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Materials and Design 54 (2014) 531–538

Contents lists available at ScienceDirect

Materials and Design


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

Parametric study of development of Inconel-steel functionally graded


materials by laser direct metal deposition
Kamran Shah a,⇑, Izhar ul Haq a, Ashfaq Khan b, Shaukat Ali Shah b, Mushtaq Khan c, Andrew J Pinkerton d
a
Institute of Mechatronics Engineering, University of Engineering & Technology, Peshawar, Pakistan
b
Mechanical Engineering Department, University of Engineering & Technology, Peshawar, Pakistan
c
School of Mechanical & Manufacturing Engineering, National University of Sciences & Technology, Sector H-12, Islamabad 44000, Pakistan
d
Department of Engineering, Lancaster University, Bailrigg, Lancaster LA1 4YR, United Kingdom

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

Article history: Laser direct metal deposition (LDMD) has developed from a prototyping to a single and multiple metals
Received 8 January 2013 manufacturing technique. It offers an opportunity to produce graded components, with differing elemen-
Accepted 22 August 2013 tal composition, phase and microstructure at different locations. In this work, continuously graded Stain-
Available online 2 September 2013
less Steel 316L and Inconel 718 thin wall structures made by direct laser metal deposition process have
been explored. The paper considers the effects of process parameters including laser power levels and
Keywords: powder mass flow rates of SS316L and Inconel 718 during the deposition of the Steel–Ni graded struc-
Laser
tures. Microstructure characterisation and phase identification are performed by optical microscopy
Deposition
Cladding
and X-ray diffraction techniques. Mechanical testing, using methods such as hardness, wear resistance
Functionally graded and tensile testing have been carried out on the structures. XRD results show the presence of the NbC
Stainless steel and Fe2Nb phases formed during the deposition. The effect of experimental parameters on the micro-
Nickel alloy structure and physical properties are determined and discussed. Work shows that mechanical properties
can be controlled by input parameters and generation of carbides provides an opportunity to selectively
control the hardness and wear resistance of the functionally graded material.
Ó 2013 Elsevier Ltd. All rights reserved.

1. Introduction producing bulk FGMs, the shapes and sizes are usually limited be-
cause of the use of dies for pressure-aided densification.
The concept of Functionally Graded Materials (FGMs) was pro- Laser direct metal deposition (LDMD) process is able to fabri-
posed in 1984 by material scientists in the Sendai area in Japan as a cate complex prototypes in near-net shape, leading to time and
means of preparing thermal barrier materials [1]. FGMs are a class machining cost savings. A variety of metals and alloys has been
of advanced materials of which the composition and microstruc- deposited by the process, for example steel such as H13 [11],
ture change gradually from one side to the other, resulting in a cor- WC–Co [12], and Stellites such as Stellite 13. Application of the la-
responding variation in the properties [2]. These materials can be ser deposition process to manufacture a metal–ceramic FGM was
designed for specific function and applications. Moreover, a graded first accomplished by Jasim et al. [13]. Various researchers have
change in material allows a reduction of stress concentrations since applied this concept to build a range of FGMs for various
appearing near a sharp interface between two different phases. To- applications. Pei and De Hosson [14] produced AlSi40 functionally
day, the FGM concept extends over a variety of sectors all across graded material using an Nd: YAG laser, whereas Thivillon et al.
the world. FGMs have found their place in fields like bio-medical, [15] analysed the fabrication of Co based Stellite 6 and Nickel super
automotive and aerospace, electronics, optics, and nuclear applica- alloy Inconel 625 by laser deposition technique. Ouyang et al. [16]
tions, reactor components and energy conversion [3,4]. developed a WC–(NiSiB alloy) ceramet/tool steel functionally
There are several techniques such as die compaction [5–7], graded material (FGM) by the laser cladding technique for high-
plasma spraying [8], slip casting [9] and powder metallurgy [10] temperature tribological applications. Lin et al. [17] investigated
that are currently used for producing FGMs. Die compaction and the solidification behaviour and the morphological evolution dur-
plasma spraying are generally applied for fabrication of function- ing the compositional gradient of stainless steel to Rene88DT.
ally graded coatings and the FGM coatings made by plasma spray- Nickel and steel alloys are widely used in the power and nuclear
ing are not dense. Although powder metallurgy can be utilised for industries. Austenitic stainless steels possess high corrosion resis-
tance due to the formation of a chromium-rich thin oxide film at
⇑ Corresponding author. Tel.: +92 334 593 4002. the surface. This can vary in thickness and also develop into a du-
E-mail address: Kamran.Shah@nwfpuet.edu.pk (K. Shah). plex layer with an additional outer layer in some conditions but

0261-3069/$ - see front matter Ó 2013 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.matdes.2013.08.079
532 K. Shah et al. / Materials and Design 54 (2014) 531–538

Table 1
Experimental process parameters.

