Materials and Design 84 (2015) 402–410

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Materials and Design

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

Laser metal deposition of functionally graded Ti6Al4V/TiC

R.M. Mahamood a,b,⁎, E.T. Akinlabi a
a
Department of Mechanical Engineering Science, University of Johannesburg, Auckland Park Kingsway Campus, Johannesburg 2006, South Africa
b
Department of Mechanical Engineering, University of Ilorin, Nigeria

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

Article history: Functionally graded materials (FGMs) are advanced materials with improved properties that enable them to
Received 25 November 2014 withstand severe working environment which the traditional composite materials cannot withstand. FGM
Received in revised form 17 March 2015 found their applications in several areas which include: military, medicine and aerospace. Various manufacturing
Accepted 23 June 2015
processes are used to produce functionally graded materials that include: powder metallurgy, physical vapour
Available online 28 June 2015
deposition, chemical vapour deposition process and laser metal deposition process. Laser metal deposition
Keywords:
(LMD) process is an additive manufacturing process that can be used to produce functionally graded material di-
Deposition rectly from the three dimensional (3D) computer aided design (CAD) model of the part in one single process.
Laser LMD process is a fairly new manufacturing process and a highly non-linear process. The process parameters
Microstructure are of great importance in LMD process and they need to be optimized for the required application. In this
Titanium wear study, functionally graded titanium alloy composite was produced using optimized process parameters for
each material combination as obtained through a model that was developed in an initial study and the FGM
was characterized through metallurgical, mechanical and tribological studies. The results show that the produced
FGM has improved properties when compared to those produced at constant processing parameters for all
material combinations.
© 2015 Elsevier Ltd. All rights reserved.

1. Introduction
Functionally Graded Material (FGM) belongs to a class of advanced
materials with varying properties over its changing dimension [1,2].
Functionally graded materials are seen in nature as bones, teeth etc.
[3]. Nature designed these materials to meet their expected service re-
quirements. Functionally graded material is produced in order to elimi-
nate the sharp interfaces that exist in the traditional composite material
where failure is always initiated [4]. These sharp interfaces are replaced
with a gradient interface that produces smooth transition from one ma-
terial to the other [5]. One unique characteristics of FGMs is their ability
to be tailored for a specific application [1]. Functionally graded materials
find their applications in aerospace, automobile, medicine, sport, ener-
gy, sensors, optoelectronic etc. [6,7]. There are different kinds of fabrica-
tion processes for producing functionally graded materials, they
include: Physical or Chemical Vapour Deposition (PVD/CVD), Plasma
Spraying, Self-propagating High temperature Synthesis (SHS), powder
metallurgy technique, centrifugal casting method, and laser metal depo-
sition process [3,8]. Laser metal deposition process is a class of additive
manufacturing process that is capable of producing a functional part di-
rectly from its three dimensional (3D) computer aided model (CAD) of
⁎ Corresponding author at: Department of Mechanical Engineering Science, University
of Johannesburg, Auckland Park Kingsway Campus, Johannesburg 2006, South Africa.
E-mail address: mahamoodmr2009@gmail.com (R.M. Mahamood).
the part [9]. The part can also be made with functionally grade material
because LMD can use more than one material simultaneously.
Many researches have been conducted in the literature on the laser
metal deposition process [10–19] and specifically on functionally grad-
ed Ti6Al4V/TiC composite [20–22]. The importance of producing func-
tionally graded parts directly from the 3-D CAD model in one single
step has been the driving force for the research interest in FGM, by
using LMD. The earlier works tried to establish the feasibility of making
FGM through the LMD process [23,24]. In some other works, FGMs were
built using the LMD process, and then characterized. For example, in a
study conducted by Zang et al. [22], they deposited functionally graded
Ti/TiC on a Ti6Al4V substrate. They first established the processing pa-
rameters for various volume fractions of Ti/TiC composite in their pre-
liminary works. They used the results from their preliminary work to
successfully deposit a thin wall of functionally graded material — by
adjusting the processing parameters during the deposition process.
They showed that the wear-resistance performance of the Ti6Al4V sub-
strate was improved with the addition of TiC. They also showed that
FGM can be produced with LMD without a discrete interface. In their
preliminary studies, the method used to obtain the optimal process pa-
rameters for the various premix of Ti and TiC was not clear. Also,
premixing the powder before deposition can result in having the pow-
der with higher density to be deposited first before the less dense pow-
der. And this could affect the results (density of Ti is 4.5 g/cm3 and that
of TiC is 4.93 g/cm3). This could be one of the reasons why they observed
cracking in the deposit at 40% TiC. In another study performed by Wang

