Results in Engineering 24 (2024) 102966

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Results in Engineering
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Wear and corrosion properties of mechanically coated 316 stainless

Steel-TiC nanocomposites
Hesamoddin Hamedi , Taghi Isfahani *
Materials Engineering Group, Golpayegan College of Engineering, Isfahan University of Technology, 87717-67498, Golpayegan, Iran

A R T I C L E I N F O A B S T R A C T

Keywords: The mechanical coating (MC) method was used to deposit 316 stainless steel (SS316), TiC, and SS 316-TiC
Mechanical coating method nanocomposite coatings on SS 316 substrates using a ball mill machine at milling durations of 1, 2, 5, 10, and
TiC-SS 316 15 h using relatively cheap and abundant raw material. The chemical composition of the SS 316, TiC, and SS 316-
Wear properties
xTiC (x = 20, 50, 80 wt%) nanocomposite coatings deposited by the mechanical coating method has been
Corrosion properties
Microhardness
investigated and the hardness values and the wear and corrosion mechanisms were presented. Dense and uniform
coatings were obtained using a ball-to-powder weight ratio (BPR) of 20:1 and an MC duration of 5 h. Among the
samples, the SS316-20 wt%TiC coating exhibited the best wear and corrosion resistance. The least mean coef­
ficient of friction was 0.3 for the SS316-20 wt%TiC deposited sample while the largest mean coefficient was for
the SS316-80 % TiC sample to be 0.76. The SS 316-20 wt% TiC sample had the lowest wear rate where the
highest value was for the %100SS 316 sample being 0.36 × 10− 6 and 19 × 10− 6 (mm3/Nm), respectively.
Corrosion tests revealed that the SS316-20%TiC sample had the best corrosion resistance among the composite
samples having a corrosion resistance of 4.9358 μm/Y. The corrosion resistance decreased with the increase of
TiC whereas the 80 % TiC coating had severe pitting. Cracks and pores present in the non-uniform 100 % TiC
coating resulted in lower corrosion resistance compared to the 100 % SS 316 and composite coatings.

1. Introduction coating ceramics and ceramic-reinforced MMCs on metals. Up to now,

techniques such as chemical and physical vapor deposition, etc. [6] have
The unique properties of 316 stainless steel (SS 316) such as its su­ been used to apply carbide coatings on SS 316 substrates. The main
perior ductility and excellent corrosion resistance [1] have made it limitation of most techniques is that it is quite impossible or tricky to
widely applicable in various industries. However, its limited strength obtain coatings with high amounts of ceramic reinforcement particles.
and weak resistance to wear and abrasion at room and high tempera­ To overcome this problem mechanical coating technique can be applied.
tures have limited its application in harsh environments [2]. To over­ This technique can be applied to obtain a homogeneous distribution of
come this limitation, several techniques mostly having several reinforcement particles even in high amounts. The mechanical coating
complicated procedures using expensive equipment have been used to technique is a coating process that can be applied to obtain pure or
strengthen the steel alloys by coating ceramic particles or uniformly composite coatings. This technique uses a milling machine to mechan­
dispersing ceramic particles in the alloy matrix [3,4]. These methods are ically mill and deposit powders on a substrate [7] and is a simple
limited because of the significant physical difference between the steel low-cost and very effective technique in preparing coatings of appro­
substrate and ceramic coating. Furthermore, the potential properties of priate thickness [8]. In this technique, mechanical milling and me­
the ceramic reinforced metal matrix composite coatings (MMCs) are not chanical surface treatment are used. The ball collisions during the
used by many industries mostly due to the need for high processing procedure result in atomic interdiffusion providing a metallurgical
temperatures and melting point, fast solidification, high cost, and bonding by activating the surfaces of the milled powders [9]. The dy­
complicated process control equipment for safety precautions [5]. namic nature of this process is due to the intense ball-powder-substrate,
However, despite coating methods such as thermal and cold spraying, ball-powder-ball, and ball-substrate-ball collisions which result in
there is still a great demand for other low-cost and simple techniques for continuous cold welding and fracture phenomena [10]. This bonding

* Corresponding author.
E-mail address: t.isfahani@iut.ac.ir (T. Isfahani).

