of optical microscope (OM), the interfacial microstructure and element distribution character-
scanning electron microscope (SEM), EDS and electron backscatter istic were analyzed by an optical microscope and a SUPRA 55 field
diffraction (EBSD). emission scanning electron microscope equipped with an Oxford
INCA energy-dispersive spectrometer and HKL electron backscatter
2. Experimental diffraction system.

Ti64 is a typical a þ b duplex phase alloy, and the thickness of 3. Results and discussion
Ti64 foil utilized in this study is 0.35 mm. The nominal composition
of g-TiAl alloy is Ti-43Al-9V-0.3Y (at%) which is composed of 3.1. Microstructural analysis of the interface for the as-prepared
massive g-TiAl phase, a small amount of lamellar a2/g, stripe-like joint
B2, YAl2 and Y2O3 phase.
Before diffusion bonding, the two base materials were succes- Fig. 1 shows the OM micrographs of the as-prepared joint. It is
sively ground on silicon carbide abrasive papers from no. 600 to seen that the interfacial zone is uniform with no obvious defects,
1500. In order to remove the superficial oil and oxidation con- such as voids or gaps. Typical equiaxial structure appears in Ti64
tamination, they were then cleaned with acetone and etchant (10% alloy, which can be attributed to the distortion happened in the
HF; 5% HNO3; 85% H2O in volume fraction) sequentially. After duplex phase field. Obvious stratification phenomenon can also be
mounted in a mould, the materials were heated up to 920  C from found at the interfacial zone.

Fig. 2. (a) SEI of the interfacial zone of the as-prepared joint, (b) The corresponding line distribution of elements.
X.R. Wang et al. / Intermetallics 36 (2013) 127e132 129

Fig. 3. (a) EBSD analysis field of the as-prepared joint interface, (b) the front backscatter electron micrograph of the EBSD analysis field in (a), (c) the schema of phase distribution in
the EBSD analysis field.

Fig. 4. SEI of the as-prepared joint with (a) showing the location of EDS point analysis at the interfacial zone; and (b) showing the location of the YAl2 phase.

The stratification phenomenon and element distribution char-


acteristic in the interfacial zone were further studied by SEM and
EDS analysis. Fig. 2 shows the secondary electron imaging (SEI) of
the interface and the corresponding line analysis curves of ele-
ments. It can be seen that the interfacial zone can be divided into
two regions as marked in Fig. 2a. The region close to Ti-43Al-9V is
marked as region 1, while the region close to Ti64 is marked as
region 2. The thickness of the interfacial zone, region 1 and 2 are
about 11.2 mm, 6.7 mm, 4.5 mm, respectively. Obviously, it can also be
seen that the grains in the interfacial zone are refined. The condi-
tion of 920  C and 45 MPa is adequate to arouse dynamic recovery
and recrystallization for these two alloys, which can then refine the
interfacial grains [13].

Table 1
The EDS analysis result of the interfacial grey white phase in Fig. 4a.

Element O Ti Al V Y
Fig. 5. SEI showing the discontinuous microvoids in the interfacial zone of the as-
Content (at%) 9.32 8.13 50.85 0.52 31.18
prepared joint.
130 X.R. Wang et al. / Intermetallics 36 (2013) 127e132

3.2. Interface growth way

Rare-earth element Y was added into the Ti-43Al-9V alloy to


refine grains and structure. Element Y will pile up along grain
boundary to form the refractory phase YAl2 during the casting
process of the alloy. Therefore, those YAl2 which are exactly located
at the surface can be regarded as a tag to observe the interface
growth way. Fig. 4 shows the EDS point analysis position of the grey
white phase, and the relevant results are listed in Table 1. It in-
dicates that the analyzed phase is YAl2 which was also detected by
other researchers using XRD analysis in Ti-43Al-9V alloy [14]. The
location of the YAl2 can imply the interface growth way, i.e. the
original interface intrudes into both Ti-43Al-9V and Ti64 simulta-
neously, and the interface growth rate toward Ti-43Al-9V is higher.
Discontinuous microvoids can also be observed in very few re-
gions of the interfacial zone, as shown in Fig. 5. Since a few regions
of the bonding surface are not very flat, some microvoids appeared
after diffusion bonding. However, what is no doubt is that the
Fig. 6. The established schema of the interface growth way (DB is short for diffusion location of these microvoids is the original interface of the two base
bonding). materials. The location of these microvoids can also be regarded as
a tag to confirm the interface growth way described above.
Therefore, a simplistic schema of the interface growth way can
There is a gradient variation of Al, Ti and V at the interfacial zone be established, as shown in Fig. 6. From the schema, it can be seen
as shown in Fig. 2b, which indicates that evident atomic diffusion that the original interface grows into both Ti-43Al-9V and Ti64
happened. Fig. 3a shows the SEI of the as-prepared joint interface simultaneously, and the interface growth rate toward Ti-43Al-9V is
and the EBSD analysis field, and Fig. 3b is the front backscatter higher. Therefore, the thickness of region 1 is bigger than that of
electron micrograph of the analysis field. From Fig. 3b, the mor- region 2.
phology of grains can be seen clearly. Fig. 3c is the distribution of
phases in the analyzed field which was partly drawn by hand ac- 3.3. Vacuum thermal exposure
cording to the synthesized analysis of EDS and EBSD analysis re-
sults. From Fig. 3c, it can be seen that the interfacial phase sequence In order to investigate the element diffusion characteristic at
is Ti-43Al-9V/g/B2/a2/a/Ti64. The position of B2 phase can be elevated temperature, part of the as-prepared joints was thermally
confirmed by the peak of V content curve in Fig. 2b. The ratios of Ti exposed in vacuum. Fig. 7 shows the SEI of the interfacial zones
and Al can also illustrate the appearance of a2 and a. This result is which were thermally exposed under different conditions in vac-
consistent with the previous TEM analysis in reference [8]. There- uum. The average interfacial thickness of the joints thermally
fore, there is the mixture phase of B2 and a2 in region 1 while only exposed under 920  C/5 h and 920  C/17 h are about 17 mm and
a phase in region 2. 24 mm, respectively, which indicates that the interfacial zone

