Journal of Alloys and Compounds 787 (2019) 543e550

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Journal of Alloys and Compounds

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

Production and mechanical characterization of Ni-coated carbon fibers

reinforced Al-6063 alloy matrix composites
€
Anıl Alten, Eray Erzi, Ozen € kçe Hapçı Ag
Gürsoy, Go aog € khan Orhan*
lu, Derya Dispinar, Go
Istanbul University-Cerrahpasa, Faculty of Engineering, Metallurgical and Materials Engineering Department, 34320 Istanbul, Turkey

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

Article history: In this study, it aimed to produce carbon fiber (CF) reinforced aluminum metal matrix composite by
Received 12 November 2018 squeeze casting method. In order to overcome the wetting problem between the aluminum matrix and
Received in revised form the reinforcing agent, carbon fibers were coated with Ni coating with electroless technique. Different
31 January 2019
bath pH values and hypophosphite (HP), coating durations and bath temperature were investigated. SEM,
Accepted 4 February 2019
EDS and XRD methods used to determine the characterize the layers. It has been observed that increasing
Available online 5 February 2019
the pH of the bath, coating time, bath temperature and amount of hypophosphite increases the thickness
of the Ni coatings on the carbon fibers. Two different thicknesses of coatings were used with different
Keywords:
Aluminium matrix composite
volume fractions of fiber used to reinforce the 6063 aluminum as matrix alloy. Squeeze casting process
Squeeze infiltration was used for the production of the composites to increase the connection between the matrix and the
Carbon fiber carbon fibers. After achieving a good bonding, three-point bending, Charpy impact, and Vickers hardness
Reinforcement tests were carried out to investigate the difference of at the mechanical properties. It was observed from
Mechanical properties the mechanical tests that while the hardness and the three-point bending strength was increasing the
impact strength was decreasing after the carbon fiber addition. Also coating, in general, helping the
mechanical properties, mechanical properties of composites are badly affected by higher coating
thicknesses.
© 2019 Elsevier B.V. All rights reserved.

1. Introduction 700e800 grades of melting temperature of alumina in general

Aluminum alloys are one of the main materials used in the metal
matrix composites. Their low density and low melting point are
some of the key factors for their wide usage. In addition, the fact
that base aluminum has low mechanical properties requires that
aluminum is strengthened in some way. The use of carbon fiber in
MMCs, one of the strengthening methods of aluminum, has gained
momentum and began to be used within a few decades [1]. The key
features expected in the production of aluminum matrix carbon
fiber reinforced composites are high strength and elastic modulus,
low density, easy formability and ease of production [2,3]. However,
in addition to these advantages, there are difficulties encountered
during the production of the composite. The matrix phase and the
reinforced phase should act as one single material providing
complete bonding within operating conditions. The problem of
wetting, one of the problems encountered in aluminum-carbon
fiber reinforced MMCs, is particularly limited in the range of
* Corresponding author.
E-mail address: gorhan@istanbul.edu.tr (G. Orhan).
[1,4e6]. In addition, increasing the exposure time causes a much
more heterogeneous composite structure to improve the situation.
As the wetting improves with increasing temperatures, this time
the reaction between the aluminum matrix phase and the carbon
fibers results in undesirable brittle Al4C3 structure [7].
Some different approaches have been applied in order to pre-
vent the formation of this structure and to ensure sufficient
bonding even at the casting temperatures of aluminum. Increasing
the contact surface with pressure [1] alloying aluminum alloy with
Cu and Ni coating of carbon fibers [8e11], and/or squeeze casting
are some of the methods [12e14]. Lacoste [15] has reviewed a
thorough investigation of possible problems that occur for the
wettability of reinforcements. For enhanced wettability, one of the
most important parameter is the rapid cooling of the liquid metal.
Additionally, the heating of the reinforcement has been a typical
application. When the interaction between the matrix and the
reinforcement is low, this results in microporosity formation
[16e18]. It is important to note that the flow of liquid through the
fibers also generates the issue of decreased permeability of the
liquid [19e21]. Thus, application of pressure has been the ultimate
solution to much problems.

