The International Journal of Advanced Manufacturing Technology

https://doi.org/10.1007/s00170-019-04243-7

ORIGINAL ARTICLE

Fabrication and characterization of AA6061/CNTs surface

nanocomposite by friction stir processing
Hussnain Riaz 1 & Tareq Mnazoor 2 & Ali Raza 3

Received: 12 March 2019 / Accepted: 31 July 2019

# Springer-Verlag London Ltd., part of Springer Nature 2019

Abstract
Aluminum matrix composites (AMCs) are among the advanced materials that are employed in numerous industrial applications.
AMCs have good stiffness and strength. They have low weight that makes them valuably handy for improving fuel efficiency and
economy in the structures made from them. The friction stir processing (FSP) is a novel technique which is highly advantageous
for producing composites, which are reinforced with particles that are sub-micron in size particularly in light weight metal matrix
composites (MMCs). Current study is done to examine the potential of AA6061-based surface nanocomposites by reinforcing it
with carbon nanotubes (CNTs) (as-received and purified) employing FSP. Fabrication of the composites is carried out by filling
CNTs into the grooves of different sizes and friction stir processed (FSPd). Various parameters are investigated to attain best
mechanical properties and dispersion of CNTs in the matrix. Metallography is used to reveal the material flow and grain size
variation in the zones formed by the FSP. Micro hardness and tensile tests are conducted to evaluate the mechanical properties and
an increase of 47.3% hardness and an increase of 32.4% ultimate tensile strength (UTS) are observed from the base FSPd
material. Electron microscopic techniques are also employed to reveal the microstructural details.

Keywords Aluminum matrix composites . Friction stir . CNTs . Tensile . Microstructure

1 Introduction technique that, in a single pass, improves the mechanical prop-

In loads of industrial applications, primarily in aerospace, au-
tomotive, and railway industries, material selection with spe-
cific properties is of paramount importance. However, cost
and time of production are the limiting factors to produce
the alloys with specific properties like high strength. But, if
we increase strength, ductility goes down. Hence, to flourish
processing techniques by which high strength and high duc-
tility at the same time by keeping in check, the time of pro-
duction and cost are needed [1, 2]. FSP is a new processing
* Tareq Mnazoor
tareqmanzoor@cuilahore.edu.pk
1
Dalian University of Technology, Dalian, China
2
COMSATS University Islamabad, Lahore Campus, Lahore, Pakistan
3
COMSATS University Islamabad, Sahiwal campus,
Sahiwal, Pakistan
erties and microstructure of a material with less time and cost.
In FSP, a revolving tool pin is sticked to the surface of a
material to be welded and crossed through its surface. Plastic
and friction distortion produced by tool is used to heat the
workpiece and make it soft. The local region is then modified
by the rotating pin [3]. When reinforcement like CNTs is
added in a groove or hole to form a composite, they are dis-
persed uniformly in the stirred zone by the tool [4]. FSP offers
many advantages over the conventional processes like the use
of low-cost tool, robust finishing process requirement, utiliza-
tion of easily accessible machine tool technology, automation
suitability, energy efficiency, and environmental friendliness.
The addition of CNTs into different matrices as a reinforce-
ment is getting a lot of interest in research community. In
addition to higher chemical and thermal stability, CNTs have
the capacity to exhibit high yield strength (YS) and elastic
modulus values. CNTs have an ability to work as strengthen-
ing agents by the process of preventing atomic movements [3,
5–10]. Thus, CNTs have great potential as reinforcement in

