Journal of Alloys and Compounds 738 (2018) 182e187

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Journal of Alloys and Compounds

journal homepage: http://www.elsevier.com/locate/jalcom

Production of CNT-bearing melt-spun Al-2Sc-0.05CNT alloys

M. Fatih Kilicaslan a, *, Ercan Karako
€ se b
a
Kastamonu University, Department of Materials Science and Nanotechnology Engineering, Kastamonu, Turkey
b
Karatekin University, Faculty of Sciences, Department of Physics, 18100 Çankırı, Turkey

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

Article history: In the present work, rapidly solidified Ale2Sc-XCNT (X ¼ 0, 0.05) alloys were successfully fabricated by
Received 2 November 2017 melt spinning under Ar atmosphere. The effects of addition of CNT on the microstructural, thermal,
Received in revised form microhardness, and electrical properties were investigated by using scanning electron microscopy (SEM),
11 December 2017
X-ray diffractometer (XRD), differential calorimeter (DSC), Vickers microhardness testing and a four point
Accepted 13 December 2017
Available online 14 December 2017
probe resistivity tester. Experimental results illustrated that the addition of 0.05 wt% CNT to melt-spun Al
e2Sc alloys led to the formation of equiaxed globular-like morphologies with size from 0.3 to 2.7 mm in.
In the microstructure of Al-2Sc-0.05CNT alloy, CNTs covered by Al with size (width and length) changing
Keywords:
AleSc alloys
from 40 to 55 nm and 255e295 nm, respectively, were observed. The addition of CNT led to a net
Microstructure increment (~25%) in microhardness values due to solitary strengthening of the carbon nanotubes, solute
Melt spinning solution hardening and modification of the morphologies of Al3Sc intermetallics. In addition, because of
Microhardness CNT addition there was a decrease in the electrical resistivity.
Carbon nanotube © 2017 Elsevier B.V. All rights reserved.

1. Introduction corrosion resistance and high strength-to-weight ratio to ensure

Rapid solidification offers some distinct advantages over con-
ventional ingot metallurgy to meet the increasing demand for high
performance materials [1e4]. A refined microstructure, increased
structural and chemical homogeneity, and extension of solid solu-
bility are some of the unique features achieved through rapid so-
lidification [5,6]. On the other hand, in the competition for the
improvement of new alloys and composites that compensate the
requirements of increased specific hardness and durability at lower
intensity, aluminum and aluminum based composites are the most
commonly used materials owing to their indispensable physical
and mechanical features. Due to its high thermal and electrical
conductivities, excellent corrosion resistance, ease of fabrication
and high strength-to-weight ratio, aluminum and its alloys and
composites are used in a wide range of industrial applications such
as the automotive, aerospace industry, building and construction
and electrical transport networks. Because of unique properties of
aluminum alloys, they have vital importance for aircraft industry. In
particular, an aircraft engine is made up of three main parts, namely
a compressor and combustor turbine placed in an aluminum cas-
ing. These materials provide high temperature properties,
* Corresponding author.
E-mail address: fkilicarslan@kastamonu.edu.tr (M.F. Kilicaslan).
efficient fuel consumption for economic operating of flights and
longer operation life. However, the use of aluminum has been
restricted by its low degree of strength and poor corrosion resis-
tance. Among aluminum alloys Al-Sc ones have generally been used
in aircraft and missile constructions, due to scandium addition
enhanced strength and corrosion resistance [7,8]. For example,
additions of 1e3wt%Sc to Al have been reported to reduce the as-
cast grain size and increase the operating temperatures of AleSc
alloys up to 210  C without a loss in the tensile strength [9]. Also,
precipitated Al3Sc intermetallics which have smaller lattice
parameter than in other intermetallics phases, increased the fre-
quency of heterogeneous nucleation for both intermetallics and
aluminum phases, resulting in a refined and modified microstruc-
ture [10]. Venkateswarlu et al. [11] found that a small amount of Sc
in Al reduced the final particle sizes by %50 in comparison to the
same amount of Sc in Al-5Ti-1B. Additions of Zr together with Sc in
Al alloys may also decrease the particle sizes of Al-Mg-Si-Mn
samples [12,13], and also among Sc, Zr and Si, Sc has the stron-
gest effect on mechanical properties [13]. It is well known that
carbon nanotubes (CNTs) have excellent mechanical properties,
electrical conductivity and thermal stability. As to the mechanical
properties, their tensile strength and elastic modulus can be as high
as 150 GPa and1 TPa, respectively. Also CNTs with remarkable
physical and mechanical features offer encouraging potential as a
reinforcing material to improve the physical, thermal, and

https://doi.org/10.1016/j.jallcom.2017.12.130
0925-8388/© 2017 Elsevier B.V. All rights reserved.

