Atasoy 2008
Atasoy 2008
Article history: Titanium and low carbon steel plates were joined through diffusion bonding using a silver
Received 3 September 2007 interlayer at various temperatures for various diffusion times. In order to determine the
Received in revised form strength of the resulting joints, tensile-shear tests and hardness tests were applied.
11 January 2008 Additionally, optical, scanning electron microscopy examinations and energy dispersive
Accepted 11 January 2008 spectrometry elemental analyses were carried out to determine the interface properties of
the joint. The work showed that the highest interface strength was obtained for the
Keywords: specimens joined at 850 °C for 90 min. It was seen from the hardness results that the highest
Diffusion welding/bonding hardness value was obtained for the interlayer material and the hardness values on the both
Titanium sides of the interlayer decreased gradually as the distance from the joint increased. In
Interlayer energy dispersive spectrometry analyses, it was seen that the amount of silver in the
Microstructure interlayer decreased markedly depending on the temperature rise. In addition, increasing
diffusion time also caused some slight decrease in the amount of silver.
© 2008 Elsevier Inc. All rights reserved.
⁎ Corresponding author.
E-mail address: nizamettinkahraman@gmail.com (N. Kahraman).
1044-5803/$ – see front matter © 2008 Elsevier Inc. All rights reserved.
doi:10.1016/j.matchar.2008.01.015
1482 M A TE RI A L S C H A RAC TE RI ZA T ION 5 9 ( 2 00 8 ) 1 4 8 1–1 4 9 0
Weight (%) 0.0986 0.022 0.0307 0.015 0.0183 0.0363 0.0233 0.006 0.026 0.0586 0.001 Balance
a recommended joining method [17–19]. Diffusion bonding is a applied. The transverse microhardness measurements across
solid-state bonding method [20]. Diffusion bonding provides a the silver interlayer, the two interfaces (titanium-silver and
novel joining operation for similar and dissimilar materials steel silver) and the base materials were carried out. One of the
without gross microscopic distortion and with minimum di- microhardness measurements was taken in the centre of the
mensional tolerance [21,22] and almost no phase transforma- interlayer and the others on both sides of the bonded
tion or microstructural change occurs during the process [23]. specimens by the distances of 25, 40, 40, and 200 µm away
Diffusion bonding can minimise structural in-homogeneities from the silver interlayer. Three measurements were carried
due to negligible effect of temperature gradient, which results out from each point and the results were averaged. From the
in considerable cost and weight savings in comparison to tra- diffusion bonded assemblies a transverse section was taken
ditional joining technique and provides a near net shape form- and then prepared by usual techniques (grinding and polish-
ing process [24]. ing) for metallographic observation. The Ti side was etched
The present study considers the shear strengths of diffu- with a mixture of 73% H2O–16% HF–6% HNO3–5% HCl while the
sion bonding of commercially pure titanium and low carbon low carbon steel side was etched with 2% nitric acid + 98%
steel using silver as interlayer at the temperatures of 700, 750, methanol. A NIKON Epiphot 200 optical microscopy was used
800, and 850 °C. Four different bonding durations (30, 60, 90 for the microscopic examination of the etched specimens.
and 120 min) were used in the study. This investigation also Scanning electron microscopy (SEM) examinations were car-
examines the influence of bonding temperature and diffusion ried out on these specimens using a JEOL 6060 LV SEM device
time on the interface microstructure and tensile-shear proper- and the diffusion zones were analysed by energy dispersive
ties of the bonded assemblies. spectrometry (EDS).