https://doi.org/10.1016/j.rineng.2024.102966
Received 11 May 2024; Received in revised form 29 August 2024; Accepted 20 September 2024
Available online 24 September 2024
2590-1230/© 2024 The Authors. Published by Elsevier B.V. This is an open access article under the CC BY-NC license (http://creativecommons.org/licenses/by-
nc/4.0/).
H. Hamedi and T. Isfahani Results in Engineering 24 (2024) 102966

Table 1
Chemical composition of the initial coating material of TiC and SS 316 powders.
Element (weight percent) TiC C Cr Ni Mo Mn Si P S Fe O Ca N Cu
Starting material

316 Stainless steel powder – 0.03 16 12 3 2 1 0.04 0.03 Balance – – – –

TiC powder 99.9 – – <2.8 ppm – – <22 ppm – – <201 <0.5 % <8 ppm <430 ppm <3 ppm
Ppm

obtained between the coating and substrate is strong and easily obtained
Table 2
at low temperatures without the need for expensive and complex facil­
Sample codes and the composition of the coated samples.
ities and complicated procedures [11]. These advantages have gained
the attention of many researchers for applying different coatings such as Sample code Sample

ceramic, metallic, and composite coatings [12] on different substrates. 100 % TiC 100 wt% TiC powder
Different parameters such as the ball-to-powder ratio (BPR) [13], and 80 % TiC 80 wt% TiC- 20 wt% SS316 powder
50 % TiC 50 wt% TiC- 50 wt% SS316 powder
the location of the substrate [12] are also important and affect the
20 % TiC 20 wt% TiC- 80 wt% SS316 powder
coating property. The MC technique has the advantage of obtaining 100 % SS316 100 wt% SS316 powder
thick coatings in short milling durations at room temperature and
ambient atmosphere without the need for special time-consuming and
expensive surface preparation before deposition [8] even when used to by powder metallurgy method has been reported. In that method the
obtain coatings of material such as intermetallics, nitrates, and amor­ composition was not uniform, the particles were not well distributed and
phous materials. The reinforcement particles establish the properties of there was no control on the grain size. Moreover, the reinforcements in
the particulate-reinforced MMCs by their size, type, nature, volume the composites prepared by the powder metallurgy method were ther­
(weight) percent, and shape [14,15]. Using small-sized reinforcement modynamically unstable at the metal matrix interface [5,29]. Shaojiang
particles results in uniform distribution and high thermal stability [16]. [30] used microwave and conventional sintering and investigated the
For structural applications usually low volume fraction of reinforcement wear resistance of SS 316L-TiC (2, 5, 10, and 15 %) composites. They
(5%–30 %) and when resistance to hardness and wear is needed usually concluded that the composites containing lower amounts of TiC had the
a high-volume fraction (50–80 %) is used [16]. Furthermore, among the best densification and tribological properties [20]. Furthermore,
different metal matrix composite coatings the ones reinforced by Szewczyk [20] showed that with the increase in the TiC amount the
ceramic particles such as TiC, WC, NbC, and Al2O3 particles typically corrosion rate decreased in the TiC-stainless steel composites. Several
with 10–40 vol% [17–19] have gained a lot of interest due to their in-situ processing routes for the formation of TiC coatings on steels such
capability for use in tribological and corrosive applications and their as casting and microwave sintering have also been reported [31] but to
stability and high strength to density [20,21]. Moreover, the strength of our knowledge, the ex-situ synthesis of SS 316-TiC nanocomposite
the alloys is increased by the ceramic particle dispersion due to the coatings on SS 316 substrate by MC technique has not been reported
decrease in the dislocation movements within the alloy matrix which elsewhere.
makes them suitable for applications in the automotive, aerospace, and In this research, a process for depositing nanocomposites of SS 316-
biomedical industries. Between the different carbides and different TiC on SS316 substrates by mechanical coating technique using abun­
reinforcement particles; TiC has proved its suitability with Fe or dant and cheap raw material to protect the surfaces of steel parts that are
Fe-based alloys due to its chemical stability and inertness with Fe-based under severe corrosion and wear conditions has been applied. The
matrices [13,22], extremely high hardness (2859–3200 H V) at both coating is sacrificed keeping the steel substrate in a good condition and
room and elevated temperatures [23], high oxidation and corrosion increasing the lifetime of the workpiece.
resistance, low density (~4.93 g/cm3), high melting temperature The main goal of the present research is to produce uniform hard TiC,
(~3430 K), high elastic modulus (~440 GPa), desirable electrical and SS 316, and SS 316-x TiC (x = 20, 50, and 80) nanocomposite coatings
thermal conductivity [24], and good wetting [25] which makes it a on SS 316 substrate by MC technique. In addition, the effect of the
suitable coating material on steels [26,27]. Degan and Shipway [28] amount of TiC on the wear properties and its effect on the corrosion
showed that TiC reduces metal-metal contact during sliding and has a property has also been investigated. The microstructure, composition,
high load-bearing capacity which improves the wear performance of coating thickness, and microhardness were measured. The coating for­
TiC-containing metal matrix composites. mation mechanism and wear mechanism of the deposited coatings were
Furthermore, the addition of TiC powder to Fe and Fe alloy powders also elucidated.