M.F. Kilicaslan, E. Karako
Table 1
Chemical compositions of the melt spun Al-Sc alloys.
Sample Sc (wt%) CNT (wt%)
AS 2 0
ASC 2 0.05
mechanical features of composites material [14]. Hence, in the
literature they are seen as potential reinforcements for composite
materials.
In terms of Al e based metal matrix composites, aluminum
based carbon nano tube composites (A-CNTs) are very promising
material, for many industrial applications because of the excellent
nanoscale reinforcement character of CNTs. The addition of CNT to
aluminum and its alloys can considerably increase their physical,
mechanical, thermal and electrical properties [15,16]. Until now,
dozens of Sc containing Al alloys have been investigated. However,
according to the best of our knowledge there are so less or no
comprehensive information about melt-spun Al-Sc alloys in the
open literature. Moreover, in the open literature we were unable to
find any information about CNT doped melt-spun Al-2Sc alloys.
Therefore, in this study we have successfully produced CNT doped
melt-spun Al-2Sc ribbons and investigated effect of CNT addition
on the morphological, microhardness and electrical properties. For
this purpose, the resulting microstructures, thermal behaviors
mechanical and electrical features were investigated and analyzed
by the XRD, SEM, Vickers microhardness and four point probe re-
sistivity test methods.
2. Experimental
The Al-2Sc and Al-2Sc-0,05CNT master alloys used for this
investigation were induction melted from starting materials of
elemental Al (99.9% purity, the size of varied from 7 to 15 mm), CNT
(99.5% purity), and Sc (99.99% purity, the size of varied from 2 to
Fig. 1. SEM micrographs showing the microstructural evolution of melt-spun Al-Sc alloys with the addition of CNT. While (a) shows the SEM micrograph of the CNT free alloy Al-2Sc
(AS), (b) depicts the SEM micrographs of the alloy containing 0.05 wt% CNT (ASC), respectively.
€se / Journal of Alloys and Compounds 738 (2018) 182e187
183
10 mm). The Sigma-Aldrich's carbon nanotubes (CNTs) used for the
present study were multi walled carbon nanotubes and synthe-
Al (wt%) sized by chemical vapor deposition. The diameter  wall
bal.
thickness  length of the CNT varied from 20 to
bal. 30 nm  1e2 nm  0.5e2 mm, respectively and the density of CNTs
was 2.1 g/mL at 25  C. The purity of the CNT powder was 95% and it
contained 5% amorphous carbon. Melt-spun counterparts of the
master alloys were produced using an EZE Nanoteknoloji EE01
melt-spinner, in which the molten alloy in a quartz crucible was
ejected onto a polished copper wheel with 20 m/s disc velocity by
pressurized argon at a rate of 200 mbars. All experimental pro-
cesses were performed in Ar atmosphere. For the present work, all
percentages are weight percents unless otherwise stated. The CNT
free samples and those with 0.05 wt%CNT are denoted as AS and
ASC respectively. All of the samples fabricated are illustrated in
Table 1. The microstructure analyses and phase descriptions were
performed by using FEI Quanta FEG 250 scanning electron micro-
scopy (SE mode was used) with energy dispersive spectrometry, a
Bruker D8 and Advance X-ray diffractometer with high-energy
monochromatic CuKa radiation (0.15418 nm) in the 2q range of
20e80 at a scan rate of 0.05 /s. In order to determine the phase
formation during heating from 50 (room temperature) to 700  C, a
DSC instrument (Setaram TG-DTA/DSC) with a heating rate of 10  C/
min was used. The hardness tests of the alloys were made a
Durascan 70 model digital Vickers microhardness tester at 25  C.
This device performed of 0.098, 0.245, 0.49, 0.98, 1.47 and 1.96 N
applied loads and a loading period of 10 s. The electrical resistivity
measurement was performed with a four-probe dc electrical re-
sistivity instrument. Electrical resistivity was calculated by equa-
tion (1):
VG
r¼ (1)
I
where G is the geometric correction constant and V is the voltage
184 €se / Journal of Alloys and Compounds 738 (2018) 182e187
M.F. Kilicaslan, E. Karako
drop. Total electrical resistivity was calculated by equation (2):
r ¼ r0 1=expð  Ea =kTÞ (2)
where r is the electrical resistivity, Ea is the activation energy, r0 is
electrical resistivity at absolute temperature (T), and k is the
Boltzmann factor [17].
3. Results and discussion
The SEM micrographs seen in Fig. 1 show the microstructural
evolution of melt-spun Al-Sc alloys with the addition of CNT. While
Fig. 1 (a) shows the SEM micrograph of the CNT free alloy Al-2Sc
(AS), Fig. 1 (b) depicts the SEM micrographs of the alloy contain-
ing 0.05 wt% CNT (ASC), respectively. In addition, the XRD patterns
from these specimens are seen Fig. 2 According to the SEM mi-
crographs and XRD patterns, the microstructure of the melt-spun
Al-2Sc alloy consisted of an a-Al matrix and Al3Sc intermetallic
compounds (Figs. 1 (a) and 2 (a)). However, the microstructure of