Fig. 1 Typical FSW system
making composites. CNTs in polymeric matrix composites
(PMCs) and ceramic matrix composites (CMCs) are already
being used [7]. But few have explored the MMCs with CNTs
reinforcements [11–14]. A schematic diagram of friction stir
welding is shown in Fig. 1.
Nanocomposites are multiphase materials in which one of
the phases has at least one dimension less than 100 nm, or
there are some structures which have nanoscale repeated dis-
tance among the phases. Reinforcement in case of nanocom-
posite may have different morphologies like particles, sheets,
and fibers [14–17]. Since the last decade or so, a lot of re-
search has been carried out incorporating CNTs in composites
as reinforcement with matrices like polymers, metals, and ce-
ramics. Now with the development of newer and better tech-
niques like FSP and equal channel angular processing
(ESAP), gradual increase in the number of publications on
CNTs-reinforced MMCs can be expected [6, 11, 18–24].
FSP has many advantages like friction stir processing
(FSP) to boost superplasticity and formability of materials
with low melting point [25], friction stir casting modification
commonly identified as friction thermomechanical processing
[26], friction stir microforming [27], friction stir powder pro-
cessing [28], and friction stir channeling [23–29].
The system breaks up the weld zone into different regions,
as follows:
& Unaffected material/parent metal: The material away from
the weld is unaffected.
Table 1 Composition of AA6061
Element Al Si Mg Fe Mn Cu Others
Mass % 96.4 0.8 1.2 0.7 0.15 0.4 0.3
Int J Adv Manuf Technol
& Heat-affected zone (HAZ): The domain of materials af-
fected by the thermal effects produced in the weld and it
modifies the mechanical properties and microstructure.
& Thermomechanically affected zone (TMAZ): The materi-
al undergoes plastic deformation, and is also affected by
the heat produced by the FSW tool.
& Weld nugget/stir zone (SZ): This region is fully recrystal-
lized, also called the stir zone [30].
Friction stirring has the following notable benefits in con-
trast to other techniques for metal working.
& Densification, homogenization, and microstructural mod-
ification can be achieved in one process.
& Control of microstructure and along with it mechanical
properties is obtainable by optimization of process param-
eters, design of tool, and thermal cycles through which
material undergoes processing.
& The depth of the composites which are processed can eas-
ily be obtained by adjusting the pin length of the tool. This
alteration of thickness is very difficult to emulate or even
attain through other process.
& This technique is quite flexible in terms of making, devel-
oping, and processing of variety of materials.
& As no after machining and treatments are required, this
process becomes very economical, efficient in energy us-
age, and also friendly to the environment.
& The dimensions of the component produced remain al-
most identical before and after processing [31].
Friction stir welding of materials with low melting
point is getting very popular. Hundreds of commercial
and defense companies from different parts of the world
like Lockheed Martin, Boeing, Airbus, US Navy,
Mitsubishi, and Kawasaki are already using it [31, 32].
Int J Adv Manuf Technol

Fig. 2 Schematic of the plate with

groove (1 mm × 3 mm) having
backing plate and clamps

Fig. 3 a Groove made in the

plate. b Side view of the groove

Fig. 4 Tool geometry

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Fig. 5 Annealing cycle of the tool

[48–52]

Fig. 6 Austenitizing and air

quenching [48–52]

Fig. 7 Tempering treatment

[48–52]
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Fig. 8 Flow chart for the

fabrication of AA6061/CNTs
surface composites

Table 2 Compositions and process parameters for FSP composites produced

CNTs Sample no. Rotational speed (RPM) Linear speed (mm/min) Groove depth (mm) Groove width (mm)

As received 1 1180 95 1 0.5

As received 2 1180 95 2 0.5
As received 3 1180 95 3 0.5
As received 4 1180 95 3 1
None 5 1180 95 - -
Purified 1 1180 95 1 0.5
Purified 2 1180 95 2 0.5
Purified 3 1180 95 3 0.5
Purified 4 1180 95 1 3
None 5 1180 95 – –
As received 1 1500 95 1 0.5
As received 2 1500 95 2 0.5
As received 3 1500 95 3 0.5
As received 4 1500 95 3 1
None 5 1500 95 - -
 Int J Adv Manuf Technol

Raman spectrum of SWCNTs showed that CNTs sur-

vived under the high process temperature, stresses, and
strains involved in FSP of the material [34].
A healthy number of investigators have successfully
fabricated composites with friction stir processing either
on the surface or as a bulk. Reinforcements used are
primarily micro to nanoscale level. In some cases, FSP
with some other processes like deposition and powder
metallurgy was combined to get added benefit of these