http://dx.doi.org/10.1016/j.matdes.2015.06.135
0264-1275/© 2015 Elsevier Ltd. All rights reserved.
 R.M. Mahamood, E.T. Akinlabi / Materials and Design 84 (2015) 402–410 403

et al. [21], a functionally graded material of Ti6Al4V/TiC was deposited. Table 1

They used Ti6Al4V wire and TiC powder; and the two materials were Optimized process parameters.

fed simultaneously. They achieved the compositional grading by keep- Sample % TiC Laser power Scanning Powder flow Gas flow rate
ing the wire feed rate of Ti6Al4V constant; while they varied the TiC designation (kW) speed (m/s) rate (rpm) (l/min)
powder feed rate. Also, other processing parameters were kept con- A 0 2.0 0.01 2.00 2.00
stant. They did not consider the effect of processing parameters on the B 5 2.0 0.0075 3.00 2.00
resulting deposit properties. Liu and DuPont [25] successfully deposited C 10 2.2 0.0075 2.00 2.00
D 15 2.26 0.0075 2.00 2.00
functionally graded material of Ti/TiC composite using LMD. They relied
E 20 2.21 0.0077 2.00 2.00
on the controller in LENS, which monitors the melt pool area and con- F 25 2.19 0.0078 2.00 2.00
trols the laser power to achieve a constant melt pool area, for the depo- G 30 2.16 0.0079 2.00 2.00
sition of their FGM. The melt pool area control in LENS is intended to H 35 2.14 0.0080 2.00 2.00
control the dimensional accuracy in the deposited part. Hence it does I 40 2.12 0.0081 2.00 2.00
J 45 2.10 0.0082 2.00 2.00
not control other properties of the deposited part. Shah [26] deposited K 50 2.07 0.0083 2.00 2.00
functionally graded material of Inconel 718 Nickel alloy and Ti6Al4V
using the laser-metal deposition process. The effect of the laser pulse
parameters and the powder flow rate on residual stress was studied.
The study found that the layer thickness plays an important role in the In this study, functionally graded Ti6Al4V/TiC was developed using
crack behaviour of the functionally graded material produced. The effect laser metal deposition process. The process parameters used to deposit
of the powder flow rate on the melt pool size was also studied; increas- each layer were obtained using a model that was developed in our ini-
ing the powder flow rate was found to increase the melt pool size. Lin tial study [30]. Trial experiments were first performed in order to estab-
et al. [27] used the laser-metal deposition process to produce function- lish the process window for the deposition of the porous free and fully
ally graded material of stainless steel-SS316L/super alloy-Rene88DT. dense deposit of TiC/Ti6Al4V composites. The results from these trial
They investigated the solidification behaviour and the microstructural runs formed the basis for the selection of the lower levels selected for
evolution of the FGM. Epitaxial growth and columnar dendrites' micro- the design of experiment. Screening experiment was then performed
structure were also observed. In situ functionally graded material using using full factorial design of experiment. The parameters screened
the laser-metal deposition process was also studied in the literature. Qin were: laser power, scanning speed, powder flow rate and gas flow
et al. (2011) [28] produced in situ functionally graded TiC reinforced ti- rate. The gas flow rate was found to be the least significant process pa-
tanium matrix from Ti and Cr3C2 powder using laser metal deposition rameter. The percentage TiC was then added to the remaining process
process. The functionally graded material was achieved by changing parameters for the RSM that was used to develop the model. The
the powder flow rate of the Ti and the Cr3C2 powder. The microhardness model was used to generate the optimized process parameter for each
and the wear-resistance properties were studied. The microhardness of the layers in the functionally graded Ti6Al4V/TiC composite. The de-
and the wear resistance were found to be greatly improved. The prob- veloped FGM was characterized metallurgically, mechanically and
lem with functionally graded material produced in situ is that the mag- tribologically. The developed FGM produced at optimized process
nitude of reinforcement achieved will largely depend on the reactions parameters was compared to the one produced at constant process
taking place during the deposition and cooling process. It would be parameters and the substrate. The results are presented and discussed
very difficult to achieve a desired percentage ratio of the reinforcement in detail.
and the matrix.
There is no doubt that different Ti6Al4V/TiC ratios would have differ- 2. Materials and methods
ent optimal process parameters; but these were not considered in any of
the above studies. It has also been demonstrated that having powders Annealed 5 mm thick sheet of 99.6% pure Ti6Al4V was used as the
placed in separate hoppers is an effective way of producing composite, substrate for the laser metal deposition of the functionally graded
with proper composition control, and without segregation due to differ- Ti6Al4V/TiC composite samples. The sheet was supplied by supplied
ence in the densities of the powders [29]. This method was employed in by the VSMPO-AVISMA Corporation, Russia. The sheet was cut into
this study. square shape of 72 × 72 mm and sandblasted and cleaned with acetone