Fig. 1. SEM image of the: (a) initial TiC and (b) initial SS 316 powders.

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H. Hamedi and T. Isfahani Results in Engineering 24 (2024) 102966

20, 50, 80, and 100 are used as the coating material (Table 2).
SS 316 plates with 3 mm thickness and 50 ± 0.05 mm diameter were
used as the substrate. Before the coating process, the SS 316 plates were
ground using abrasive SiC paper washed with alcohol and water,
cleaned ultrasonically, and dried. To carry out the coating process the
substrate was located on the upper end of the steel milling vial. A
schematic illustration of the coating setup is shown in Fig. 2. A planetary
ball mill with the optimized milling parameters of: ball to powder
weight ratio (BPR) of 20:1, and a rotation speed of 300 revolutions per
minute (rpm) for 1, 2, 5, 10, and 15 h was used for the coating process.
The coating procedure was done using 48 bearing steel balls of 8 mm
and 48 bearing steel balls of 10 mm diameter. XRD analysis and whole
pattern Rietveld refinement using Topas software were applied to
investigate the crystallite size and phase composition of the constituents
of the coatings using a Philips machine model PW 1730 with a λkαCu =
1.54060. Optical microscope and a VEGA II TESCAN SEM were used to
investigate the cross-section, morphology, layer thickness, and micro­
structure of the coatings. For this reason, the sample was cold-mounted
and cut using a micro cutter, and the thickness of the coating was ob­
tained from the cross sections using an optical microscope, and its
thickness was determined by CLEMEX software [32]. The presented
amounts are mean amounts of 15 measurements obtained from 5 images
taken from different sections of the coating. A microhardness test was
applied on the cross sections using a load of 100 g and a dwell time of 25
s using a micro-Vickers hardness tester. The mean value of ten mea­
surements was reported. ASTM G99 was used to perform the dry
pin-on-disk wear tests at ambient temperature. A normal load of 50 N
and a rotation speed of 0.07 m s− 1 with a radius of 11 mm for 700 m
sliding was used. An AISI 52100 hardened steel pin with a hardness of 55
HRC was used. Each specimen was weighed before and after the wear
test with a precision of 0.1 mg. The specific wear rates (WR in m2/N) of
the coating and the correlation between the hardness and the wear rates
(Archard’s law) are obtained by equations (1) and (2) as shown below:

WR=Vwear/L. N (1)

WR=K L.N/H (2)

Whereas the Vwear, L, N, K, and H are the total volume of the produced
wear debris (mm3), total sliding distance (m), total normal applied load
(N), wear coefficient (m3/Nm or mm3/Nm)), and the hardness (HV),
respectively.
The corrosion response of the coatings was evaluated using an Ori­
gaLys potentiostat machine by obtaining the Tafel polarization curves.
The potentiodynamic polarization studies were done by immersing the
coated samples in a 3.5 % NaCl solution.