Fig. 9 CNTs filled into the slot before friction stir processing these into
sheet

To achieve the desired combination of properties within

a structure, one can use surface modification in local-
ized regions. This means that a gradient of properties
within a structure is available. This method enhances
and broadens the design capabilities of MMCs surfaces.
CNTs survivability is vital for better and usable com-
posite. So its study is a must, as FSP involves high
stresses, temperatures, and strains. Thermomechanical
processing involved can destroy or damage CNTs. Lim
et al. [33] have also shown that CNTs can survive in
aluminum-based composite made by friction stir lap
welding of 7075-T6/6111-T4 [33]. Johannes et al. [34]
have investigated the survivability of CNTs during the
friction stir processing of an aluminum alloy. They have
introduced single-walled carbon nanotubes (SWCNTs)
into 6.4-mm thick 7075Al plate using friction stir pro-
cessing and analyzed the fracture surface of tensile sam-
ples taken from the region that was friction stir proc-
essed with CNTs. SEM analysis and characteristic

Fig. 11 a Groove of dimension 1 mm × 3 mm filled with CNTs and

friction stir processed into the 6061Al sheet. b Reference friction stir
Fig. 10 20 HP conventional vertical milling machine at HMC (II) Taxila, pass done without reinforcement. c Failed FSP specimen. d Failed
Pakistan, used for friction stir processing specimen cross-section
Int J Adv Manuf Technol
Fig. 12 Schematic of FSP of
aluminum alloy with CNTs as
reinforcement
Fig. 13 Hardness profile
markings for indents
processes. Composite made on the surface by FSP
shows better surface and wear properties along with
tougher core material makes them better as compared
with simple metallic or metal matrix composites
[35–38]. Achievement of best properties in surface met-
al matrix composites (SMMCs) is critically dependent
on the selection of the reinforcement [39–42]. Liu
et al. [43] have fabricated aluminum-based CNTs com-
posites by powder metallurgy and then friction stir proc-
essed it, achieving yield strengths 23.9% and 45.0%
respectively by varying CNTs from 1 to 3% by weight.
Lim et al. [33] also fabricated aluminum alloy 6111-T4+
7075-T6 with CNTs by friction stir welding and obtain-
ed a rise of 50% in hardness with 7.8% reinforcement
of CNTs. Morisada [44] developed a magnesium alloy–
Fig. 14 Schematic of tensile
specimen used for tensile test
based nanocomposite reinforced with CNTs and
achieved 90% increase in hardness. Johannes et al.
[34] have shown that CNTs can survive during severe
conditions of FSP in a 7075 aluminum alloy but their
agglomeration rendered any improvement in mechanical
properties negligibly. Misak [45] had analyzed what dif-
ference the variation of dimensions to the grooves
makes and shown that shallow and narrow grooves
show better dispersion of CNTs. He used CNTs with
aluminum powder and 2024-T3Al to make composite
and also studied flow patterns made by the CNTs.
Luick [46] used single-walled CNTs in aluminum matrix
and done FSP on it and rolled it afterwards to check the
effect of CNTs on thermal conductivity but found no
improvements. Wasim [47] used as-received CNTS in
 Int J Adv Manuf Technol

