Int.

Journal of Refractory Metals and Hard Materials 56 (2016) 18–26

Contents lists available at ScienceDirect

Int. Journal of Refractory Metals and Hard Materials

journal homepage: www.elsevier.com/locate/IJRMHM

An investigation on metallurgical characteristics of tungsten based tool

materials used in friction stir welding of naval grade high strength low
alloy steels
S. Ragu Nathan a,⁎, V. Balasubramanian b, S. Malarvizhi b, A.G. Rao c
a
Department of Manufacturing Engineering, Annamalai University, Annamalai Nagar 608 002, Tamil Nadu, India
b
Centre for Materials Joining & Research (CEMAJOR), Department of Manufacturing Engineering, Annamalai University, Annamalai Nagar 608 002, Tamil Nadu, India
c
Marine Materials Division, Naval Materials Research Laboratory (NMRL), Ambernath, Mumbai 421 506, Maharastra, India

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

Article history: A non-consumable tool is a vital requirement for friction stir welding (FSW) of high melting point alloys such as
Received 26 August 2015 steel and titanium. In this investigation, an attempt was made to understand the pre-weld and post-weld micro-
Received in revised form 20 November 2015 structural characteristics of three tungsten based alloy FSW tools viz. 90%W, 95%W and 99%W. A naval grade high
Accepted 11 December 2015
strength low alloy (HSLA) steel plates of 5 mm thickness were welded using the above tools with a tool rotational
Available online 15 December 2015
speed of 600 rpm and welding speed of 30 mm/min. Microstructural characteristics of the FSW tools, before and
Keywords:
after welding, were analyzed using optical microscopy (OM) and scanning electron microscopy (SEM) with
Friction stir welding energy dispersive spectroscopy (EDS). From this investigation, it is found that the tool made of 99% W doped
HSLA steel with 1% La2O3 exhibited microstructural stability at elevated temperatures during FSW process.
Tool material © 2015 Elsevier Ltd. All rights reserved.
Tool life
Microstructure

1. Introduction advantage of the FSW process itself. However, the tool should withstand
and counter various forces generated at the initial plunge stage along
Friction stir welding (FSW) is a promising solid state joining tech- with other factors and the tool also should traverse in the weld direc-
nique for welding of high melting point alloys such as steel, titanium tion. The tool pin is responsible for plasticizing the stir zone, excavating
and nickel. FSW is known for green, high productive welding technolo- the softened material from advancing side to retreating side and consol-
gy with lower emission of harmful gases as compared to fusion welding idating beneath it so as to begin the next cycle [5]. Almost care is
process [1]. Mechanical action in the form of frictional stirring on the required to avoid interaction gap between consecutive cycles, which
base material modify the coarse grain microstructures into fine grains eliminates defects like wormholes, pin hole, tunnel defect, etc. at the
due to plastic deformation and fast cooling rate [2]. Welding of steels advancing side [6].
will be affected by both the temperature and composition which Jiye et al. (2014) explained the tool wear mechanism of W–La tool
extensively affects the microstructure evolution. Tool wear and plastic and advocated the use of conical pin with large pin length as compared
deformation are the two major problems encountered during FSW of to smaller one for better stability [7]. Hence, the taper conical larger pin
high melting point alloys (L80 steel) [3]. The tool wear is either due to was mostly recommended. During the tool transverse motion, the tool
mechanical damage or chemical affinity of the tool and work piece; shoulder should support the pin by generating optimum heat to plasti-
however, the plastic deformation is associated with the variation in cize the parent material which in-turn reduce the flow stresses. This
stress, strain rate and temperature during FSW. Therefore, the tool supportive heat generation should be uniform throughout the weld
must withstand high frictional and resultant forces experienced by the length. The variation in flow stresses during welding will lead to pin
pin during initial plunge stage [4]. damage resulting in poor weld quality. Consolidation of the material
Most of the tool failures are reported during plunge stage, thus extruded is secondary function of the shoulder. The tool distortion
resulting in poor stirring and non-uniform grain refinement of the such as expansion or contraction, rubbing wear and if any one of the
parent material in stir zone and thereby, violating the primary situation prevails will lead to poor weld quality, loss of tool pin, and
severe plastic deformation [8].
Much of the tool degradation may be attributed to the high heat
⁎ Corresponding author.
E-mail addresses: [email protected] (S. Ragu Nathan), [email protected]
(temperature around 1200 °C) and stresses generated during FSW of
(V. Balasubramanian), [email protected] (S. Malarvizhi), [email protected] steel. The brittle tendency of the polycubic boron nitride (PCBN) tool
(A.G. Rao). used for FSW of steel and titanium alloys can cause tool breakage due