3. Results and discussion

3.1. Visual and microscopic observations

Visual inspection of the mechanically coated samples showed that a

uniform coating was successfully obtained for all of the mechanically
coated samples. For further investigation, the quality of the coatings was
observed using an optical and SEM microscope by investigating the
surface and cross sections of the coatings (Fig. 3). Although visual in­
spection showed that a uniform coating is obtained by the mechanical
coating process the SEM investigations on the cross-section of the coated
Fig. 2. A schematic illustration of the coating setup. samples showed that with the increase of the TiC; the deposited particles
are not adequately dense and compact and a suitable adhesive coating is
2. Experimental procedure not obtained. The effect of the composition and also the coating duration
on the mean coating thickness of the produced coatings was obtained
The chemical composition of the TiC (US Research Nanomaterials, using optical and SEM images of the cross-sections of the samples as
Inc.) and SS 316 (Atlantic Equipment Engineers) powders used as the presented in Fig. 4. The mean coating thickness of the 1-h mechanically
coating material is presented in Table 1. In Fig. 1 the morphology and coated samples showed that the 100 % TiC (4.2 μm) and 100 % SS 316
size of the initial TiC and SS 316 powders can be seen from the SEM samples (8.1 μm) had smaller coating thickness compared to the com­
images. Powder mixtures of TiC and SS 316 with weight percentages of posite coatings. It should be mentioned that for all the mechanical

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H. Hamedi and T. Isfahani Results in Engineering 24 (2024) 102966

Fig. 3. (a) The image of the top surface of the 20 % TiC sample, (b) the optical microscope image of the cross-section of the 5-h mechanically coated 20%TiC sample,
and the SEM images of the cross-sections of the: (c) 80 % TiC and (d) 100 % TiC coatings obtained after 5-h milling and (e) 2-h mechanically coated 100 % TiC, and
(f) 2-h mechanically coated 20 % TiC sample.

coating durations the 100 % TiC coating has the least mean coating
thickness among all samples while the 100 % SS316 and 20 % TiC coated
samples have the largest mean coating thickness after 15 h of mechan­
ical coating to be 36.4 and 38.1 μm, respectively. Also, it can be seen that
after 5 h of mechanical coating, the mean coating thickness for all
samples is around 20 μm except for the 100 % TiC sample which is
around 13.9 μm. Furthermore, it is obvious that for all the samples up to
10 h of mechanical coating with the increase in the coating duration, the
mean coating thickness increases. It was also shown that with further
milling of the 100 % TiC, 80 % TiC, and 50 % TiC samples a slight in­
crease is still obtained while for the 100 % SS 316 and 20 % TiC samples
the coating thickness increases with a higher rate. Fig. 3 (a) shows the
image of the top surface and Fig. 3(b) shows the optical microscope
image of the cross-section indicating the mean coating thickness of the
samples cut along the z-direction of the 20 % TiC sample obtained from
the 5-h milling sample to be around 21.3 μm. According to Fig. 3(a), it
can be seen that a uniform coating is obtained and from the visual in­
spection it can be seen that all samples obtained using the optimized
milling procedure have a uniform coating on the top surface. According
to the mean amounts (average of 15 measurements) presented in Fig. 4
obtained from the different samples deposited at different milling times,
Fig. 4. The mean layer thickness of the different samples deposited by coating it was seen that for the composite samples with the increase in the
durations of 1, 2, 5, 10, and 15 h.
amount of the SS 316, the thickness increased while the 100%TiC
coating had the least coating thickness. The lower mean coating thick­
ness of the 100 % TiC coating was probably due to the absence of the SS

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H. Hamedi and T. Isfahani Results in Engineering 24 (2024) 102966

during the coating procedure. Furthermore, it should be mentioned with

milling times higher than 5 h cracks are formed in all of the deposited
samples due to the impact of the balls on the substrate and coating. The
cracks and pores are not observable in any of the samples at lower
milling times shown in Fig. 3(e) and (f) for the 2-h milled 100%TiC and
20 % TiC samples, respectively.