https://doi.org/10.1016/j.jallcom.2019.02.043
0925-8388/© 2019 Elsevier B.V. All rights reserved.
544 A. Alten et al. / Journal of Alloys and Compounds 787 (2019) 543e550

A. Daoud [22] used 2014 Aluminum alloy as metal matrix and
tried to use carbon fibers to strengthen the alloy by using gas
pressure infiltration technique. First attempts were unsuccessful
because of the lack of wettability between of carbon fibers and
aluminum alloy. A. Daoud coated the carbon fibers with Ni and
overcome this problem. Successful parameters for the experimental
was 730
C for infiltration temperature and 50 kPa pressure and
2 min infiltration duration. The technique was successfully applied
and carbon fibers were evenly distributed. Tensile modulus and
ultimate tensile strength were increased but the elongation of the
composites was reduced compared to the base 2014 aluminum
matrix itself. H. Naji et al. [1] have studied the volume percent and
aspect ratio of carbon fibers on fracture toughness for the
aluminum matrix. Composite was prepared by using stir casting.
LM2 aluminum alloy was selected as the matrix material and 5 wt%
Mg was added to increase the fluidity of the liquid metal and also
protect the system from aluminum carbide. Carbon fibers were
prepared in three different aspect ratios and after preparation fi-
bers were added into melted Al alloy gradually. The melt then
mixed with a propeller for homogenous distribution of the fibers.
Finally, three different volume fraction (1%, 2% and 3%) and three
different aspect ratios of samples were produced by casting
method. As a result, it was found that the fracture toughness of
matrix material was increased with carbon fiber addition and both
volume fraction and aspect ratio of the used carbon fibers were
important. It was found that the crack deflection was the dominant
mechanism for fracture at aluminum-carbon fiber matrix com-
posite. M. Tavakol. et al. [23] used shockwave sintering technique to
produce Al/SiC metal matrix composites with nano-sized particles
using Molecular Dynamics simulation. After simulations, it was
found that micro-sized ceramic particles increased the yield and
tensile strength but lowered the ductility but on the other hand,
nano-sized addition has also better ductility than the metal itself.
Also, an appropriate cooling rate also helps the mechanical prop-
erties. J. Zhang et al. [24] have also used Al-Mg alloy as a matrix
material and coated the fibers with Ni/P layer. %99.7 Al was used to
produce 5% Mg aluminum alloy and the fibers were heated up to
773 K (500
C) for 45 min to eliminate resin glue. Six different
stabilizers used at the deposition stage and lactic acid have the best
stabilizing effect. Fibers were coated with Ni/P layer and pre-heated
agent. Table 1 lists the bath composition and the conditions for the
deposition process. The effect of pH value, time and temperature on
deposition was also investigated.
A two-step pretreatment process known as sensitization and
activation was applied to the sized fibers prior to the electroless
process. Surface sensitization was conducted by immersing the
samples into an aqueous solution which contained 20 g/l SnCl2 and
40 ml/l HCl. The specimens were subsequently rinsed with deion-
ized water as take a dip and activated through immersion into a
solution which contained 0.25 g/l PdCl2 and 2.5 ml/l HCl. The
sensitization and activation steps were applied to the ultrasonic
bath for 10 min at room temperature. Finally, the specimens were
immersed in the electroless plating bath with magnetic stirring.
After deposition products were washed with distilled water and
then dried in an oven at 120
C for 2 h.
Carbon fiber reinforced aluminum composites were produced
using different volume ratios of fiber with two coating thicknesses
of 0.9 and 4.2 mm by squeeze casting method. Table 2 shows the
chemical composition of 6063 Al alloy which was used as matrix
materials. In Table 3, experimental codes belonging to the com-
posites produced are given.
The Ni-coated fibers were preheated at 500
C and then were
moved into the squeeze casting die, which was preheated up to
250
C. Right after that, the 6063 molten aluminum was poured
into the die at 750
C and the 30 MPa pressure was applied for 30 s
to reinforce the carbon fibers. After that, the pressure was removed
and the samples were extracted from the die.
The structure of as-deposited Ni-P alloy was analyzed by X-ray
diffractometer (XRD, Rigaku Miniflex, Japan) with CuKa radiation
(l ¼ 1.54050) and monochromator at 50 kV and 300 mA with the
scanning rate of 2
/min. Scanning electron microscope (SEMeJeol
JSM 5600) with energy dispersive X-ray analysis (iXRF 500)
attachment was used to determine the surface morphology and
elemental composition of the deposits.
Table 1
Chemical composition and working conditions of the electroless nickelplating
bath.
Bath composition A1 A2