Sample no. Power (W) Powder mass flow rate (g/s)


1 450 0.632
2 550 0.632
3 650 0.632
4 750 0.632
5 450 0.834
6 550 0.834
7 650 0.834
8 750 0.834

their good resistance to corrosion remains [18]. Joining steels is not


usually a problem as austenitic welds are resistant to hot cracking,
stress and severe impacts during service conditions [19,20]. The Fig. 1. Direct laser metal deposited SS316L/Inconel 718 functionally graded Sample
nickel-chromium alloy Inconel 718 alloy is appropriate in applica- no. 6 (A) 100% SS 316L, (B) 75% SS 316L, (C) 50% SS 316L, (D) 25% SS 316L and (E) 0%
tions where high temperatures are observed and the atmosphere is SS 316L.
highly carburising and oxidising [21,22]. The properties of nickel
and stainless steel alloys make them suitable for many applica-
tions, for example nuclear power generation and oil refineries
where such conditions exist. Nevertheless, these two alloys are of-
ten still joined together by fusion welding, which can result in
weak resistance to solidification cracking [23]. To overcome this
problem of cracking, functionally grading of the alloys represents
a viable solution but there are many process parameters to control.
This study investigates the influence of process parameters on a
graded Stainless Steel 316L and Inconel 718 thin wall structure
made by the direct laser metal deposition process. The aim of the
investigation is to establish the effect of the process parameters
on the microstructure, hardness and wear resistance. Although
these two materials have been well studied separately, this is an
investigation that has not been performed with this combination
previously. An earlier paper by Wu et al. [24] performed hardness
wear and microstructure examinations of a graded 316L-Inco-
nel718 wall but considered only one wall built at a single set of
parameters.
The most meaningful parameters in LDMD are commonly taken
as specific energy (defined as power/(beam diameter  traverse
speed)), which gives the energy density on the surface, and line
mass (defined as powder flow/traverse speed), which gives the
mass of material available for deposition per unit length of track
[25]. In this work, the effects of both are tested by taking laser
power and powder mass flow rate as the ‘primary’ process vari-
ables. Traverse speed and other ‘secondary’ process parameters
such as gas flow speeds and substrate finish and temperature are
maintained constant. Existing studies show that different fixed val-
ues of these parameters would likely affect the absolute value of
the measured results but not the fundamental LDMD process and
trends identified [26,27].

2. Experimental procedure

A Laserline LDL160-1500 1.5 kW Diode laser was used for the


laser deposition process. A Stainless Steel 316L substrate was
positioned such that the beam was orthogonal to the surface
and of size 2.5 mm (fast axis)  3.5 mm (slow axis) at the sub-
strate. Before the experiment, SS316L substrate was grit blasted
in a Guyson grit blaster and then degreased using ethanol. The
movement in x and y-axes (horizontal plane) was controlled by Fig. 2. (a) Effect of laser power and powder flow rate on mean layer height. (b)
a CNC table. The whole setup was kept in an argon-filled chamber Effect of laser power and powder flow rate on mean layer width.
(glove box). A FST PF-2/2 disc-type powder feeder, containing two
powder canisters with a capacity of 1.5 L each was used to deliver
Stainless Steel 316L powder (50–120 lm particle diameter) and 1.0% Si, 16.0–18.0% Cr, 10.0–14.0% Ni, 2.0–3.0% Mo, 60% Fe and
Inconel 718 (53–150 lm diameter). The chemical composition 0.042% C, 18% Fe, 19% Cr, 0.5% Al, 1% Ti, 3% Mo, 5% Nb and 55%
of Stainless Steel 316L and Inconel 718 were 0.03% C, 2.0% Mn, Ni respectively.
K. Shah et al. / Materials and Design 54 (2014) 531–538 533

Fig. 3. Sample 3 transverse cross section showing the Inconel 718 addition along the wall.