3.2. Effect of milling time on the crystallite size and particle size

X-ray diffraction and the whole pattern Rietveld analysis [33–36]

were applied on all samples to determine the crystallite size of the
constituents of the different deposited coatings obtained for milling
durations of 1, 2, 5, 10, and 15 h. In Fig. 5 the whole pattern Rietveld
refinement applied on the X-ray diffraction pattern of the SS 316-20 wt%
TiC sample is presented. Furthermore, the crystallite size of all the
samples obtained from the X-ray diffraction patterns using Rietveld
refinement is presented in Table 3. As can be seen from Fig. 5 the peaks
present in the XRD pattern are very broad and low in intensity which is
due to the milling process. The internal structure of the particles un­
Fig. 5. X-ray diffraction and Rietveld refinement of the SS316-20%TiC coated dergoes continuous refinement and severe plastic deformation during
composite sample. the milling. The kinetic energy of the high-density steel balls used in the
milling procedure results in the crushing of the powders and the
316 particles. In contrast to the TiC particles the SS 316 particles have reduction of the crystallite size. This reduction is a result of the forma­
the same composition as the substrate and are ductile with an adhesive tion of large amounts of dislocations resulting in regions in the grains
nature therefore they can be easily deposited on the SS 316 substrate. In with large densities of dislocations [37]. Moreover, it is well-known that
the composite samples, the SS 316 powders gather around the TiC the lower crystallite size obtained during severe plastic deformation is
powders and mechanically bond and cold weld to the substrate resulting due to an increase in the dislocation density. With the increase in
in a higher increase in the coating thickness while for the 100 % TiC dislocation density low-angle boundaries are formed by rearrangement
sample, there is no SS 316 powder to help in the attachment and forming smaller diffraction domains [37–39]. Additional milling of the
adhesion of the powder to the substrate and the formed coating is ob­ sample results in small grains and distributes them in the entire sample
tained with weak mechanical bonding. In other words, as the weight and therefore the mean crystallite size is reduced.
percent of the SS316 powder decreases the weight percent of the TiC The crystallite size of the initial TiC and SS 316 powders are 112.1
powder increases and less adhesion and coating thickness is obtained. In and 127.5 nm, respectively. Comparing the crystallite size of the coat­
other words, when the SS 316 powder is present, cold welding is an ings obtained after 1-h milling shows that the TiC crystallite size of the
important reason for obtaining an adhesive coating. The sample thick­ 100 % TiC coating is the least among all the samples having an amount
ness of the 100 % SS 316 sample (4.2 μm) is lower than the 50 % TiC of 57.4 nm while the largest mean crystallite size is for the 100 % SS 316
(9.5 μm) and 20 % TiC (13.9 μm) coating after 1-h coating procedure due particles to be around 101.9 nm. The mean crystallite size of the %100
to the smaller particle size of the SS 316 particles compared to the TiC TiC sample reduces over time and reaches 23.8 nm after 15 h mechanical
particles. With the increase in the milling time the amount of the coated coating. Furthermore, it is obvious that for the composite samples with
SS 316 powder on the substrate increases while for the TiC particles due the increase in the amount of SS 316, the TiC crystallite size slightly
to its non-adhesive and brittle nature, the coating thickness increases reduces and reaches around 29 nm for the 50 % TiC and 80 % TiC
slightly even at long mechanical coating times this is due to the reason samples after 15 h of milling. The crystallite size of the SS 316 powder in
that during the mechanical coating process, some of the TiC particles the different samples is also presented in Table 3. According to the re­
attach to the coating while some particles detach from the coating due to sults, the crystallite size of the SS 316 in the 100 % SS 316 coating has
the ball impact. Fig. 3(c) and (d) show the 5-h mechanical coating layer the largest crystallite size of around 101.9 nm after 1-h mechanical
of the 80 % TiC sample and 100 % TiC sample, respectively. The sam­ coating. As can be seen, the milling decreases the crystallite size of the SS
ple’s mean thicknesses are measured to be 18.6 and 13.9 μm for the 80 % 316 particles in all cases. Although for milling times higher than 10 h the
TiC and 100 % TiC samples, respectively. The coating of the 100 % TiC crystallite size changes slightly or reaches a constant value which is a
sample is not uniform and along with several cracks, pores, etc. The result of the severe plastic deformation. It has also been shown by others
incomplete powder compaction of the 100 % TiC and TiC-rich (80 % TiC that the mean strain increases and crystallite size decreases with the
and 50 % TiC) coatings is the reason for the presence of micropores, increase of the milling time. In other words, the particle’s severe plastic
cracks, and pores from the coating/substrate interface which is due to deformation obtained during the milling procedure increases the lattice
the inadequate bonding of the brittle, hard and angular TiC particles strain [39], dislocation, and vacancy defects. The increased lattice
strain, defects, and the formation of low-angle grain boundaries by the