Fig. 1. (a) Experimental set-up and (b) schematics of the LMD process [31].
404 R.M. Mahamood, E.T. Akinlabi / Materials and Design 84 (2015) 402–410

prior to the deposition process. The purpose of the sandblasting is to

roughen the surface of the substrate in order to aid the laser-power ab-
sorption process. Shining surface would reflect most of the laser beam.
The Ti6Al4V and the TiC powder used in this study were supplied by
F.J. Brodmann and Co., L.L.C., Louisiana. The Ti6Al4V powder use is of
99.6% purity, with particle size range of between 120 and 350 μm. The
TiC powder used is a ball-milled powder of particle size range below
60 μm. A 4.0 kW Nd: YAG laser was used for the deposition process

Fig. 3. Photograph of the functionally graded Ti6Al4V/TiC.

and it was attached to a KUKA robot. The laser spot diameter was main-
tained at 2 mm at a focal distance of 195 mm above the substrate. A co-
axial nozzle was attached to the robot's end effector for the powder de-
livery into the melt-pool. The shield gas used for carrying the powder as
well as to protect the deposited samples from the environmental attack

Fig. 2. (a) The micrograph of the substrate (Ti6Al4V) [33]. (b) The SEM micrograph of the Fig. 4. Optical micrograph of the functionally graded Ti6Al4V/TiC at: (a) optimized parameter
Ti6Al4V powder [33]. (c) The SEM micrograph of the TiC powder [33]. settings and (b) fixed parameter settings.
 R.M. Mahamood, E.T. Akinlabi / Materials and Design 84 (2015) 402–410 405

was Argon gas. The experimental set-up is available at the CSIR National Spectrometry (EDS). The microhardness profiling was taken on the
Laser Center, Pretoria and it is shown in Fig. 1a. The laser metal deposi- cross section of the samples (polished) using the MH-3 Vickers Micro-
tion process was achieved by creating a melt pool on the surface of the hardness indenter (by Metkon) with a load of 500 g and a dwell time
substrate by the laser and the powders were delivered into the melt of 15 s. The distance between the indentations was maintained at
pool by a powder feeder. Each of the powders was placed in each hop- 12 μm which is more than twice the indentation diameters. The X-ray
per of the powder feeder. The nozzles from the feeder were attached co- diffraction analysis was performed using the X-ray diffractometer (by
axially to the robot. The substrate was fixed in place and the robot was Ultima IV) which was used to study the phases present. The tribological
moved to perform the deposition process. The schematic of the LMD property was conducted on the surface of the samples after grinding to
process is shown in Fig. 1b. 1000 μm using the ball on a disk tribotester (by Cert) with tungsten car-
The functionally graded material was produced from 100% Ti6Al4V: bide ball of diameter 10 mm. A load of 25 N, a sliding distance of 2000 m
0% TiC to 50% Ti6Al4V: 50% TiC. The optimized process parameters that and the sliding speed of 0.02 m/s were employed during the wear test.
were used to deposit each of the functionally graded layers are present- The tests were conducted in the dry air without lubrication. The wear
ed in Table 1. To be able to compare the results, another functionally volumes were calculated using the equation proposed by Sharma et al.
graded Ti6Al4V/TiC was deposited at constant process parameters as [32] in Eq. (1).
follows: laser power 2.5 kW, scanning speed 0.01 m/s, powder flow
rate 2 rpm and gas flow rate 2 l/min. Four layers each was deposited
at 50% overlap percentage. "  1=2 #