up to 673 K (400
C) and then fixed on to 993 K (720
C) pre-heated NiSO4$6H2O (g/l) 30 30
graphite mold. Aluminum melt at 993 K (720
C) poured into the NaPO2H$H2O (g/l) 10 30
C6H5Na3O7$5H2O 30 30
mold and to control the solidification time different thicknesses of
NH4Cl (g/l) 50 50
asbestos were used. Solidification durations were changing CH4N2S (mg/l) 2 2
100e700 s 10 mm thickness samples were cut and then pressed Deposition conditions
with hot pressing at 773 K (500
C). It was found that increasing the pH 7, 8, 9, and 10
solidification time increase the bonding degree between the metal Temperature (
C) 70, 80, and 90
Stirring speed (rpm) 175
matrix and the carbon fibers but also overly long durations increase Electrodeposition time (min.) 15, 30, 60, and 120
the tendency of the crack happening from the centers of the woven
fibers. Hot pressing was also helpful to mitigate the crack and
cavities that happened during the casting process.
Table 2
The aim of the present study was the effects of plating param- The chemical composition of 6063 Al alloy (%wt.).
eters such us pH of the plating bath, plating bath's temperature,
Fe Si Cu Mn Mg Zn Cr Zr
stabilizer concentration, temperature and time on the coating
thickness and phosphor content of deposit investigated. In addi- 0.35 0.4 0.1 0.1 0.55 0.1 0.1 0.15
tion, in this study, aluminum matrix composites were produced by
squeeze casting using nickel coated carbon fiber with different
coating thicknesses and different volume ratios, and the mechan- Table 3
The samples prepared in the experiments and the codes.
ical properties of these composites were tested.
Sample code Thickness and volume ratio
2. Experimental procedure S1 0.9 mm ± 0.05 and 2 vol %
S2 0.9 mm ± 0.05 and 4 vol %
The NieP coating was deposited on the carbon fibers surface S3 4.2 mm ± 0.1 and 4 vol %
using an alkaline bath containing nickel sulphate as a source of S4 4.2 mm ± 0.1 and 2 vol %
S5 base alloy (Al 6063)
nickel, and different amount sodium hypophosphite as a reducing
 A. Alten et al. / Journal of Alloys and Compounds 787 (2019) 543e550 545

The mechanical properties of the samples were analyzed by a

three-point bending test (Instron) with a span length of 60 mm and
a crosshead speed of 3.0 mm min1. The Charpy impact tests of
composite materials were carried out on a 10 kg pendulum
weighted impact device, without applying notch effect to the
samples. The results obtained are calculated as energy absorption
per unit area. The Vickers HV 10 hardness test was applied to the
composite specimens in the Zwick brand hardness tester, which
applies a constant load of 10 kg. The averages of the hardness values
taken from 8 different points of each sample were taken and the
comparisons were made on average values.