Table 3
Crystallite size (nm) of the TiC and SS 316 particles in the different coated samples.
Time 0 1h 2h 5h 10 h 15 h

TiC SS 316 TiC SS 316 TiC SS 316 TiC SS 316 TiC SS 316 TiC SS 316

Initial powders 112.1 127.5 – – – – – – – – – –

100 % TiC ​ ​ 57.4 ​ 24.8 ​ 23.9 ​ 22.1 ​ 23.8 ​
80 % TiC ​ ​ 71.2 85.4 34.4 44.7 28.7 39.4 28.1 27.8 27.9 26.1
50 % TiC ​ ​ 89.9 99.7 47.1 62.3 36.2 49.9 29.1 38.8 29.1 33.4
20 % TiC ​ ​ 97.4 101 78.7 78.2 61.5 56.6 42.4 44.2 39.2 42.7
100 % SS 316 ​ ​ – 101.9 – 84.2 – 60.7 – 47.7 – 46.5

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H. Hamedi and T. Isfahani Results in Engineering 24 (2024) 102966

Fig. 6. The crystallite size versus milling time for: (a) TiC and (b) SS 316 phases present in the TiC, SS 316, and SS 316-TiC coatings.

Fig. 7. SEM images of: (a) initial TiC powder, (b)milled TiC powders, (c) initial SS 316 powder, (d) milled SS 316 powder and (e) milled 20 % TiC powder for 5 h.

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H. Hamedi and T. Isfahani Results in Engineering 24 (2024) 102966

Fig. 8. The scheme of the mechanical milling process occurring during the milling of the initial SS 316 (path I), initial TiC (path II), and SS 316-TiC composite
particles (path III).

rearrangement of dislocation result in decreased crystallite size and alloy components. In Fig. 6(a) and (b), the TiC and SS316 crystallite sizes
smaller diffraction domains [37,40,41]. Moreover, with the increase in are plotted versus milling time, respectively. It can be revealed from
the milling time, the high collision energy from the milling balls applied Fig. 6 that the crystallite sizes decrease rapidly in the initial milling
to the powders increases which decreases the crystallite size and in­ stages (up to 5 h) and with further milling the mean crystallite size
creases the lattice microstrain. However, the fracture of the powders decreases at a smaller rate where the mean crystallite size reaches a
results in the release of the microstrain. This therefore results in a slow minimum and after 10 h of milling the crystallite size nearly reaches a
increase in the lattice microstrain. Also, in the case of cold welding constant value. Furthermore, it could be mentioned that the crystallite
which is a result of the increase of the surface energy of the powders size decreases with the increase in the amount of TiC in the composite
causing grain coarsening the average crystallite size decreases. More­ samples at a more rapid rate which is a result of the brittle nature of the
over, the work hardening of the powders also results in the decrease of TiC particles induced in the SS 316 matrix.
average crystallite size. Therefore, when a balance between the rate of Fig. 7 shows the morphology of the initial SS 316, initial TiC, 100 %
fracture and cold welding is reached there is no significant change in the TiC, 100 % SS 316, and the 20 % TiC powders milled for 5 h. As can be
average crystallite size and lattice microstrain [42]. seen, the mean particle size decreases, and size distribution increases
In this research, although the reduction rate is different for the with the milling of the initial powders. At the early stages of the milling
different samples the decrease in the crystallite size is obvious with procedure interatomic bonds in the crystal rupture and new surfaces
increasing the milling time for both the brittle TiC and ductile SS 316 form as a result of the cleavage of crystalline grains until reaching a

Fig. 9. SEM image of (a) the %20 TiC coating on the SS316 substrate and (b) the uncoated 20 % TiC powder remaining from the mechanical coating procedure.