w
w 2 w2
After the deposition process, the samples for the metallurgical ex- 2 −1
V ¼ L r sin − r −
amination were sectioned to reveal the cross sections. The cut samples 2r 2 4
"    1=2 #
were mounted in hot resin; the mounted samples were ground and 2 1=2
π 3 2 2 w w2 2 w2
polished according to the standard metallurgical preparation of titani- þ 2r −2r r − − r − ð1Þ
3 4 4 4
um and its alloys. The polished samples were etched using Kroll's re-
agent. The microstructures were studied using Olympus Optical
microscope (BX51M; Olympus) and the Scanning Electron Microscope where V is the wear volume in mm3, r is the ball radius, w is the wear-
(SEM) (by TESCAN) equipped with the Oxford Energy Dispersion track width and L is the stroke length.

Fig. 5. Micrograph of the top layer of the functionally graded sample at: (a) optimized process parameters; (b) (a) at higher magnification; and (c) at fixed-process parameters; (d) (c) at
higher magnification.
406 R.M. Mahamood, E.T. Akinlabi / Materials and Design 84 (2015) 402–410

3. Results and discussion

The micrographs of the substrate are shown in Fig. 2a, the morphol-
ogy of the Ti6Al4V powder is shown in Fig. 2b and that of the TiC powder
is shown in Fig. 2c. The microstructure of the substrate (see Fig. 2a)
shows white parts and the dark parts. The white part is the alpha grains
while the dark parts are the beta grains which are the characteristic of a
typical Ti6Al4V. The Ti6Al4V powder is spherical in shape (see Fig. 2b)
which is typical of a gas atomized powder. Spherically shaped powder
is more favoured in the laser deposition process because they maximize
laser absorption. The TiC powder is an irregular shaped powder which is
the characteristic of a ball milled powder. The photographs of the
deposited functionally graded materials are shown in Fig. 3. The sample
labelled 1 is the FGM produced at constant or fixed processing parame-
ters, i.e. for material combinational ratio from 100% Ti6Al4V: 0% TiC to
50% Ti6Al4V: 50% TiC, the same processing parameters (laser power
2.5 kW, scanning speed 0.01 m/s, powder flow rate 2 rpm and gas
flow rate 2 l/min.) were used to deposit all these material compositions
in the FGM sample. The micrograph labelled 2 in Fig. 3 is the one in
which each layer of the FGM was produced at optimized process
parameters as obtained in Table 1. The macrograph of the FGM sample
produced with the optimized process parameters is shown in Fig. 4a
and the one produced at a fixed-process parameter is shown in
Fig. 4b. It can be seen from Fig. 4 that the FGM produced at optimized
process parameter is taller than the FGM produced at constant process
parameters.
Whereas the width of the sample produced at constant process pa-
rameters is larger than that produced using optimized process parame-
ters. This can be attributed to higher dilution seen in the sample
produced at constant process parameter that makes is to be shorter
and wider. Dilution rate has been established to be proportional to the
melt pool size produced [33]. The bigger the melt pool, the longer it
takes to solidify and hence the more the degree of mixing of the base
material and the deposited powders.
The microstructures of the topmost parts of the two samples are
shown in Fig. 5. The sample produced at the optimized process param-
eters is shown in Fig. 5a; the unmelted Carbides (UMC) is seen in the
microstructure. The higher magnification of the sample in Fig. 5a is Fig. 6. (a) The SEM microstructure of the optimized FGM sample showing the UMC; and
(b) the EDS analysis of the point A label in (a).
shown in Fig. 5b. The sample produced at fixed-processing parameters
is shown in Fig. 5c; and fewer UMCs are seen in the microstructure.
This shows that most of the TiC powder had fully melted; and the higher
magnification micrograph of the sample in Fig. 5c shown in Fig. 5d
displayed mostly dendritic TiC. The phases are: alpha Ti, TiC and Ti3 Al. The TiC has the highest
Comparing Fig. 5b and d, it can be seen that that there are a larger percentage of 49%. The intermetallic compound Ti 3Al formed is
number of UMCs in the sample that was produced at optimized process 22%. The Ti3Al is shown in Fig. 9 as indicated by EDX analysis of the
parameters (see Fig. 5b) compared to the sample produced at fixed SEM micrograph of the optimized FGM sample.
processing parameters. The SEM micrograph of the sample prepared The average wear volume obtained using Eq. (1) for the optimized
at optimized process parameters is shown in Fig. 6a, showing some functionally graded Ti6Al4V/TiC composite, designated as sample A,
of the UMCs. and that of the one produced at fixed-process parameters (sample
To confirm the UMC particles, an EDX analysis was performed on the B) are presented in Table 2. The wear volume of the substrate, designated
UMC, using the Oxford EDX equipped with the TESCAN SEM. The EDX as PM, is also presented in the Table for comparison.
analysis of the label ‘A’ in Fig. 6a is shown in Fig. 6b. The EDS confirms From Table 2, it may be seen that the sample produced with the