http://dx.doi.org/10.1016/j.ijrmhm.2015.12.005
0263-4368/© 2015 Elsevier Ltd. All rights reserved.
 S. Ragu Nathan et al. / Int. Journal of Refractory Metals and Hard Materials 56 (2016) 18–26 19

Table 1
Chemical composition (wt.%) of the base metal.

C Mn N Si Mo Ti V Nb Ni Cu Al W

0.08 1.42 0.015 0.19 0.02 0.016 0.032 0.035 0.69 0.126 0.032 0.04

to sudden spike in load or vibration during tool plunging and traversing

[9]. Apart from the tool material selection, researchers had also investi-
gated other possibilities to reduce tool wear and breakage such as pilot-
hole and partial penetration. However, the problems are not solved yet
completely. Recent developments in the tool material, tool design and
processing strategies fetters feasibility of friction stir welding of high
melting temperature materials.
Tool cost is also considered as important factor, which restricts the
application of FSW technology for steels. However, the tungsten base al-
loys are cheaper than W-Re/W-Re-HfC/PCBN tools. Therefore, tough
tungsten base alloys were selected as FSW tool materials for the present
investigation. Tungsten has a high energy threshold for physical
sputtering and offers distractive physical properties which includes
the highest melting point of all metals, the lowest vapor pressure,
good thermal conductivity and high temperature strength and tough-
ness [10]. Also, these alloys that contain small amount of impurities
are known to increase the high temperature creep resistance.
Hence, in this investigation, high strength low alloy (HSLA) steel was
welded using FSW process to check the feasibility of tungsten based tool
materials. As the tool experiences severe temperature and forces during
FSW, it is appropriate to investigate the microstructural characteristics
of tungsten base alloy tools before and after welding.

2. Experimental

The rolled plates of 5 mm thick high strength low alloy (HSLA) steel
were used as base material. Plates were machined to the dimensions of
150 × 300 mm (width and length) to get the final weld coupon size of
300 mm × 300 mm. The chemical composition and mechanical proper-
ties of the base metal are presented in Tables 1 and 2 respectively.
The microstructural features of base metal are shown in Fig. 1 and it Fig. 1. Micrograph of base metal. a. Optical micrograph; b. SEM micrograph.
primarily consists of ferrite with small amount of pearlite. The three dif-
ferent grades of tungsten base alloy were used as the tool materials in
the present investigation to weld HSLA steel. The tool was produced Table 3
Chemical composition (wt.%) of the tool materials.
by powder metallurgy route and supplied by M/s. Heavy Alloys
Penetrator Project (HAPP), Tiruchirappalli, India. The chemical compo- Tool designation W Ni Fe Mo Co La2O3
sition and the mechanical properties of tool materials are presented in W90 90.11% 5.96% 3.56% 0.22% 0.15% –
Tables 3 and 4, respectively. Tool materials are designated as W90, W95 95.09% 3.01% 1.73% 0.11% 0.06% –
W95 and W99 for the purpose of convenience. W99 tool was made by W99 99% – – – 1%
doping 1% Lanthanum Oxide (La2O3) in 99% tungsten and other two
tools (W90, W95) were made by powder metallurgy route.
The tools were machined to the dimensions and configuration as torque throughout the weld (Fig. 2a). The welding parameters used to
shown in Fig. 2. Based on our earlier experience (Balasubramanian fabricate the joints are presented in Table 5.
et al., 2009) in FSW of stainless steel, tool configuration is expected to The weld bead appearance of the joints is displayed in Fig. 3. After
be more effective in preventing tool wear and failure [8]. Using these the welding process, tools were sliced for postweld tool metallographic
three tools, HSLA steel plates were joined by FSW process. The process examination. Specimens were extracted and sectioned to the required
was done in “worst-case set-up” that is, without using shielding gas, sizes from the tool materials before and after the weld as shown in
pre-heating the base metal, etc. A designated tool holder with cooling Fig. 3a and then polished using different grades of emery papers. Final
arrangement was also not used to hold the tool, which avoids escaping polishing was done using the diamond compound (0.1 μm of particle
of tool from the holder and in turn it supports and maintains the same size) in the disc polishing machine. Polished specimens were then

Table 2
Mechanical properties of the base metal.