percentage of Inconel 718 in the deposition mixture by 25% every 3


layers while reducing that of the SS 316L powder. Powders were con-
veyed to the melt pool by argon gas from a coaxial nozzle. A two-
channel powder feeder was used allowing mixing of the powders in
the nozzle before deposition. The nozzle was aimed at the centre of
the laser beam on the substrate and moved parallel with the slow axis
at the traverse speed of 4 mm/s. The process parameters used in the
experiments are shown in Table 1. Exact values of process parameters
were chosen based on previous experiences with the experimental
setup, which showed an operating window of approximately 42–
80 J/mm2 specific energy for good quality tracks.
Prepared wall samples were sectioned in a transverse plane,
mounted in Struers epoxy resin and polished to 4000 grit size.
All samples were electrolytically etched in 10% oxalic acid using
a 6 V DC potential. The graded microstructures were studied by
means of optical microscopy technique. Energy dispersive X-ray
spectroscopy (EDS) analysis was used to investigate the elemental
composition. Micro-hardness testing was carried out on the cross-
sectional planes of built walls. Wear testing was carried out using a
Teer Coatings (POD-2) pin-on-disc wear tester in which samples
were subjected to wear by rotation in contact with a WC–Co ball.

3. Results

3.1. Macrostructure and dimensions

All parameter combinations formed thin continuous wall struc-


tures. All of the samples produced for analysing the effect of power
Fig. 4. Equiaxed grain structure observed at the side of the walls (this image taken
from sample 4). and powder flow rates were well adhered to the substrate with no
signs of track discontinuity and appeared structurally sound. Fig. 1
The Stainless Steel 316L and Inconel 718 powders were initially shows an example of a graded wall produced at a power of 550 W
weighted separately and then mixed with a mechanical stirrer for and powder mass flow rate of 0.834 g/s (sample 6).
30 min according to the desired weight percentage. Grading of the Analysis of the track dimensions revealed a marked trend to-
two materials was achieved by depositing 3 layers of 100 wt% wards larger deposits with increasing power. The variation in layer
SS316L on SS316L substrate block and then increasing the weight height and layer width with the primary input variables of
534 K. Shah et al. / Materials and Design 54 (2014) 531–538

Fig. 6. (a–e) XRD patterns at different location along the SS 316L-Inco 718 gradient
obtained for sample 8. (a) 100% SS 316L, (b) 75% SS 316L, (c) 50% SS 316L, (d) 25% SS
316L and (e) 0% SS 316L.

all the FGM structures. Fig. 3 shows how this occurred in sample
3 as an example. At the edges of the cross-section, columnar to cel-
lular dendritic growth transitions were observed and these struc-
tures was also seen to prevail at layer boundaries throughout all
the parts as shown in Fig. 4.
The secondary dendrite arm spacing (SDAS) was measured for
each layer of all the samples and the average of three layers was
taken to represent deposition at each powder composition. Plots
of average SDAS for 0.632 g/s and 0.834 g/s powder flow rate depo-
sition are shown in Fig. 5(a and b). For the range of parameters ana-
lysed, SDAS ranging from 4.49 lm to 8.44 lm were measured for
Fig. 5. (a) Change in Mean SDAS from bottom to top of the wall at low powder flow low powder flow rate deposition, with the highest SDAS being pro-
rate (0.632 g/s). (b) Change in Mean SDAS from bottom to top of the wall at high duced with the 100% Inconel 718 powder. For high powder flow
powder flow rate (0.834 g/s). rate deposition parameters, SDAS ranged from 4.13 lm and
delivered power and powder mass flow rate are shown in Fig. 2(a 7.76 lm. This trend clearly suggests that with increased powder
and b) respectively. flow rate, SDAS is decreased. This effect can be attributed to the in-
Mean layer heights ranging from 0.54 mm to 0.76 mm were ob- creased powder mass flow rate leading to more rapid quenching
served for low powder flow rate deposition samples, while the that produces the finer dendritic structure observed. Moreover,
mean layer height range for high powder flow rate deposition SDAS increased with the height of the build showing that the local
was between 0.63 mm and 0.84 mm, with track height increasing cooling rate also decreased somewhat with increasing distance
with increasing power. Similar trends were observed for track from the substrate, which acts as a heat sink. This is because the
width, with the lowest mean layer width of 1.31 mm at a power average thermal gradient in the build direction decreases as the
of 450 W and a mean of 1.65 mm at a power of 750 W for the distance from the substrate increases.
low powder flow rate deposition process. At high powder flow rate, The microscopic characteristics of samples produced under dif-
a lowest mean layer width of 1.37 mm at 450 W and highest mean ferent powder flow rates are not significantly different apart from
layer width of 1.68 mm at 750 W were observed. their secondary dendritic arm spacing (SDAS).
For all the samples, layer dimensions are limited by the avail- No evidence of liquation cracks or solid-state cracks induced by
able laser power; however when laser power is increased above the thermal stresses produced in the wall were observed despite
a critical value in layer height and width start to plateau. This the different pool compositions produced during the deposition
shows that when laser power is increased above a critical value of a full wall. The liquation cracking susceptibility of both austen-
insufficient powder is available to utilise all that laser power and itic alloys such as 316L and nickel alloys such as Inconel 718 in-
consequently the deposition moves from a laser power limited re- creases markedly with grain size [28,29] so it is probable that
gime to a powder limited regime [25]. This explains the flattening the fine microstructure detailed above provided some protection
of the graphs in Fig. 2(a and b). against this.