In this study, commercially pure titanium (ASTM Grade 2) was The results of diffusion bonding operations showed that bon-
bonded to low carbon steel by diffusion bonding method. The ding was effected for almost all the conditions. On the other
bonding was carried out using a silver interlayer, which was hand, bonding at 700 °C and for 30 and 60 min of diffusion times
supplied in sheets of 10 × 10 × 0.08 mm. The hardness of the could not be achieved. The failure of bonding at 700 °C for 30 and
original materials were measured as 122, 132, 268 HV for low 60 min of diffusion times can be attributed to both the low
carbon steel, titanium and silver, respectively. Chemical temperature and the insufficient diffusion times. When diffu-
analyses of all the materials are given in Tables 1, 2, and 3. sion time was increased to 90 min or bonding temperature was
Specimens were prepared in the dimensions of 40 × increased to 750 °C without any increment in diffusion time,
10 × 1.5 mm and all the specimens' surfaces were subjected bonding could be effected. It is well known that adequate heat,
to mirror-like polishing using the conventional metallo- diffusion time, and pressure are required for atoms to diffuse in
graphic polishing steps. And then, they were cleaned by this bonding method. Diffusion time is a dependent operation
alcohol prior to the welding. Samples were then placed in the parameter and is interrelated with temperature, pressure, and
chamber of the diffusion welding equipment (Fig. 1). The the type of bonding. Time needed for bonding different
samples were oriented as shown in Fig. 2. In order to eliminate
the oxidation problem, Ar gas was introduced into the test
chamber during welding. Temperature was then increased up
to the test temperature in steps of 20 °C/min and the samples
were kept there for predetermined diffusion times under
3 MPa uniaxial load and then cooled down to the room tem-
perature. Welding parameters for these experiments are given
in Table 4.
To determine the mechanical properties of the bonding,
tensile-shear test was carried out on the bonded specimens
(Autograph-Shimadzu) with the speed of 1 mm s− 1. Hardness
specimens were mounted in bakelite. Microhardness was
measured using a Shimadzu HMV unit and 200 g load was
Ti–Ag–Fe 1 700 30
Ti–Ag–Fe 2 700 60
Ti–Ag–Fe 3 700 90
Ti–Ag–Fe 4 700 120
Ti–Ag–Fe 5 750 30
Ti–Ag–Fe 6 750 60
Ti–Ag–Fe 7 750 90
Ti–Ag–Fe 8 750 120
Ti–Ag–Fe 9 800 30 Fig. 2 – Dimensions of the diffusion bonded specimens (mm).
Ti–Ag–Fe 10 800 60
Ti–Ag–Fe 11 800 90 materials or material couples can vary from several seconds to
Ti–Ag–Fe 12 800 120
several hours. Longer diffusion time is not only disadvanta-
Ti–Ag–Fe 13 850 30
Ti–Ag–Fe 14 850 60
geous for bonding economy, but also it leads to some undesir-
Ti–Ag–Fe 15 850 90 able effects which deteriorate the mechanical properties of
Ti–Ag–Fe 16 850 120 bonding such as; porosity formation, alteration of the composi-
tion and formation of brittle intermetallic compounds [25].
Fig. 3 – Test graphs of tensile-shear tests for the specimens bonded at (a) 700 °C, (b) 750 °C, (c) 800°C and (d) 850 °C for 120 min.
1484 M A TE RI A L S C H A RAC TE RI ZA T ION 5 9 ( 2 00 8 ) 1 4 8 1–1 4 9 0
Fig. 5 – Hardness results taken from the specimens bonded at (a) 700, (b) 750, (c) 800 and (d) 850 °C.
M A TE RI A L S C H A RAC TE RI ZA T ION 5 9 ( 2 00 8 ) 1 4 8 1–1 4 9 0 1485
Fig. 6 – Macrostructures of the specimens obtained at 750 and 850 °C for various diffusion times.
In their study, Peng et al. [4] stated that strength increased interlayer as distance from the joint increases. In addition, it
with increasing diffusion time up to a certain point and then it was determined that hardness values taken from the speci-
decreased due to intermetallic formation in diffusion welding. mens (titanium, low carbon steel, and silver as interlayer)
Ghosh and Chatterjee [26] bonded pure titanium and 304 bonded at 700, 750, and 800 °C are lower than the values taken
stainless steel couples at 950 °C for diffusion times of 30, 60, 90 from the original materials. However, the hardness value of
and 120 min and determined that 30 min of diffusion time led the silver interlayer of the specimen bonded at 850 °C is sig-
to the highest strength. They also determined that strength nificantly higher (about 450 HV). The decrease in hardness
decreased sharply with increasing diffusion time. In their values after bonding can be attributed to the decrease in
work, this sharp decrease was attributed to the growth of number of dislocations during bonding, which were relatively
intermetallic compounds and formation of voids. In a similar abundant in the original material. Another reason for this
study, Liming et al. [27] bonded different metallic materials reduction in hardness may be grain growth which occurs in the
at various diffusion temperatures and reported that shear both materials due to high temperature and long diffusion time.