3. Results and discussion

3.1. Effect of pH

The microstructure of the NieP coated carbon fiber performed

at 80
C for 60 min in A1 plating bath at different pH in the longi-
tudinal direction is shown in Fig. 1.
From the Fig. 1, it can be seen that the coating are uniform and Fig. 2. Variation of phosphorous content and coating thickness as a function of pH.
continuous in the range of mm in the fiber bundle also with (80
C, 60 min, A1 bath).

increasing pH of the bath solution, the coating thickness increases,

which is in good agreement with the results literature [25,26]. The
fiber, where pH varies from 7 to 10 are shown in Fig. 3. The
properties of the coating depend on its structure and chemical
diffraction around 44.5
(2Ɵ) reveals Ni (111) (JCPDS card No.
composition. It is well known that the nickel-plating using sodium
40e0850). The relative intensity of Ni 111 with rising pH value due
hypophosphite as a reducing agent is a binary alloy of nickel and
to the increased deposition rate for higher pH value. Also, the Ni 111
phosphorus. Among all working condition, pH is one of the most
peak became sharper as the pH value increased. It is evident from
dominant factors, which controls phosphorous content in the de-
the Fig. 3 that at low pH (pH:7) coating is amorphous structure,
posits. All other parameters are fixed, the phosphorous contents of
whereas at high pH (pH:10) it shows semicrystalline structure. It
the coatings and its thickness when plating condition with respect
is consistent with XRD results with P content in alloy varying ac-
to pH is varied from 7 to 10 are detected by SEM and EDX analysis
cording to pH value. As the rate of P decreases at increasing pH
and also shown in Fig. 2. It is found that the pH value of the coating
values, the structure has changed from amorphous to semi-
bath has a noticeable effect as expected. The results indicated that
crystalline.
the phosphorus content decreases as the pH value increased. When
the pH increases in plating bath inhibit deposition of P in the
coatings [26]. As a result, when it is desired that the coating 3.2. Effect of temperature
thickness and composition remain constant, it is extremely
important to keep the pH of the bath constant during the coating In order to study the effect of bath temperature on NieP coating
process. experiments were carried out at 70
C and 90
C at pH value of 8 for
The XRD patterns of the electroless nickel deposits on carbon 1 h in the A1 plating bath. The results also showed that the

Fig. 1. SEM micrographs of the as received and nickel-coated carbon fiber as a function of pH of the coating bath (a) as uncoated, (b) pH 7, (c) pH 8, (d) pH 9 and (e) pH 10. (80
C,
60 min, A1 bath).
546 A. Alten et al. / Journal of Alloys and Compounds 787 (2019) 543e550
Fig. 3. XRD of NiP coated carbon fiber as a function of pH.
Fig. 4. Variation of phosphorous content and deposition rate of the NieP coated car-
bon fiber as a function of temperature. (pH 8, 60 min, A1 bath).
phosphorous content dramatically decreased with increasing
deposition temperature. On the other side, the coating thicknesses
increased with rising temperature as expected (Fig. 4). The higher is
the temperature of the electroless nickel bath, the faster is the
Fig. 5. SEM micrographs of the nickel-coated carbon fiber as a function of bath temperature (a) 70
C, (b) 90
C (pH 8, 60 min, A1 bath).
deposition rate. SEM images of the coatings at pH value of 8 in A1
bath carried out at 70
C and 90
C are given in Fig. 5.
3.3. Effect of deposition time and HP with different pH value on the
coating
The effect of deposition time on coating thickness for different
HP containing bath and pH value were investigated. Time-
dependent coating thicknesses are given in Fig. 6. Although the
deposition rate varies with the amount of HP in the bath, this
tendency to change is the same for both pH values and different HP
values (Fig. 6a and b). It can be seen in Fig. 6 that the coating
deposition curve with deposition time does not follow a completely
linear relationship for both different pH value and for different HP
containing bath. The deposition rate between 15 min and 60 min
increased linearly with the coating duration, while the rate
decreased after 60 min for all experimental condition. This may be
due to the deterioration of the Ni/P ratio in the bath composition
due to the increased coating time. Fig. 7 shows the SEM images of
the coatings obtained in the conditions of pH 8 g/l and 30 g/l HP for
different coating time. The effect of the HP concentration in the
bath on the deposition rate can be evaluated by the coatings given
in Figs. 1c and 7c. In the coating process, where the pH value was 8
and the time was constant for 1 h, the coating thickness increased
from approximately 4 to 11 mm by increasing the HP concentration
from 10 g/l to 30 g/l. The percentage of P also increased from 2.5 to
4.5 with rising HP concentration.
3.4. Composite production by squeeze casting
Sample codes for the produced composites are given in Table 3.
Fig. 8a shows the SEM images of 0.9 mm Ni-coated CF used in the
production of S1 and S2 coded composites. In Fig. 1c, 4.2 mm Ni
coated CF (S3 and S4) composites were given. Fig. 8b and c show
different views of the Ni-coated fibers (S1) in the Al metal matrix. It
can be seen that there is a full infiltration to aluminum alloy.
Fig. 9 shows the wettability of fibers with the cast aluminum
matrix. It can be seen that when uncoated fibers are used (Fig. 9a),
there is complete no wetting of the fibers. The fibers are agglom-
erated and a porous region observed around the fibers. This is also
supported by the sessile drop test which is given as inset in Fig. 9a.
It can be seen that wetting angle is around 114
. According to Ip
et al. [27], the contact angle between the aluminum and graphite is
140
. Ip also measured the wettability of Ni coated graphite and
found that the angle was decreased to 31
which is an indication
that the wettability was increased. Similarly, as seen in Fig. 9b, Ni-
coated fibers were wetted by the aluminum matrix with a sessile
drop angle of 81
. In Fig. 9a, the non-wetted fibers can be observed
in macroscale. On the otherhand, in Fig. 9b, it can be clearly seen in
 A. Alten et al. / Journal of Alloys and Compounds 787 (2019) 543e550 547