0.2% offset yield strength Ultimate tensile strength

Elongation in 50 mm gauge length (%) Impact toughness @ RT (J) Hardness of base metal @ 0.5 kg load (HV)
(MPa) (MPa)

540 610 24 62 270

20 S. Ragu Nathan et al. / Int. Journal of Refractory Metals and Hard Materials 56 (2016) 18–26

Table 4
Mechanical properties of the tool materials selected.

Tool designation Density 0.2% offset yield strength Ultimate tensile strength Elongation in 11.35 mm Vickers's hardness of tool
(g/cm3) (MPa) (MPa) gauge length (%) material @ 0.5 kg load (HV)

W90 18.70 850 1100 20 570

W95 18.62 1190 1400 14 610
W99 18.92 1210 1475 11 506

etched with solution of ammonia mixed with a small amount of hydro-

Table 5
gen peroxide to reveal the microstructure of the tool specimens. Process parameters and welding conditions used to fabricate joints.
Microstructural examination was carried out using a light optical
Rotational speed (rpm) 600
microscope incorporated with an image analyzing software. Field-
Welding speed (mm/min) 30
emission scanning electron microscopy (FESEM) with attachment of D/T ratio of tool 5
energy dispersive spectroscopy (EDS) was used to reveal the Tool shoulder diameter (mm) 25
micrograph and to detect elements present in the tool material. The Pin length (mm) 4
phases present in the pre- and post-weld tool material were identified Tool inclined angle (°) 0

by X-ray diffraction.

3. Results

3.1. Evaluation of tool degradation

Fig. 4 clearly reveals the macrographs of all the three tungsten base
alloy tools used in this investigation before and after friction stir
welding of HSLA steels. W90 tool experienced maximum deformation
and thus ended in mushrooming effect (Fig. 4c). The tool visually
deformed during initial plunging stage itself. Upon retraction, the
tool was visibly inspected and the extent of deformation was
confirmed. The deformation and tool wear were observed in pin
and shoulder regions (Fig. 4d) due to flow stresses generated in the
base material during FSW. W90 tool was able to weld 130 mm of
length only.
On the other hand, W95 tool showed better performance compared
to W90 tool but the damage on the top region of the tool pin is observed
(Fig. 4e). Pin damage was clearly shown in Fig. 4f. In contrast, severe
deformation, tool wear and pin damage were not observed in the
W99 tool (Fig. 4g). Fig. 4h illustrates the dimensional stability of the
W99 tool and no wear or deformation was observed. Further
understanding of microstructural phenomena during FSW could be
done by characterizing the tool materials using optical microscopy
and scanning electron microscopy.

Fig. 3. Photographs of FSW experimental setup and joints fabricated using three different
tungsten based alloy tools. a. FSW experimental setup details; b. joint fabricated by W90
Fig. 2. Photograph of tungsten based alloy tool and tool dimensions. tool; c. joint fabricated by W95 tool; d. joint fabricated by W99 tool.
 S. Ragu Nathan et al. / Int. Journal of Refractory Metals and Hard Materials 56 (2016) 18–26 21

Fig. 4. Photographs and macrographs of tungsten based alloy tools used in FSW of HSLA steel. a. Tool profile; b. configuration of specimen to be extracted; c. W90 tool after welding; d. W90
tool profile after FSW; e. W95 tool after welding; f. W95 tool profile after FSW; g. W99 tool after welding; h. W99 tool profile after FSW.