that those points are unmelted carbide particles. The SEM micrograph optimized-process parameters (sample A) has the lowest wear volume.
of the sample produced at optimized process parameters is shown in The substrate material (PM) has the highest wear volume. This is ex-
Fig. 7, showing the different layers. pected because of the property of titanium that makes it chemically re-
It can be seen how the how the microstructure changes with the active to itself, or to other materials with which it comes into contact in
height of the functionally graded material. The point D, which contains sliding or rubbing action. The wear mechanism that takes place on the
the lowest percentage of the TiC displayed a microstructure that is typ- PM sample is a combination of abrasion, adhesion and plastic deforma-
ical of laser deposited Ti6Al4V, which is columnar in nature that grows tion. The abrasion wear mechanism starts the moment the counter body
epitaxially on the globular microstructure of the heat affected zone. This is engaged, as a result of the rubbing action of the two surfaces in con-
shows that the low percentage of the TiC is not seen as a different mate- tact. As the rubbing action of the two surfaces in contact continues,
rial, which is the aim of the functionally graded material: That is, the the frictional force between the two surfaces increases. The increase in
eradication of the sharp interface that shows the distinction between the frictional force resulted in strong adhesion of the two surfaces in
the different materials. An XRD analysis was performed on the opti- contact. This causes the coefficient of friction (COF) to increase. The
mized FGM sample; and it revealed three different phases, as shown COF of the substrate and that of the optimized FGM sample are compared,
in Fig. 8. and shown in Fig. 10.
 R.M. Mahamood, E.T. Akinlabi / Materials and Design 84 (2015) 402–410
Fig. 7. SEM micrograph of the sample produced at optimized-processing parameters, showing the top (A); middle (B); lower level (C); and the dilution region (D).
This strong adhesion and the sliding action of the two surfaces in-
creases the temperature of the surfaces, which resulted in plastic defor-
mation, which eventually leads to shearing and tearing of the surface of
the Ti6Al4V. Some of the debris produced from the tearing and shearing
of the Ti6Al4V surface adheres to the surface of the tungsten carbide
ball; while the rest stays in between the two surfaces. This debris
worsens the wear action, as it changes the two-body wear mechanism
to a three-body wear mechanism.
As the sliding action continues, the debris becomes work-hardened
and it cuts deeper and deeper into the substrate. The debris cutting
Fig. 8. XRD analysis showing the phases present in the optimized FGM sample.
407
into the substrate results in the characteristic parallel grooves, as de-
scribed by Wu et al. [34], and this is shown in Fig. 11. Fig. 11a shows
the low magnification of the wear track of the substrate; and the higher
magnification is shown in Fig. 11b.
The wear track of the sample produced at a constant process param-
eter is shown in Fig. 12a. The wear resistance of this sample is far better
than that of the substrate shown in Fig. 11b because of the TiC content of
the FGM sample. Although, the sample was not produced at optimized-
process parameters, yet the wear behaviour is better than that of the
substrate. The wear track of the optimized sample is shown in Fig. 12b.
The sample showed the best wear resistance behaviour, because
there were reasonable quantities of UMC retained in the sample,
which then forms powder lubrication between the surfaces during the
sliding action [33]. The few UMC found in the sample produced at
fixed-process parameters also helped in the wear resistance behaviour
of that sample; but not as much as that of the sample produced at
optimized-process parameters. The process parameter optimization
using the developed model was really helpful in producing the low
wear volume observed in the optimized sample. Although intermetallic
compounds are present in the sample, which are very hard, but it was
found that this compound is not detrimental to the wear property of
this composite. Instead, it served as reinforcement, and helped to im-
prove the wear-resistance property of the FGM sample. The Ti3Al has
been proved in the literature to improve the wear properties of some
metals [35,36].
The microhardness test was performed on the optimized FGM sam-
ple, and the substrate using the Vickers hardness tester with a load of
500 g. Fig. 13a shows the microhardness graph of the optimized FGM
sample. Fig. 13b shows the bar chart of the average microhardness
value of the optimized FGM sample and compared to that of the parent
material.
It may be seen that the microhardness value of the topmost part of
the FGM sample is as high as 1200 HV, which is as high as four times
408 R.M. Mahamood, E.T. Akinlabi / Materials and Design 84 (2015) 402–410