Fig. 6. Deposition rate of NieP coated carbon fiber as a function of pH and HP concentration (a) A1 bath (b) A2 bath.

Fig. 7. SEM micrographs of the nickel-coated carbon fiber as a function of deposition time (a) 15, (b) 30, (c) 60, (d) 120 min (pH 8, A2 bath).

Fig. 8. SEM micrographs of the nickel-coated carbon fiber (a) and transverse (b) and longitudinal directions (c) in MMC.

microscale that the fibers were completely wetted by the porosity or gap between the fibers and the matrix.
aluminum matrix. This is also supported by the SEM-EDS analysis Fig. 10a shows the SEM micrographs of composite samples
given in Fig. 10. The cross-section of the Ni-coated fiber reinforced fabricated with nickel coated carbon fibers under 30 MPa applied
matrix reveals that the contact is quite high with no apparent pressures and shows EDX spectrums (Fig. 10bed) obtained from
548 A. Alten et al. / Journal of Alloys and Compounds 787 (2019) 543e550
Fig. 9. The wettability of fibers with the cast aluminum matrix (a) SEM image of failed
composite produced using uncoated fiber and (b) cross-sectional view of the com-
posite produced using electroless Ni-coated fiber. In the inner pictures for uncoated
and coated fibers sessile drop test image are given.
selected points in Fig. 10a. It can be seen that the Ni coating is a
uniform layer separating the carbon fiber and the matrix. Naturally,
carbon has been identified at the fiber structure (Fig. 10b). Ni was
detected only at the interface between the fibers and aluminum
matrix alloy (Fig. 10c). However, no carbon or Ni was detected by
EDX in the aluminum alloy matrix (Fig. 10d).
3.5. Mechanical properties
The mechanical properties of the composite obtained through
the squeeze casting method were analyzed by three-point bending
test. Fig. 11 shows the bending stress of the composite samples
which is listed in Table 3. The bending strength of the Al 6063
matrix is 160 MPa, and the failure deflection is 5 mm. All AlNi
coated fiber composites show higher bending stress than Al 6063
base alloy and the S1 composite have the highest bending stress
with average value 258 MPa. This corresponds to 1.6 times
improved bending strength. It can be concluded CF increase me-
chanical properties which are attributed to the perfect wetting of
fibers as shown in SEM images Figs. 8b and c, 9b and 10a. When
compared to the same volume fractions of the samples, it is seen
that the composites produced by finer Ni coated fiber show better
strength behavior. It is suspected that increased Ni thickness on the
fibers causes embrittlement which decreases bonding between the
fiber and the matrix. Similarly, Hajjari [18] noted that the increase
in coating thickness negatively affects mechanical properties.
Additionally, it was also found that the composites produced in 2%
volume fraction exhibit better resistance than 4% volume fraction
(for both coating thicknesses). The decrease in bending strength
due to the increased volume fraction of fibers is mainly due to the
homogeneous distribution of fibers in the matrix. Closepacked
distribution of Ni coated fibers will generate notch effect which
decreases bending strength. Due to the accumulation of fibers, the
energy that needs to be absorbed by the matrix increases due to the
decreased aspect ratio. It is important to note that homogeneous
distribution of the short fibers can be achieved by mechanical
stirring [1]. On the other hand, Aybarc [28] shows that ultrasonic
stirring resulted in a better distribution of reinforcements.