3.2. Evaluation of microstructural stability at elevated temperature material at elevated temperatures is evident from Fig. 5h & i. The micro-
structure of the tool pin and the shoulder region after FSW are more or
3.2.1. Optical microscopy less similar to raw stock microstructure (before FSW).
Optical micrographs of the pin and the shoulder regions of the tools
before and after welding are depicted in Fig. 5. Grain growth and grain 3.2.2. Scanning electron microscopy
coarsening were observed in all the tools after FSW. Grain coarsening, Fig. 6 presents the SEM micrographs of the postweld W90 tool at low
W/matrix separation was observed at the pin region (Fig. 5b) and the and high magnifications. The tool pin region micrograph (Fig. 6a) re-
compressed grains were observed at the shoulder region (Fig. 5c). veals the adhesive wear and severe deformation of the tool. Coarsened
From the Fig. 5a–c, it is clear that recrystallization occurred in tool ma- tungsten grains and partially melted matrix are visible in the SEM
terial well before its actual recrystallization temperature. This was due image (Fig. 6a) and it illustrates the instability of the tool to withstand
to the instability of the tungsten matrix of W90 tool to withstand the high forces at peak temperature generated by the friction between
thermo-mechanical stresses. Fig. 5d shows the W95 tool raw stock mi- tool and work piece during FSW process. The coupled effect of thermal
crostructure (before FSW) consisting of fine equiaxed tungsten grains and mechanical forces is responsible for the grain growth and removal
merged with the matrix. W-cleavage failure was observed in the tool of softer Fe–Co–Ni phase, thereby resulting in heavy wear of the pin
pin region (Fig. 5e) and the confined amount of compression of W/W and shoulder (Fig. 6b).
grains was also witnessed at the shoulder region (Fig. 5f). The raw mi- Intergranular crack on the pin region and the discontinuous transfer
crostructure (before FSW) of W99 tool is shown in Fig. 5g and it consists layer of work piece are observed in the W95 tool (Fig. 7a). Increase in
of elongated grains with uniformly dispersed oxide at the grains and volume of transfer layer material from the workpiece might have led
grain boundaries. The lanthanum oxide particles pin the grain boundary to increase the sticking torque and sliding force on the tool pin surface
during high temperature deformation and thus restrict the grain growth and resulted in the failure at the corner of the tool pin (Fig. 7a). The
during FSW. The better thermomechanical stability of W99 tool tool undergoes compression due to the upward (extrusion action) and
22 S. Ragu Nathan et al. / Int. Journal of Refractory Metals and Hard Materials 56 (2016) 18–26

Fig. 5. Optical micrographs of tungsten based alloy tools before and after FSW process.

downward (forging action) forces particularly at the tool pin (relatively

small area), tool material loses its densification and crack propagates
along the matrix as portrayed by high magnification SEM micrograph
in the Fig. 7b.
The diffusion of very few elements from the work piece to the tool
was observed in the W99 tool (Fig. 8a) and it demonstrates the
microstructural stability of the tool material at high thermo-
mechanical conditions. However, the high magnification SEM image
shown in Fig. 8b, reveals the deformation and orientation of the grains
on the top region of the tool pin after FSW process.

3.3. Evaluation of transfer layer

Adhesion between tool and the base metal is high in W90 and W95
tools compared to W99 tools (Fig. 9a). Thickness of adhered material
layer increases the stress concentration at the tool pin corner and lead
to cracking, followed by pin failure. Wear resistivity greatly reduced
due to this stress induced crack tip. Whereas no adhesion of workpiece
material is observed on W99 tool surface. Instead of adhesion, tool and
workpiece interaction zone named as reaction zone (a thin layer on tool
pin) is evident and it influences the tool life by reducing severity of grain
deformation as shown in Fig. 8a. Deformation is not observed in W99
tool pin and this may be due to the acceptable range of deformed and
un-deformed grains at the pin top corner to sustain the tool configura-
tion. To identify the formation of new phases or layer present on the
tool pin top region, Backscattered SEM analysis was performed at tool
cross section. The analysis revealed the presence of transfer layer
(Fig. 9b). To reveal the details of phase formation on the tool surface,
electron diffraction spectroscopy (EDS) and X-ray diffraction (XRD)
analysis were carried out and the results are presented in Figs. 10 and
11.
Black dots on the pin top surface are confirmed as work piece mate-
rial. From Fig. 10a, the area selected for EDS is highlighted and pre-weld Fig. 6. SEM micrographs of W90 tool at low and high magnification. a. W90 tool pin top
tool EDS results revealed the presence of lanthanum, oxygen and region at 500×; b. W90 tool pin top region at 2000×.
 S. Ragu Nathan et al. / Int. Journal of Refractory Metals and Hard Materials 56 (2016) 18–26 23