Fig. 9. (a) The SEM microstructure of the optimized FGM sample showing the intermetallic compound; and (b) the EDS analysis of the spectrum labelled 2 in (a).

Table 2 4. Conclusion
Wear volume for samples A, B and PM.

Sample designation Wear volume (mm3) Functionally graded Ti6Al4V/TiC composite has been developed
A 0.021
using laser metal deposition process and characterized in terms of
B 0.033 microstructure, microhardness and wear resistance behaviour.
PM 0.120 The functionally graded material was produced using optimized process
parameters obtained from earlier developed empirical model. The
optimized functionally graded Ti6A4V/TiC composite produced
was compared with a functionally graded Ti6Al4V/TiC which was
produced at fixed-process parameters as well as the substrate.
The wear behaviour of the two functionally graded samples was
compared with that of the substrate material (Ti6Al4V). The results
showed that the optimized functionally graded produced sample
has the best wear-resistance behaviour. Also the microhardness is
found to be improved and as high as 1200 VHN which is four
times that of the substrate. The high microhardness also contributed
to the improved wear resistance. In the literature, functionally graded
materials are usually produced using constant processing parameters
Fig. 10. The plot of coefficient of friction versus sliding time of the substrate and the opti- for each of the compositional ratio in the FGM. The same setting
mized FGM. for each of the layer in the FGM does not produce each layer optimized
for the property of interest. This study has shown that producing
that of the substrate as shown in Fig. 13b. The high hardness is as a result functionally graded material using optimized process parameters
of the TiC content; and it is responsible for the improved wear resistance for each compositional material ratio in the gradient has a better
behaviour of the optimized FGM sample. property.

Fig. 11. The SEM micrograph of the wear track of the substrate at (a) low magnification [33] and (b) higher magnification [33].
 R.M. Mahamood, E.T. Akinlabi / Materials and Design 84 (2015) 402–410
Fig. 12. SEM micrograph of the wear track of: (a) FGM at fixed-process parameter and (b) FGM at optimized-process parameters.
Because each of the layers of the functionally graded material is able
to withstand extreme working condition even if the succeeding layer
has been lost to wear.
Fig. 13. (a) The microhardness of the optimized FGM across the section of the sample;
(b) the bar chart of the average microhardness of the optimized FGM and that of the sub-
strate material.
409
Acknowledgements
This work is supported by the Rental Pool Programme of National
Laser Centre, Council of Scientific and Industrial Research (CSIR-NLC
Reference: LREIB00), Pretoria, South Africa. The Department of Chemi-
cal and Metallurgical Engineering is appreciated for the facilities used
at the materials lab.
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