Fig. 15 Dimensions of tensile

sample

aluminum matrix and achieved an increase in mechani-
cal properties after FSP. The objectives of current work
are:
1. To develop CNTs-reinforced aluminum alloy (AA6061)
matrix composite using FSP.
2. To get better dispersion of the reinforcement, i.e., CNTs
into the alloy matrix as better mechanical properties are
linked with good dispersion.
3. To study the influence of as-received and purified CNTs
on the mechanical properties of the composite produced.
4. Process parameter variation to get better mechanical
properties.
The paper is subdivided into four sections. In the first sec-
tion, introduction is given; in the second section, experimental
work is given; and in the third section, results are discussed. In
the fourth section, comparison with earlier work is given and
finally the whole work is summarized.
2 Experimental
A schematic of the plate along with groove (U type),
clamping with nut and bolt, and backing plate is shown
in Fig. 2. Deep grooves measuring 1 mm, 2 mm, and
3 mm were cut lengthwise at the middle top surface of
the plates by slotting saw of 0.5 mm and 1 mm thick-
nesses by vertical milling machine (VMM). Different
angles of the groove cut are shown in Fig. 3a, b.
Carbon nanotubes were used as reinforcements to produce
the FSP composites. The CNTs used were as received from
Sky Spring Nanomaterials, Inc., Houston, USA, having a di-
ameter of 20–30 nm and their purity level was 95%.
2.1 Friction stir processing tool fabrication
A rod of H13 steel having a diameter of 25 mm was cut into
the required length and machined to get the desired dimension
friction stirring tool. A 25-mm shoulder diameter with a con-
cavity of 5°, a threaded (1.5 mm pitch) cylindrical pin tapered
at 10° with a base diameter of 4.5 mm and length of 4 mm
with rounded edge, was machined using a conventional lathe.
The actual and schematic of the tool fabricated are shown in
Fig. 4.

Rolled sheet of aluminum alloy AA6061 having the

composition as shown in Table 1 with 5 mm thickness 2.2 Tool heat treatment
was used in this study as a matrix. Specimens with
dimensions of 200 mm × 100 mm were cut out of it. Tool heat treatment was done in order to increase its
hardness. Initially its hardness was 8–12 HRC and after
Table 3 Specimen dimensions heat treatment, it reached 53–57 HRC [48–52]. It need-
Parameters Dimensions (mm) ed heat treatment because low hardness of the tool
made it sticks to the aluminum matrix and produces a
G, gage length 25 very rough top surface as shown in Fig. 11c. First an-
W, width 6 nealing of the tool was done at 850 °C for 2 h by
T, thickness, max 5 (6 max) heating the tool from room temperature in steps. After
R, radius of fillet, min 6.5 (6 min) annealing, austenitizing at 1050 °C was done which was
L, overall length, min 107 (100 min) followed by air cooling to 50–60 °C. After cooling, the
A, length of reduced section, min 32 (32 min) specimen tempering was done at a pre-set heated fur-
B, length of grip section, min 30 (30 min) nace at 500 °C for 2 h followed by air cooling at room
C, width of grip section, approximate 19 (10 min) temperature. Heat treatment cycles are shown in Figs. 5,
6, and 7 respectively.
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Fig. 16 SEM images of as-

received CNTs

Fig. 17 Raman spectroscopy of

the as-received and purified CNTs

2.3 Purification of CNTs 2.4 Compositions and process parameters

Proper safety measures are taken before handling of
CNTs like wearing gloves, mask, and lab coat. The
desired quantity (i.e., 10 g) of CNTs is taken and mixed
in 37% HCl solution by stirring. Soaking at room tem-
perature was done for 12 h. Vacuum filtration was done
using deionized water to fix pH at neutral. Lastly CNTs
were oven-dried at 120 °C for 12 h. The process flow
chart for the fabrication of AA6061/CNTs surface com-
posites is shown in Fig. 8.
All the compositions and process parameters used in this study
are shown in the form of Table 2.
2.5 Filling the reinforcements into the grooves
A custom tool cutout of sheet with thickness less than that of
grooves was made for placing the reinforcements into the
grooves. Specimen filled with Reinforcement which was
clamped to the VMM is shown in Fig. 9.

Table 5 Chemical composition of AA6061 sheet

Table 4 G/D ratio of the
CNTs Type of CNTs As received Purified Element Al Si Mg Fe Mn Cu Others

G/D 0.997 1.007 Mass % 95 1.35 2.22 0.48 0.37 0.27 0.31
 Int J Adv Manuf Technol

Fig. 18 EDS spectrum of

AA6061 sheet

2.6 Machine used along with some defective test
samples
VMM was used at HMC-II Taxila for FSP purposes and
shown in Fig. 10. Furthermore, FSP also produces defects
[53–56] and some of the defective test samples are shown in
Fig. 11c and d along with good samples in Fig. 11a and b. A
schematic of the FSP process is also shown in Fig. 12.
by a cloth with 1-μm diamond paste on it. To expose friction
stir processed regions, Keller’s reagent was used. Etching was
done at room temperature in a solution containing 20 ml of
38% HCl, 20 ml of 70% HNO3, 10 ml of 40% HF, and 50 ml
distilled water. Samples were etched by soaking the etchant in
cotton and gently rubbing it on the specimen for 6–10 s. After
that, specimens were thoroughly cleaned in distilled water and
analyzed under the optical microscope.