Fig. 7. SEM micrographs of W95 tool at low and high magnification. a. W95 tool pin top Fig. 8. SEM micrographs of W99 tool at low and high magnification. a. W99 tool pin top
region at 100×; b. W95 tool pin top region at 2000×. region at 200×; b. W99 tool pin top region at 5000×.

tungsten (Fig. 10b). Hence, the raw stock tool was confirmed as and inadequate thermal stability of the W90 tool. This is due to
W–La2O3 and Fig. 10c reveals the presence of iron, nickel, tungsten, mismatch in the coefficient of thermal expansion of W-grains and the
and aluminum on the pin top region. Further it was verified and matrix phase. It was also reported by Kim et al. (1998), that intermedi-
confirmed through XRD analysis (Fig. 11). XRD result confirmed the ate temperatures lead to reduce the contiguity of W-grains mainly due
presence of iron and nickel on the W99 tool pin top surface. From this to thermal coefficient variations of W-grain and the matrix phase [12].
analysis, it is understood that the lanthanated tungsten tool (W99) is From the postweld W90 tool micrographs at low and high magnifi-
capable of withstanding high forces and high temperatures during cation (Fig. 6), the W/matrix decohesion, matrix tearing and
FSW of HSLA steel. However, there is a possibility of transfer of elements W-cleavage mechanism were revealed which could be the reason for
from the workpiece to tool by diffusion process. the inferior mechanical properties of W90 tool at elevated tempera-
tures. The results displayed in Table 2b indicate that the W90 tool
4. Discussion material has superior mechanical properties at room temperature
[10]. The recrystallization temperature of the W90 tool is approximately
The selected tool material should possess good mechanical proper- 1000 °C. However, the high temperature during the FSW (nearly
ties at elevated temperature, durable at high torque, high hardness to 1200 °C) along with high forces could have melted the matrix, due to
resist wear and good thermal conductivity. The favorable material the presence of softer Fe–Ni–Co phase. It was also investigated and re-
flow around the tool pin can be catered by suitable tool material ported by Mabuchi et al. (1997) that smaller amount of grain boundary
selected particularly by considering the base metal properties. It may segments does not necessarily lead to high strength at higher tempera-
influence the tool life, weld quality and cost of the tool material too. tures [13]. The hardness difference between W and the matrix also plays
The ability of the tool in FSW process is to lead the material to root major role in load bearing ability and thermal stability at higher temper-
the weld and to plasticize the material under the tool without change atures. The inferior mechanical properties of W90 tool material operat-
in dimension/configuration in the tool profile. In fact, as pointed out ing at higher temperatures were reported, by Jiten et al. (2014), they
by Thompson and Babu (2010), tool degradation in FSW of hard metals opined that the application of tungsten heavy alloys as tool material is
is influenced by flow stresses and welding temperatures that generated restricted mainly due to ductile to brittle transition temperature
during frictional stirring [11]. The formation of mushroom effect, severe (DBTT) and recrystallization temperature of the matrix phase [7].
deformation and adhesive wear shown in the macrostructure (Fig. 4c & Compared to W90 tool material, W95 tool has superior strength,
d) and microstructures (Fig. 5b & c), could be attributed to insufficient toughness, elongation and hardness (Table 2b). Because of the
24 S. Ragu Nathan et al. / Int. Journal of Refractory Metals and Hard Materials 56 (2016) 18–26

Fig. 9. Optical micrograph and backscattered SEM image of the W99 tool after FSW. a. W99
tool microstructure showing the transfer layer of the work piece; b. backscattered image
showing the diffusion of work piece elements in to the W99 tool pin top region.