3.3. Phase analysis using X-ray diffraction technique


3.2. Microstructure
Fig. 6(a–e) shows the XRD patterns from representative wall
The multi-layered walls showed good bonding between the lay- sections taken perpendicular to the gradient direction for sample
ers. It was noted that columnar dendritic growth prevailed in the 8. Similar patterns were obtained for the rest of the samples.
K. Shah et al. / Materials and Design 54 (2014) 531–538 535

Fig. 7. Fractured surface of sample 1 with enlarged view of the surface.

of sample 1 as an example of the failure surface seen for all


samples.
A summary of the ultimate tensile strength data plotted versus
laser power in Fig. 8 shows a trend for ultimate tensile strength to
decrease with laser power. Moreover, tensile strength seems to in-
crease with power mass flow rate. The low powder flow rate depo-
sition process is found to give tensile strengths of 526–573.5 MPa,
while the high powder flow rate deposition process gives tensile
strengths ranging between 531 MPa and 596 MPa. The reduction
of tensile strength can be explained by the fact that the grains
get larger in size with the increasing heat input and thus offer less
resistance to the applied load [30].

3.5. Hardness distribution

Vickers micro-hardness measurements of walls produced at dif-


ferent powder mass flow rates and power levels were made along
Fig. 8. Effective ultimate tensile strength variation as a function of power at
the height of walls from bottom to top. Results are plotted in Fig. 9
different powder flow rates. as a function of the number of layers from the substrate. Fig. 9(a)
shows an approximately parabolic distribution of hardness with
Fig. 6(a and b) shows that structures produced with 100% and 75% a maximum measured hardness of 186.1 HV0.1 in the final layer
of SS316L were entirely austenitic with a minimum degree of fer- and 168.1 HV0.1 in the first layer with high powder flow rate depo-
rite. It also indicates lack of any clear orientation of the microstruc- sition. Hardness value of 155.6 HV0.1 and 179.3 HV0.1 are observed
ture. As the Inconel 718 weight percentage increases, new phases in the bottom and top layer for low powder deposition process. For
comprised of Niobium Carbide (NbC) and Fe2Nb are formed, as the other three power levels, similar distributions are measured,
shown in Fig. 6(c–e). with variation in the magnitudes measured. Furthermore, high
powder flow rate deposition exhibits higher hardness compared
to low powder flow rate deposition in most cases. Fig. 9(a–d)
clearly shows that, within the multilayer builds studied, the hard-
3.4. Tensile testing ness initially decreased until weight percentage of Inconel 718 was
approximately increased to 50%. From this percentage onwards,
Tensile tests were carried out parallel to the deposition or laser and increase in the hardness of layers was observed.
scanning direction at room temperature using an INSTRON 4507 It is worth noting that there is a significant increase in the hard-
universal tensile testing machine operating with a crosshead speed ness in the top layers of all the samples. This could be explained by
of 1 mm/s. All the samples were tested on an as-deposited basis the fact that the final layer was not reheated, unlike the other lay-
and effective ultimate tensile strength was calculated for each ers beneath it.
sample. After tensile testing, the fracture surface was observed
using a Hitachi S-3400N SEM. 3.6. Wear testing
All samples failed by ductile fracture with only a moderate
amount of deformation. For all samples, fracture started initially All the sample walls were separated from the 316L substrate,
at the 100% stainless steel 316L side and then propagated rapidly sectioned longitudinally at the middle of the wall and mounted
to the 100% Inconel 718 side. Fig. 7 shows the fractured surface on a Teer Coatings (POD-2) pin on disc wear tester. Specific wear
536 K. Shah et al. / Materials and Design 54 (2014) 531–538