the CNT-containing sample (ASC) includes an additional phase of
Al4C3 in addition to the a-Al matrix (this phase homogeneously
spread out throughout the microstructure) and the Al3Sc inter-
metallic compounds (Fig. 1 (b) and 2 (b)).
It is clearly seen from Fig. 1 that the addition of CNT drastically
changed the morphology of the ASC sample. It can be observed
from Fig. 2 (a) that the microstructure of the CNT-free alloy (AS)
consisted of cubic and rectangular prism - like phases with, size
Fig. 2. X-ray diffraction (XRD) patterns from the specimens AS (a) and ASC (b).
from 1 to 3 mm. It can also be observed that some of the cubic and
rectangular phases were removed during deep etching due to cubic
and rectangular gaps remaining. From the XRD analyses (Fig. 2 (a))
and literature [18] we concluded that these cubic and rectangular
prism-like phases were Al3Sc intermetallics. According to the Al-Sc
phase diagram for an aluminum alloy with1 and 2 wt%Sc, the for-
mation of the Al3Sc intermetallic phase can be anticipated [18]. In
Fig. 1 (b), at this low magnification the presence of CNTS cannot be
observed due to their low concentrations. However, it is clearly
seen that, with addition of 0.05 wt% CNT, the morphologies of the
Al3Sc intermetallics changed from cubic and rectangular prism-like
to equiaxed globular-like types with size, from 0.3 to 2.7 mm. These
kinds, of small equiaxed phases are desirable for a structure,
generally lead to improved toughness and ductility [19]. The for-
mation of globularelike intermetallics can be explained based on
the literature as following, due to growth of a seed crystal diffusions
controlled, and the radial growth rates of an isolated crystal floating
in the melt are basically isotropic. Also, solute gradients in the small
volume of melt surrounded by a tiny seed are radial symmetrical,
which is also in favor of a rounded outline. It has been reported that
a higher undercooling level can help these tiny seed crystal, to grow
isotropically, resulting in a rounded/globular shape [20]. On the
other hand, it has been reported that in Al alloys, an increased
concentration of modifier agent in liquid phase brings about an
increased constitutional undercooling [21]. The purity of our CNTs
was 95 wt%, meaning CNT powders contain 5 wt% amorphous C.
Hence, in our case we think that some carbon atoms (most likely
amorphous C) from the CNTs played a role as a modifier agent in the
liquid Al matrix and led to an increment in the constitutional
undercooling, which resulted in the formation of rounded/
globular-like intermetallic phases. Using a high magnification the
SEM micrograph of the nano size fiber like phases (they are located
within the ellipses) from the CNT-containing sample ASC and the
energy dispersive spectrometer measurement (EDS) from these
phases are given in Fig. 3 (a) and (b), respectively. The sizes (Width
X Length) of the fibers, seen in spots 1 and 2, were 55 nm  295 nm
and 40 nm  255 nm, respectively (Fig. 3 (a)). According to the EDS
result (Fig. 3 (b)), this fiber is compose predominantly of C, which
means that CNTs can be detected in the microstructure of melt-
spun Al-Sc alloy. Mansour and Shahid reported [22] in their ex-
periments, that because of good wettability the carbon nanotube
surface was fully covered by pure Al, resulting in a thick Al coating
on the surface as a result of which the diameter of the carbon
nanotubes reached to 100 nm. In our case, diameter of the CNTs
increased from 10 e 15 nm to 40e55 nm (Fig. 3 (a)). In addition, in
EDS analyses we could detect the Al together with C. Hence, we
think that reason for the increment in the diameter of CNTs was
because of Al coating on the surfaces of CNTs.
The calculated lattice parameters and FWHMs (full width at half
maximum) obtained from the Al (111) peaks of the AS and ASC
alloys are given in Table 2, while Fig. 4 shows the peaks with the
highest intensity of Al (111). It is clearly seen from Table 2 and Fig. 4
that compared to the CNT-free alloys (AS), the Al (111) peaks shift to
the right in the ASC sample with the addition of CNT, and the lattice
parameters also get smaller with the addition of CNT. Actually, the
atomic radius of carbon (0.84 Aº) is smaller compared to Al (1.21
Aº); however the atomic radius of Sc (1.74 Aº) is bigger than that of
Al [23]. On the other hand, it is known from the literature that an
increased cooling rate leads to greater undercooling during rapid
solidification. Also, an increment in the undercooling level results
in an increase in the solute solubility limits [24,25]. Therefore, we
think that due to the increased undercooling caused by the very
rapid cooling during melt spinning extended the solute solubility
limits and brought about the dissolution of some of the carbon
atoms from in the CNT powder (probably amorphous carbon) in the
 €se / Journal of Alloys and Compounds 738 (2018) 182e187
M.F. Kilicaslan, E. Karako 185