2.7 Characterization techniques 2.7.2 Raman spectroscopy

A number of characterization techniques were utilized for
qualitative analysis of the composite produced with CNTs
reinforcement used in AA6061 aluminum alloy matrix. The
techniques comprise of metallography, Raman spectroscopy,
scanning electron microscopy, and mechanical and micro-
hardness testing. The details of the characterization techniques
that are used to analyze the composite produced in current
work are as follows.
2.7.1 Optical microscopy
For microstructural analysis, an Olympus B061 light micro-
scope was used. First, the samples were ground from rough
grinder to fine grinding up to 2400 grit size paper and polished
Raman Spectroscopy was done to check whether purification
of the CNTs was achieved or not with respect to the as-
received ones. It was done using ANDOR DV420-OE at
CIIT. Purification was carried out by the technique discussed
earlier.
2.7.3 Scanning electron microscopy and EDS analysis
The distribution of CNTs and their presence in the matrix was
shown by scanning electron microscopy (SEM). It showed the
fracture surface and the morphology of the composite. SEM
micrographs along with Energy Dispersive Spectrometer
(EDS) analysis were done on JEOL JED-2300 at NUST and
on HITACHI SU-1500 at CIIT.

Table 6 Chemical composition of groove samples 2.7.4 Mechanical behavior

Element Al Si C Mg Others
Mass % For applications that require surface of the material to
have better mechanical properties then hardness mea-
0.5 mm × 1 mm 94.27 1.30 1.98 2.16 0.29 surement of the surface becomes very important. It can
0.5 mm × 2 mm 87.81 1.2 9.1 1.58 0.31 be augmented by increasing the reinforcement volume
0.5 mm × 3 mm 77.02 1.1 20.7 0.88 0.30 fraction in the MMCs. In making of the composite in
1 mm × 3 mm 39.48 60.52 this study, CNTs were used as reinforcement and were
Int J Adv Manuf Technol

Fig. 19 EDS spectrum of CNTs

filled in 0.5 mm × 1 mm groove in
AA6061 sheet

mixed by FSP. Specimens were cut perpendicular to the
FSP zone produced and then the hardness profile was
measured on the line (each mark 2 mm apart) from the
cross-section and approximately 2 mm from the top FSP
surface as shown by Fig. 13. Vickers hardness machine
MATSUZAWA SEIKI DVK-2 was used to measure
hardness. Specimens were tested at 1 kg load, stay time
of around 10 s, and a loading rate of 70 μ/s.
For accurate tensile tests, surface of the composite produced
on the sheets was machined using milling machine to remove
flash of FSP weld and to have similar sheet thickness therefore
finally we get smooth surface. EDM wire cut machine was then
used to cut tensile specimens from the FSP AA6061 sheet mak-
ing sure the region that is friction stirred remains at the center of
the specimen. Tensile tests were done on a Shimadzu AG XPius
20KN universal testing machine at NUST.
During testing, the cross head speed of 1 mm/min was
applied at room temperature. The specimens were cut perpen-
dicular to the FSP line as shown in Figs. 14 and 15.
2.7.5 Dimensions of tensile specimen
The dimensions of the tensile specimens used in this work are
given in Table 3.
3 Results and discussion
3.1 Fabrication of CNTs-reinforced AA6061 matrix
composite
The composites were successfully fabricated by mixing
CNTs placed in groove formed in a 5-mm thick AA6061
sheet, using FSP. As compared with other MMCs, CNTs-
reinforced MMCs made through FSP are few in number
[16]. In present study, three different parameters were
varied, one related with variation of groove size with re-
inforcement (i.e., CNTs as-received and purified) and two
related with the variation in tool speed (1180 and 1500

Fig. 20 EDS spectrum of CNTs

filled in 0.5 mm × 2 mm groove in
AA6061 sheet
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Fig. 21 EDS spectrum of CNTs

filled in 0.5 mm × 3 mm groove in
AA6061 sheet

Fig. 22 EDS spectrum of CNTs

filled in 1 mm × 3 mm groove in
AA6061 sheet

rpm). Hence, the resulting composites which were fabri- microscopy is used to study and analyze their morphology
cated were characterized in this work. Scanning electron as shown in Fig. 16.