strength increased by diffusion temperature. When the hardness values measured on the interlayer of
the bonded specimens are compared to each other, it can be
3.2. Hardness Test seen that hardness increases with increasing temperature,
however, there is no evidence of change in hardness depend-
Fig. 5 shows the hardness test results obtained from the ing on the diffusion time. Increasing hardness with increasing
diffusion bonded joints. When the curves in Fig. 5 are gene- temperature can be attributed to the formation of interme-
rally examined, it is seen that the highest hardness value tallic compounds at high temperatures.
among the all specimens belongs to the interlayer material Kolukisa [28], Orhan et al. [19], and Yildirim and Keleste-
and hardness decreases gradually at the both sides of the mur, [29] bonded various materials by diffusion bonding at
Fig. 8 – Microstructures of the specimens bonded at 700 °C for diffusion times of 90 and 120 min.
different temperatures. They reported that the highest hard- (Rene 80) using a nickel alloy interlayer at different environ-
ness values were obtained from interfaces and the hardness ments. They reported in their study that the highest hardness
decreased as the distance from the interface increased. was observed at the interface and that the hardness decreased
Similarly Ekrami et al. [30] bonded nickel based super alloys as the distance from the interface increased.
Fig. 9 – Microstructures of the specimens bonded at 850 °C for diffusion times of (a) 30, (b) 60, (c) 90 and (d) 120 min.
M A TE RI A L S C H A RAC TE RI ZA T ION 5 9 ( 2 00 8 ) 1 4 8 1–1 4 9 0 1487
Fig. 10 – EDS and EDS line element analysis taken from the interlayer of the specimen bonded at 700 °C for 120 min.
Fig. 11 – EDS and EDS line element analysis taken from the interlayer of the specimen bonded at 850 °C for 120 min.
1488 M A TE RI A L S C H A RAC TE RI ZA T ION 5 9 ( 2 00 8 ) 1 4 8 1–1 4 9 0
3.4. Microstructure
Fig. 7 shows the microstructure of the low carbon steel and the
titanium before they were diffusion welded. Both materials
originally consist of equiaxed grains and the grains are almost
similar in size.
The microstructures of the joints bonded at 700 °C are
similar to those of the original materials and their grain sizes
are also the same as those of the original materials, Fig. 8.
However, grain growth occurs due to the temperature rise in
the microstructures of the joints bonded at 850 °C, Fig. 9.
Microstructural analysis indicates that the change in grain
morphology is more obvious for the titanium with the in-
creasing diffusion temperature and time than for the steel.
Equiaxed and more homogeneous grains are seen in these
specimens due to absence of HAZ (heat affected zone), which
Fig. 12 – (a) Weight percent of silver in the interlayer versus exist in the fusion welding methods.
temperature and time (b) weight percent of silver and copper Grain growth in bonded materials can be attributed to
versus temperature for 120 min. recrystallization and to the enveloping of small grains by
bigger ones. The tendency for grain growth after recrystalliza-
tion is related to grain boundary energy. In order to obtain a
3.3. Macroscopic Examination lower level of energy, total grain boundary per unit volume
needs decreasing and this, in turn, requires the growth of
The effects of temperature and diffusion time on bonding area grains. However, it is well known that grain growth is not
were examined in detail using an optical microscope. The desirable [31,32].
photos of the bonding areas were taken before the etching, Fig. 6.
From the optical macroscopy, the bonding region decreased in 3.5. SEM and EDS Examinations
area with increasing temperature and diffusion time for all the
specimens. If it is considered that diffusion bonding is generally The SEM and EDS analyses were performed on the silver
effected at four stages (a—plastic deformation under load, b— interlayer of the specimens diffusion bonded at 700 and 850 °C
for diffusion time of 120 min. The SEM and EDS analysis
Fig. 13 – Weight percent variations of silver and copper versus Fig. 14 – Weight percent variations of copper and silver at
the diffusion time at 850 °C. different temperatures for 120 min.
M A TE RI A L S C H A RAC TE RI ZA T ION 5 9 ( 2 00 8 ) 1 4 8 1–1 4 9 0 1489
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