Fig. 3. SEM micrograph with high magnification of the nano size fiber like phases (they are located within the ellipses) from the CNT-containing sample ASC (a) and the energy
dispersive spectrometer measurement (EDS) from these phases are given (b), respectively.

Table 2 AS < ASC. In the literature, broadening of the Al (111) peak is

Changes of microhardness, lattice parameter and FWHM of melt spun Al-2Sc alloy attributed to the reduction in the crystal size of Al the phase. In ref.
with addition of CNT.
[22], it was also reported that because of addition of CNT, there was
Sample Microhardness (HV) Lattice parameter (a) FWHM a systematic decrease in the crystallite size of pure aluminum.
AS 92 ± 3.2 0.41341 0.290 Hence, our results are good in agreement with the literature.
ASC 115 ± 5.4 0.41214 0.375 From Table 2, it can also be seen that the microhardness values
of melt-spun Al-Sc alloys considerably increased with the addition
of CNT. It is clear from Table 2 that the additions of 0.05% CNT in-
Al matrix, resulting in a decrease in the lattice parameter. The creases microhardness from 92 HV to 114 HV. That is, a net increase
FWHMs of Al (111) were found in the following order (Table 2): (~25%) in the hardness was achieved due to CNT addition. In the
186 €se / Journal of Alloys and Compounds 738 (2018) 182e187
M.F. Kilicaslan, E. Karako

Fig. 5. Differential scanning calorimeter (DSC) analyses from the samples AS and ASC.
Fig. 4. FWHMs (full width at half maximum) obtained from the Al (111) peaks of the
AS and ASC alloys.