The bending test results are in good agreement with the impact
tests. Charpy test results are given in Fig. 12. It can be seen that the
ductile 6063 without any reinforcement of fibers reveals the
highest impact properties. The CF reinforced samples that show the
highest bending strength revealed the lowest impact properties.
These findings also confirm the previously discussed effects of Ni
thickness and distribution of fibers in the matrix.
Vickers hardness test was applied from 10 different points on
the produced composite samples. The hardness values of the
samples were compared by taking the averages values. The Vickers
hardness values of the composites under a constant load of 10 kg
are given in Fig. 13. When the results were examined, the highest
hardness value was obtained at the S1 composite specimen,
although there were no significant changes in the hardness values
with the rest of the composites. The Vickers hardness increases up
to 70 HV from 40 HV for and fiberematrix interface and the matrix,
respectively (Fig. 13). Similar situation, ie, hardness change in ma-
trix and fiber-matrix interface, was also observed in other com-
posites. Comparing the two values, it can be seen that the interface
is 1.7 times harder than the matrix, which reflects the interdiffu-
sion, high solute atom concentrations and particulary good adhe-
sion at the interface.
4. Conclusions
The production of carbon fiber reinforced aluminum matrix
composites was successfully established. The wettability of carbon
fibers was enhanced by electroless Ni coating. The thickness of Ni
coating and phosphorous content was controlled by pH, time and
temperature and bath composition. As temperature and pH content
was increased, the coating thickness was increased from 3 mm to
7 mm. The increase in phosphorous content reversely affected the
coating thickness. It was found that HP content had a significant
effect on the coating thickness. The increase in concentration from
10 g/l to 30 g/l increased the thickness from 4 mm to 12 mm for
60 min where pH was between 8 and 9.
The hardness measurements revealed that the bonding and
wettability of Ni coated CF was enhanced. The matrix of 6063 had
an average of 40 HV while CF reinforced composite revealed 70 HV
in the fiber-matrix interface.
The bending strength of 6063 alloy was 160 MPa. After the
incorporation of carbon fibers, the strength was increased. The
highest strength was found to be 258 MPa for 0.9 mm Ni coated 2 wt
% CF added composite. When coating thickness was increased to
4 mm, the bending strength was decreased to 200 MPa which was
still 40% higher than the non CF added base alloy.
The impact strength of the base alloy (6063) was the highest
amongst the CF reinforced composites. The impact properties were
decreased by 42% when the alloy was reinforced with CF: As the
 A. Alten et al. / Journal of Alloys and Compounds 787 (2019) 543e550 549

Fig. 10. Microstructure and EDX results of the 6063 Al matrix in the composite. (a) SEM micrograph of the microstructure of S2, (b) EDX of point 1, (c) EDX of point 2 and (d) EDX of
point 3.

Fig. 11. Effect of volume fraction and coating thickness of CF on bending strength.
Fig. 13. Effect of volume fraction and coating thickness of CF on hardness test.

Acknowledgements

This work was supported by the Scientific Research Projects

Coordination Unit of Istanbul University (Project number: 24153).
The authors would like to thank for financial support.

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