Fig. 9. (a–d) Hardness profiles at various powers and powder mass flow.

rate was calculated using the software available with the slower the cooling rate during solidification, the longer the time
machines. available for grain coarsening.
In Fig. 10, mean specific wear rates for three layers of constant This response echoes that reported by Wu et al. [32] for tita-
composition under different power levels are shown. In all the nium alloys and Griffith et al. [26] for austenitic stainless steel
samples, mean specific wear rate (MSWR) exhibited an inverse who also found that high cooling rates at low powers resulted in
relation to the hardness as the composition was changed from fine grain structures.
Stainless steel 316L to Inconel 718. In the first three layers of It has also been noted that SDAS increased with the height of
100%, SS316L MSWR is low; it then increases when Inconel 718 the build suggesting that the local solidification time increased
is added in the next three layers. After the addition of more Inconel somewhat with increased distance from the substrate, which acts
718 in the next 9 layers MSWR reduces. This trend is noted for all as a heat sink. The increased solidification times arises from a low-
the samples. Overall MSWR is higher at higher power levels. er average cooling rate with distance from the substrate. This is be-
cause the average thermal gradient in the build direction decreases
as the distance from the substrate increases.
4. Discussion Analysis of tensile strength of the graded structure produced
under various operating conditions reveals an inverse relation be-
Varying laser power and powder flow rate has shown some tween the tensile strength and laser power. This is due to the same
scope for controlling high power diode laser deposition micro- factors discussed above except that here the cooling rates and ther-
structures. Minimising power and maximising powder flow rate mal gradients are reduced by increased power input rather than
is found to produce the finest grain structure, however these changes in heat sink properties.
changes in microstructure come at the expense of changes in layer It is interesting to note that hardness distribution in the sam-
height and width. ples followed an approximate parabolic curve unlike conventional
Refinement of the grain structure decreased and secondary arm single material deposition, in which the hardness of a sample typ-
dendritic arm spacing increased with increasing power. The de- ically decreases when measured vertically starting from the sub-
crease in cooling rate this produced meant there was enough time strate [33]. This can be explained by the XRD patterns that
for small dendrite arms to melt and disappear; thus the secondary indicate the presence of NbC and Fe2Nb when Inconel 718 percent-
dendrite arm spacing of the alloys increased [31]. Moreover, the age is increased. According to Fujita et al [34], NbC and Fe2Nb
K. Shah et al. / Materials and Design 54 (2014) 531–538 537

Fig. 10. Means specific wear rate along the gradient for various powers for 20 N load and sliding speed of 30 mm/s (a) 450 W, (b) 550 W, (c) 650 W and (d) 750 W.

improve the strength of a material, so hardness will increase when  Functionally grading of SS316L and Inconel 718 using laser
more Inconel 718 is added and more Nb is present to form NbC. deposition process is a feasible method of manufacturing.
An inverse relation is obtained for the wear rate and hardness of  Secondary dendritic arm spacing (SDAS) is strongly dependent
laser deposited SS316L and Inconel 718 graded walls. Niobium is on the power and powder mass flow rate.
currently used to modify stainless steels to get a good combination  The tensile strength of the functional part is inversely propor-
of thermal fatigue resistance, high temperature strength, corrosion tional to the laser power and increases with powder mass flow
resistance, for example in automotive exhaust systems [34,35]. It is rate.
well known that wear resistant materials can be obtained by rein-  Generation of carbide like NbC at higher Inconel proportions
forcing soft phases with harder phases [36,37] and the presence of creates an opportunity to selectively control the hardness and
hard Niobium Carbide (NbC) and Fe2Nb in the laser deposited sam- wear resistance of the functional material.
ples not only increased their hardness but also their wear resis-  The graded structure could be useful for applications where
tance. Such functional grading techniques provide a means to details of the loading conditions are known, in which case
engineer hardness and wear resistance according to an end user’s microstructure and thus properties could be designed to best
specific need. suit the loading for each section of a component.

5. Conclusions
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