Fig. 7. SEI showing the interfacial zone of the joints thermally exposed to (a) 920  C/5 h; (b) 920  C/17 h; (c) 1100  C/1 h.
X.R. Wang et al. / Intermetallics 36 (2013) 127e132 131

Table 2
EDS point analysis result of the white phase in Fig. 9.

Element O Y
Content (at%) 58.73 41.27

Fig. 9 shows the interfacial zone of the joint thermally exposed


at 920  C for 17 h. The white phase in the interfacial zone was
analyzed by EDS, and the results are shown in Table 2. It can be seen
that the white phase should be Y2O3 (melting point is 2690  C)
which is similar to YAl2. The position of Y2O3 can also be regarded
as a tag to confirm the correctness of the aforementioned interface
growth way. Furthermore, the microvoids in Fig. 7b can also be
potent evidence.

3.4. Element diffusion mechanism analysis

According to the foregoing analysis, the interface thickening is


Fig. 8. Thickening kinetics of the interface at 920  C.
controlled by diffusion. The diffusion phenomena during the whole
fabrication process can be divided into three main stages: (a) the
increased with the duration of time. Moreover, the interfacial diffusion before hot pressing; (b) the diffusion during vacuum hot
thickness can reach 27 mm after being thermally exposed at 1100  C pressing; and (c) the diffusion after vacuum hot pressing. The ele-
for 1 h. ment diffusion mechanism may be different for these stages.
It is known that the element diffusion coefficient becomes The atomic radius of Ti, Al and V are 0.145 nm, 0.143 nm and
higher at elevated temperature. So the elements will diffuse with 0.135 nm, respectively, which implies that vacancy mechanism
a higher speed both in Ti-43Al-9V and Ti64 at 1100  C than at low is the main diffusion way during the whole diffusion bonding
temperature. Moreover, the phase transformation point of Ti64 process [19].
alloy is between 980  C and 990  C, so only b phase existed in Ti64 During the course of heating up to 920  C, the concentration
at 1100  C [15]. Element diffusion coefficient is higher in b-Ti (bcc) gradient of each type of element is relative high at the original
than a-Ti (hcp) due to the lower atomic stacking density [16], which interface, which leads to a strong diffusion driving force because
will accelerate the diffusion of Ti and Al in Ti64 at 1100  C. The Ti- the diffusion in this experiment belongs to downhill diffusion.
43Al-9V alloy contains b and g phases when the temperature is Therefore, elements should diffuse rapidly in this heating process.
1100  C [17], and the b phase can accelerate the diffusion of the However, since the pressure had not been added, diffusion hap-
elements in the alloy. From the above analysis it can be easily un- pened mainly among the contact points [20]. According to the radii
derstood why the interface thickened so quickly at 1100  C for of Ti, Al and V, they diffused only via vacancies during this heating
only 1 h. stage.
Fig. 8 shows the growth kinetics curve of the interface at 920  C. Vacancy mechanism still existed during the hot pressing.
It is seen that the interfacial thickening obeys parabolic law, i.e. Moreover, dislocations formed and their density increased with the
H ¼ k$t1/2 þ b (where k is the rate constant, b and H are the original increase of pressure. As channels of diffusion, dislocations can
and final interfacial thickness, respectively). Therefore, the thick- facilitate the diffusion of elements. The distribution of elements
ening of the interface is controlled by diffusion [18]. The formula tends to homogenize as the diffusion going on, which makes it
fitted based on the experimental results is H ¼ 3.4 t1/2 þ 10. possible to produce new phases. And then the high grain boundary
energy of these metastable grains can further promote the element
diffusion [2,20]. Therefore, many effective short circuit diffusion
ways exist in this stage.
Since the element diffusion coefficient is temperature depend-
ent by Arrhenius function, it will drop quickly with the decrease of
temperature [21]. Therefore, both the diffusion rate and quantity
became less during the cooling to room temperature. The diffusion
may proceed along the grain boundaries during the cooling stage.

4. Conclusion

The interface of the Ti-43Al-9V/Ti64 joint was studied by dif-


fusion bonding in this paper. Sound Ti-43Al-9V/Ti64 joints have
been achieved under 920  C/45 MPa/2 h vacuum hot pressing.
Based on the EDS and EBSD analysis, the interfacial phase sequence
is Ti-43Al-9V/g/B2/a2/a/Ti64. The locations of the refractory YAl2
and microvoids in the as-prepared joints indicate that the original
interface grows into both base materials simultaneously with
a higher thickening speed toward Ti-43Al-9V. The microvoids and
refractory Y2O3 phase located at the interface of the thermally
exposed joints further confirm the interface growth way. Through
Fig. 9. SEI showing the interfacial zone of the joint thermally exposed at 920  C for vacuum thermal exposure, it is known that the interface growth is
17 h. controlled by diffusion, which is well illustrated by the fitted
132 X.R. Wang et al. / Intermetallics 36 (2013) 127e132

formula H ¼ 3.4 t1/2 þ 10. Moreover, the elemental diffusion [7] Çam G, Özdemir U, Ventzke V, Koçak M. Microstructural and mechanical
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