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H. Hamedi and T. Isfahani Results in Engineering 24 (2024) 102966

critical milling time [43,44]. When the size reaches a critical size, the
agglomerates are formed due to the increase in the surface energy which
is a result of the increase in the particle’s surface-to-volume ratio.
Therefore, the particles are saturated after a critical particle size which is
due to the reason that the particle size reduction as a result of the impact
energy of the balls and the increase of the milling time competes with
the reduction of the surface energy by the formation of agglomerates. It
has been shown by previously published research that a layered struc­
ture (lamellar) is obtained for the ductile particles at the initial stage of
the milling procedure due to the contiguous cold welding of the layers.
Additional milling results in particle size reduction and this is due to the
reason that continuous cold welding causes brittleness forming
granular-shaped particles. The continuous cold welding-fracture process
generates agglomerates of nanosized TiC and SS316 powder. When the
deformation is the predominant mechanism a broader particle size dis­
tribution is obtained while the welding mechanism increases the
equivalent diameter of the ductile SS316 matrix particles. The presence
of TiC reinforcement particles changes the mechanical milling classifi­
cation to a ductile-brittle component system.
In Fig. 8 a probable scheme of the milling system is presented. In path
I; elongated flat particles along with small-sized particles are obtained at Fig. 10. The Vickers hardness of the different coated samples.
the initial milling stage due to the deformation of the ductile SS 316
particles and cold working. Path II shows that the brittle TiC particles go
3.3. Microhardness
through fragmentation resulting in smaller-sized particles. For the 20 %
TiC powder (path III) it could be seen that during the ball collisions, the
Microhardness test was applied to obtain the hardness of the coat­
cold welding of the ductile SS 316 particles occurs and the brittle par­
ings. The mean value of 5 tests is presented in Fig. 10. As can be seen, the
ticles are located between the ductile particles. Therefore, the fractured
100 % TiC coating had the highest hardness (405 HVC) value while the
and refined reinforcement particles are located at the interfacial
SS 316 substrate (218 HVC) and 100 % SS 316 (248 HVC) coated sam­
boundaries of the cold-welded ductile SS 316 particles forming a com­
ples had the lowest hardness values. The higher hardness value of the
posite with uniform particle distribution. Fathy et al. also showed a
100 % SS 316 coating compared to the SS 316 substrate was due to the
similar behavior on their study on Al-Al2O3 nanocomposite powders
deposition of the nanocrystalline SS 316 coating. As shown in Fig. 10
[45]. The morphology of the particles is changed when cold welding is
with the increase in the amount of TiC the hardness slightly increased
the dominant mechanism and laminar pilled-up particles are formed.
from 248 for the 100 % SS 316 coated sample to around 270 for the 20 %
The particles harden and an increased fracture process occurs resulting
TiC and 50 % TiC samples. Further increase in the amount of TiC pro­
in equiaxed morphology due to the deformation, cold welding, and solid
vided a high increase in the hardness value to 336 HVC for the 80 % TiC
particle dispersion. Interfacial boundaries of random orientation result
sample which is due to the high amount of hard TiC ceramic nano­
in a real composite which is due to the steady state equilibrium
particles compared to the SS ductile particles. This increase indicates
welding-fracture process. In this case, optical microscopy cannot reveal
that for the 80 % TiC sample even though the metallic SS 316 component
the interfacial boundaries due to the severe refinement of the particles.
is not sufficient to obtain a continuous matrix and to embed the TiC
In Fig. 9 it can be observed from the SEM images of the coated and
particles the TiC particles have quite good adhesion and a low amount of
the uncoated powder left from the mechanical coating procedure that
porosity and cracks are present in the coating. In the reports presented
there is a big difference between the powder size of the TiC and SS 316
by Yazdani et al. [13,48] the increase in the SiC ceramic particles
constituents present in the coating and the residual uncoated powder. As
resulted in low microhardness due to the high degree of porosity and
shown in Fig. 9 for the 20 % TiC coated sample there is an SS 316 matrix
cracks present in the coating.
with embedded nano TiC particles uniformly distributed throughout the
matrix. The TiC particles have a size in the range of 50–85 nm.
Furthermore, for the uncoated powder, it is obvious that the size dis­ 3.4. Wear properties
tribution is very wide with small particles and large agglomerates. This
indicates that the substrate has a large role in the particle size reduction The mean coefficient of friction vs. distance curve for the 20 % TiC
due to the ball-powder-substrate collision of the coated powders which and 50 % TiC nanocomposite coating is presented in Fig. 11 and the
results in the continuous cold welding and fracture phenomena [46,47]. mean coefficient of friction and wear rate values for all the samples are
This larger particle size distribution of the uncoated 20 % TiC presented in Table 4.
powder remaining from the mechanical coating procedure is due to the As can be seen, the mean coefficient of friction for the 20 % TiC
presence of the ductile SS 316 particles in the powder mixture which coating is lower than the other samples and its lower value compared to
receives large portions of the energy of the ball-powder-ball and ball- the 100 % SS 316 coating is probably due to the uniform dispersion of
powder-wall collisions and deforms and flattens due to its ductile na­ the nanosized TiC particles inside the SS 316 matrix providing a wear-
ture. Furthermore, the milling of the SS316 and TiC composite powder resistant coating. The SS 316 matrix is ductile with a higher adhesive
mixture, results in the formation of agglomerates where the TiC particles nature compared to the ceramic TiC particles and can tightly keep the
are attached to the SS 316 powders due to the ductile nature of the SS particles together when present at low fractions. The higher mean co­
316 particles. The SS 316 powders are ductile and more easily cold weld efficient of friction value for the composites with higher amounts of TiC
to the substrate with good adhesion while the TiC particles have less particles (50 % and 80 %) could be due to the presence of larger abrasive
adhesion and cold weldability to the substrate due to the brittle nature of brittle TiC particles present in the exterior layer of the coating. The TiC
the TiC powders. particles have lower cohesion strength as expected from a ceramic
compared to metals and alloys when coated on a metallic substrate.
Furthermore, the lower amount of ductile SS 316 particles in the 50 %
TiC and 80 % TiC coatings compared to the 20 % TiC coating results in