Fig. 23 Material flow in the FSP

composite using as-received
CNTs at 1180 rpm, 95 mm/min
linear speed, and 2° tool angle (×
50)
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Fig. 24 Interface of stir zone,

thermomechanically affected
zone, and heat-affected zone
using as-received CNTs at 1180
rpm, 95 mm/min linear speed, and
2° tool angle (× 100)

Fig. 25 Typical grain size of the

material in TMAZ near HAZ and
stir zone using as-received CNTs
at 1500 rpm, 95 mm/min linear
speed, and 2° tool angle (a and d)
and using purified CNTs at 1800
rpm, 95 mm/min linear speed, and
2° tool angle (b and c) at × 200
(a), × 200 (b), × 500 (c), and ×
800 (d) magnification

3.2 Raman spectroscopy
The purification done on the CNTs (as mentioned in the
“Microstructural analysis” section) was checked by the
Raman spectroscopy and the results are graphed in Fig.
17. The D-band in the as-received samples is higher,
meaning it has more defects, as compared with the D-
band in the purified samples which is lower than the G-
band. That means defects were reduced in the purified
sample as compared with the as-received one. The G/D
ratio of the as-received and purified CNTs is shown in
Table 4.

Fig. 26 Flow of material showing

dispersion of reinforcement in stir
zone using as-received CNTs at
1500 rpm, 95 mm/min linear
speed, and 2° tool angle at × 100
(a) and × 500 (b)
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Fig. 27 Hardness profile for

composites developed using as-
received CNTs at 1180 rpm, 95
mm/min linear speed, and 2° tool
angle

Fig. 28 Hardness profile for

composites developed using
purified CNTs at 1180 rpm, 95
mm/min linear speed, and 2° tool
angle

Fig. 29 Hardness profile for

composites developed using as-
received CNTs at 1500 rpm and
95 mm/min linear speed and 2°
tool angle
Int J Adv Manuf Technol

Fig. 30 Engineering stress vs

engineering strain curves for
composites developed using as-
received CNTs at 1180 rpm, 95
mm/min linear speed, and 2° tool
angle

Fig. 31 Engineering stress vs

engineering strain curves for
composites developed using as-
purified CNTs at 1180 rpm, 95
mm/min linear speed, and 2° tool
angle

3.3 Chemical composition 3.3.2 EDS of FSP composites made of CNTs and AA6061

3.3.1 As received AA6061
Chemical composition analysis of the AA6061 sheets was
done by EDS and the mass percent of the elemental obtained
is given in Table 5 along with the graphs (see Fig. 18).
EDS of all the stir zones of samples (Table 6) were done and
found to be consistent with an increase in carbon content as
shown by the resulting graphs. It also shows that CNTs were
present in the samples and were not lost or blown out of the
samples during FSP. In Fig. 19, in which 0.5 mm × 1 mm groove

Fig. 32 Engineering stress vs

engineering strain curves for
composites developed using as-
received CNTs at 1500 rpm, 95
mm/min linear speed, and 2° tool
angle