improved mechanical properties, W95 tool pin has the better load
bearing ability but galling occurred between tool and the work piece Fig. 10. EDS analysis of W99 tool before and after using it in FSW process. a. Backscattrered
interaction (Fig. 4e) which is mainly due to high chemical affinity of image showing the area selected for EDS analysis on the W99 tool; b. EDS result of W99
tool before FSW; c. EDS result of W99 tool after FSW.
work piece and the tool material. The reason for failure observed in
W95 tool (Fig. 4f) is due to the increased sticking torque and local
deformation which might have caused by adhered material on the grains due to uniform distribution of La2O3 [13]. Secondary grain growth
tool. A thick layer formation around the tool pin resulted in increase of and increase in recrystallization temperature are impeded due to fine
local compressive stresses on the pin and led to failure. However, dispersion of lanthanum oxide particles in the matrix and thereby re-
microstructural result shows the failure occurred due to W/matrix sults in high strength and toughness at high working temperatures [15].
decohesion and matrix tearing as shown in Fig. 5e. The local stress gen- Deformation of the grains in the pin region of FSW tool is vital in
erated by increase in sticking torque which could increase the stress preventing the tool wear and degradation. The same was achieved by
concentration at the corners of the tool pin and hence failure occurred. the formation of protective transfer layer on both sides of the pin tip
At the same time, due to compression of vertical force and resultant as shown in Fig. 9a. The protective transfer layer was formed from the
forces from the base metal are likely to reduce the density of the matrix base metal to tool pin surface during interaction of tool with work
and crack propagates through the matrix phase as shown in Fig. 7a and piece at high temperature and load. The protective transfer layer con-
b. Density was also greatly reduced in the W95 tool revealed by pores firmed the presence of W, Fe, Ni and C through pre- and post-weld
formation (Fig. 7a). tool analysis by EDX and XRD (Figs. 10 & 11). This thin protective trans-
Therefore, it is expected that W99 tool (W–La2O3) has a great fer layer acts as a good thermal barrier around the tool pin region and
potential for carrying out FSW due to higher tungsten content with thus assists in reducing the tool wear and deformation [16,17]. Further-
lanthanum oxide particles pining the grain boundaries and higher more the recrystallization temperature of the W99 tool is around
toughness. The microstructural features before and after FSW were 1600 °C which is more than the temperature experienced by the tool
almost similar, confirming the microstructural stability during FSW. during FSW of HSLA steel. Therefore, as compared with other tungsten
The stability of microstructure is mainly due to the presence of lantha- based tools (W90 and W95), W99 tool has better stability at elevated
num oxide particles at the grain boundaries. The ultimate tensile temperature and can be used for FSW of HSLA steel plates of 5 mm
strength of W99 (W–1% La2O3) material at 1000 °C was approximately thickness.
500 MPa [14]. Moreover, the presence of lanthanum oxide particles acts
as a site for dislocation generation as well as impeding the dislocation 5. Conclusions
movement thus having good strength and toughness. Mabuchi et al.
(1997) investigated and reported that dislocation movement was great- In this investigation, an attempt was made to analyze the micro-
ly influenced by particle interaction and substructure formed in the structural changes that occurred in tungsten base tool materials during
 S. Ragu Nathan et al. / Int. Journal of Refractory Metals and Hard Materials 56 (2016) 18–26 25

Fig. 11. XRD results of W99 tool. a. XRD results (before FSW); b. XRD results (after FSW).

friction stir welding of HSLA steels. The important conclusions derived iii. From this experimental investigation, it is understood that tool de-
from this investigation are given below. formation and wear manifestation during FSW of harder alloys
could be overcome successfully by proper selection of tool material,
i. Of the three tungsten base tool materials used in this investigation, tool design and process parameters.
W99 (W–1% La2O3) tool exhibited better microstructural stability
without undergoing physical (dimensional) changes in tool configu-
ration.
ii. It was found that the tool made of 99% W and 1% La2O3 withstood Acknowledgments
high strain rate, temperature and flow stresses generated during
FSW of HSLA steel. This is mainly due to the microstructural stability The authors are grateful to The Director, Naval Materials Research
of the tool material and formation of protective transfer layer during Laboratory (NMRL), Ambernath for financial support through CARS pro-
FSW of HSLA steel. ject No: G8/15250/2011 dated 29.02.2012 and providing base material
26 S. Ragu Nathan et al. / Int. Journal of Refractory Metals and Hard Materials 56 (2016) 18–26

for this study. The authors would like to express their thanks to Mr. V.K. [8] A.K. Lakshminarayanan, V. Balasubramanian, An assessment of microstructure,
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