literature, one of the reason, for the increment in the hardness of

CNT-added aluminum alloys is the solitary strengthening of carbon
nanotubes [21]. In addition, it is well known that in aluminum al-
loys, modification and refining of the morphologies of secondary
phases such as in intermetallic compounds, can considerably
improve their mechanical properties. For example, it has been re-
ported that modification and refining of the morphologies of Fe-
bearing intermetallics upgraded or enhanced the mechanical
properties of melt-spun hypereutectic Al-Si-Fe-Co alloys [21,26]. In
our case, it can be clearly seen from Fig. 1 that the faceted mor-
phologies of Al3Sc intermetallics changed to a rounded/globular-
like morphology with the addition of CNT. Hence, we think that
one possible reason for the increment in the microhardness values
is the modification of the morphologies of Al3Sc intermetallics. On
the other hand, it can be concluded from the lattice parameters of
the aluminum matrix (Table 2) calculated from XRD analyses
(Fig. 4) that some of the carbon atoms dissolved in the Al matrix.
Fig. 6. Electrical resistivity properties of AS and ASC samples in an applied test tem-
Therefore, we conclude that solitary strengthening of the carbon perature range of 300e900 K.
nanotubes, solute solution hardening and modification of mor-
phologies of Al3Sc intermetallics led to an increase in microhard-
ness values together. feature of metals and alloys. The resistivity values of the CNT, added
The thermal characteristics of AS and ASC alloys are very critical ASC sample is smaller than that of the CNT, free AS melt-spun
properties for they define the high application temperature for sample. The reason for this reduction in the electrical resistivity
usage areas. The melting process of AS and ASC melt-spun was due to CNT, being added maybe connected to morphological
examined and analyzed by DSC analysis as seen in Fig. 5. The AS changes in the rapidly solidified alloys including Al3Sc and Al4C3
sample illustrates that one endothermic line is detected at intermetallic precipitation, the fact that C atoms reduce disloca-
628.37  C. On the other hand, the CNT added ASC sample shows tions and structural improvement. More specifically, the homoge-
that two endothermic peaks line are detected at 630.84  C and nization in grain reduces grain boundary scattering and improve
648.32  C; they correspond to the melting reaction of the crystal- the electrons mobility, therefore decreasing the electrical resistivity
line mixture of the Al with Al3Sc and Al4C3 intermetallic phases, [27,28]. This phenomenon is supported by the SEM analysis below
respectively. It is clearly seen that the addition of CNT increased the please see.
melting point temperature of the AS sample from 628.37  C to
630.84  C. We believe that the increase in melting temperature is
related to the 5% amorphous C atoms penetration in then Al matrix. 4. Conclusions
This fact is illustrated by the XRD analysis and where crystalline
Al4C3 intermetallics can be identified in the example of melt-spun In this study, we investigated the effects of CNT addition on the
ASC. microhardness, microstructural, electrical properties of as-cast Al-
Four point probe resistivity tests are convenient way to estimate 2Sc alloys. The results can be summarized as follows:
the electrical features of these kinds of metals. The electrical re-
sistivity properties of AS and ASC samples in an applied test tem- - Addition of CNT to Al-2Sc alloy led to the formation of an
perature range of 300e900 K are shown in Fig. 6. As is clearly additional intermetallic phase, which is metastable Al4C3
shown in Fig. 6, the electrical resistivity increases linearly with - With the addition of 0.05 wt% CNT, the morphologies of the
temperature in the range of 300e900 K. This behavior is a common Al3Sc intermetallics changed from cubic and rectangular prism-
 €se / Journal of Alloys and Compounds 738 (2018) 182e187
M.F. Kilicaslan, E. Karako
like to equiaxed globular-like morphologies with size from 0.3
to 2.7 mm.
- CNT, added melt-spun Al-Sc alloys were successfully
synthesized.
- The width and length of the observed CNTs changed from 40 to
55 nm and 255e295 nm, respectively.
- An increase in the diameter/width of CNTs was observed
because of Al coating on the surfaces of the CNTs.
- Addition of CNT to Al-2Sc alloy brought about a reduction in the
crystal size of the Al phase because of the dissolution of some
carbon atoms in the CNT powder in the Al matrix.
- Addition of CNT led to a net increment (~25%) in microhardness
values due to solitary strengthening of the carbon nanotubes,
solute solution hardening and modification of the morphologies
of Al3Sc intermetallics.
- Addition of CNT to Al-2Sc alloy led to a decrease in the electrical
resistivity.
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