Fig. 33 Comparison of UTS,
ductility, and YS of the
composites produced using as-
received and purified CNTs
was used, the results show some signs of carbon in it but in the
sample with groove 0.5 mm × 2 mm, carbon content increases
and so on for 0.5 mm × 3 mm and 1 mm × 3 mm respectively as
shown in Figs. 20, 21, and 22. The resulting elemental compo-
sitions are shown in the respective tables below.
The EDS analysis of the samples clearly showed that as the
groove size increased so do the amount of CNTs.
3.4 Microstructural analysis
Microstructural analysis of the specimens produced by FSP
was carried out by both optical and scanning electron micros-
copy. Different magnifications were used to reveal different
features, grain structure, and reinforcement distribution.
3.4.1 Optical microscopy
First of all, optical microscopy was conducted to reveal dif-
ferent zones produced during FSP which are heat-affected
Fig. 34 Comparison of UTS,
ductility, and YS of the
composites produced using 1180
and 1500 rpm
Int J Adv Manuf Technol
zone (HAZ), stir zone (SZ), and thermomechanical-affected
zone (TMAZ). Also the flow of material, grain size in different
regions, and banded structure was studied. Specimens were
prepared by grinding, polishing, and etching. Figure 23 shows
the typical nugget formed in FSP. Figure 24 shows the zones
formed during FSP and the difference in the grain size be-
tween them. Because of high forging and extrusion forces
involved during FSP, dynamic recrystallization takes place
which reduces the grain size. Material deformation takes place
at a very high stain rate, i.e., 100–102 s−1, and temperature,
i.e., 0.8 Tm (Tm is the melting point) [57]. Figure 25 shows
some micrographs at different magnifications. Figure 26
shows the flow of the reinforcement, i.e., CNTs in to the
AA6061 matrix.
3.5 Hardness measurement
Figures 27, 28, and 29 showed that hardness increased by
increasing CNTs volume fraction. It is evident from the graphs
Int J Adv Manuf Technol

Fig. 35 Fracture surface of the

FSP material without CNTs
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Fig. 36 Fractured surface showing CNTs (arrows) in FSP matrix (stir zone) in as-received 0.5 mm × 3mm (95 × 1500) sample
Int J Adv Manuf Technol

Table 7 Comparison between process parameters

Parameter Earlier work [47] Current work Comments

Groove sizes 0.5 mm × 1.5 mm 0.5 mm × 1 mm More amount of reinforcement

0.5 mm × 2 mm
0.5 mm × 3 mm
1 mm × 3 mm
Reinforcement Different mixtures of as-received As-received CNTs Different type of reinforcement
CNTs and aluminum powder and purified CNTs
Tool pin Simple straight cylindrical pin Threaded and tapered cylindrical pin Different tool pin profile for better mixing
Tool hardness Very low hardness 8–12 HRC Hardened to 53–58 HRC For making base material sticking less to
the tool while FSP
Tool angle Perpendicular ┴ Tilted 2° vertically % To press material better and prevent material
cutting while moving forward.
Tool transverse speed 23.5 mm/min and 60 mm/min 95 mm/min Different speed
Number of passes 1 and 2 1 To make comparison easy
Tool rotational speed 950 rpm and 1500 rpm 1180 rpm and 1500 rpm Different speeds
Tool dimensions 20 mm shoulder and 10° concavity inward 25 mm shoulder and 5° concavity Different size and profile
inward and 10° tapered pin

that increasing the size of grooves augments microhardness.
Hardness of a 30.9% (AR 1180), 45.7% (purified 1180), and
47.3% (AR 1500) increase was observed compared with base
FSP material without CNTs.
3.6 Tensile testing
The composites formed by adding CNTs into AA6061 matrix
by FSP showed an increase in overall mechanical properties.
Strain offset of 0.2% was used to determine yield strength.
Ductility and ultimate tensile strengths were also measured.
In Fig. 30, it can be observed that by increasing the groove
size, yield strength and UTS increased while the ductility de-
creased. The increase of 6.8%, 14.6%, 19.8%, and 25.3%
UTS was observed compared with the base FSP material with-
out CNTs. The increase of 5.7%, 11.8%, 20.3%, and 31.1%
yield strength was observed from the base FSP material with-
out CNTs and decrease in elongation of 5%, 9.2%, 13.8%, and
23.6% was observed from the base FSP material without
CNTs. There was a gradual increase in mechanical properties
with respect to groove size. All the grooves were filled with
as-received CNTs and FSP at 1180 rotations, 95 linear speed
at 2° angle. Figures 31 and 32 showed similar trend but
composites with 1 mm × 3 mm groove size in the latter
failed early due to cavity made during processing.
Composites produced showed better properties with in-
creasing rpm of tool and purity of CNTs. All the sam-
ples tested broke within the FSP zone.
A comparison between the composites produced using as-
received and purified CNTs in Fig. 33 shows that using puri-
fied CNTs, the yield strength and UTS increased while ductil-
ity (% elongation, i.e., ΔL/Lo × 100) decreased by increasing
the groove size. Figure 34 shows the comparison of UTS,
ductility, and YS of the composites produced using 1180
and 1500 rpm.
An increase in mechanical properties of the samples is due
to the pinning effect of dislocations by the CNTs and the
reduction in ductility is attributed to less slip taking place
due to CNTs pinning dislocation movement. Purification of
CNTs reduced the contamination in the CNTs and as a result,
specimens showed better properties.
Likewise comparison of mechanical properties of the com-
posites produced at different rotations and groove sizes is
shown in Fig. 36. It clearly showed that composites produced
with higher rotation have yielded better mechanical properties
as compared with lower rpm because in composites produced
at high rpm, reinforcements get more chance of mixing and
were well mixed during processing.
3.6.1 Scanning electron microscopy
SEM images of fracture surface of the FSP material without
CNTs in Fig. 35 and whereas Fig. 36 show fractured surface
showing CNTs (arrows) in FSP matrix (stir zone) in as-
received 0.5 mm × 3mm (95 × 1500) sample The micrographs
obtained by SEM of the fractured samples were taken and it

Table 8 Comparison of results

achieved Result type Earlier work [47] Current work Comments

Maximum hardness achieved 58 HV 80.2 HV 38.3% increase

Maximum UTS achieved 154.8 MPa 199.7 MPa 29% increase
Maximum yield strength achieved 84 MPa 119 MPa 41.7% increase

clearly showed CNTs in the matrix as shown in Fig. 36. CNTs
in the matrix can be seen in the base of the fractured surface
indicated by arrows. Also the SEM of the fractured surface of
the FSP composite without CNTs is shown in Fig. 35 and the
fractured surface was magnified for a better understanding of
the fracture surface. CNTs in the samples increased the
strength of composite by resisting fracture.
4 Comparison with earlier work [47]
There were a number of parameters which were different from
the earlier work done in the department and are tabulated in
the form of Table 7 and the comparison of results achieved is
shown in Tables 7 and 8 [47].
5 Summary and conclusions
1. Metal matrix surface nano-composites were successfully
produced through FSP by adding CNTs into the AA6061
aluminum alloy matrix. Different volume fractions of
CNTs were used along with multiple groove sizes.
2. A maximum of 47.3% increase in microhardness was
observed from the base material with the addition of
CNTs. An increase in hardness is attributed to CNTs
retarding plastic deformation
3. A maximum of 53.2% yield strength was recorded from
the base material with the addition of CNTs. It was be-
cause of CNTs acted as strengthening agents by stopping
atomic movements.
4. An increase of 32.4% ultimate tensile strength was ob-
served from the base material which was due to CNTs
pinning dislocation movement hence increasing strength.
5. A 53.04% decrease in ductility was observed by the ad-
dition of CNTs. As plastic deformation of the material was
reduced consequently its ductility as well.
6. Increasing groove size up to a certain extent (i.e., 0.5 mm
× 3 mm) was beneficial but around 1 mm × 3 mm groove
size was detrimental on the mechanical properties because
larger groove promoted cavity formation.
7. Increasing the purity of the reinforcement (in this case
CNTs) increased the mechanical properties because of
fewer defects in purified CNTs.
8. Increasing the rpm of the tool for FSP also improved the
mechanical properties because CNTs in the material were
better mixed at higher rpm. The higher the rpm, the more
agitation in the material, resulting in better mixing of
reinforcements.
9. Increasing the hardness of the tool proved to be beneficial
as well because harder tool prevented sticking of the ma-
terial with it and produced better surface finish.
Int J Adv Manuf Technol
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