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H. Hamedi and T. Isfahani Results in Engineering 24 (2024) 102966

Fig. 11. Mean coefficient of friction versus distance for (a) the 20 % TiC coating and (b) the 50 % TiC coating.

lower adhesion of the coating and looser TiC particles in the coatings.
Table 4 Therefore, the TiC particles may detach and act as a third abrasive body
The mean coefficient of friction and wear rate of the different coated samples also resulting in a high friction coefficient. The wear rates of the samples
after 700 m.
are also presented in Table 4.
According to Tables 4 and it can be seen that the 20%TiC composite
6
Sample Wear rate ×10− at 700m distance Mean coefficient of
code (mm3/Nm) friction sample has less wear rate compared to the other samples. Comparing the
100%TiC 13.6 0.7 wear rate and the hardness results shows that the inverse relationship
80%TiC 12.1 0.76 between them according to Archard’s law is not reached [49]. This is
50%TiC 0.72 0.6
due to the reason that the wear rate does not only depend on hardness
20%TiC 0.36 0.3
100 % St.St 19 0.52 but on several parameters such as the morphology, adhesion, cohesion,
toughness, roughness, hardness of the coating, and worn surface and

Fig. 12. Schematic of the coatings before and after the wear test: a) 100 % SS 316, b) 100 % TiC, c) SS 316 rich composite coating (20 % TiC), and d) TiC rich
composite coating (50 and 80 % TiC).

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H. Hamedi and T. Isfahani Results in Engineering 24 (2024) 102966

Fig. 13. SEM image of the wear surface of samples: (a) 100 % TiC, (b) 80 % TiC, (c) 50 % TiC, (d) 20 % TiC, and (e) 100 % SS 316 after 700 m.

also the difference between the hardness of the substrate and coating. and 12 (c)) the presence of adhesive SS 316 coating results in sufficient
The schematic of the wear surface of the composite coatings is shown in particle compaction and fewer defects such as cracks, etc. which could
Fig. 12. As shown (Fig. 12 (b) and 12 (d)) the 100 % TiC sample and also be due to the similar composition of the coating and substrate. The
samples with higher percent of TiC particles have larger TiC particles in SEM images of the worn surfaces of the coatings after the 700m wear test
the coating along with pores, cracks, etc. which is probably due to the are shown in Fig. 13(a–e). In Fig. 13(a) the wear surface of the 100 % TiC
insufficient particle compaction and non-uniform coating. Therefore, sample shows fragmentation and detachment of TiC particles this in­
the TiC particles are loose and can easily be detached and removed dicates that some of the particles do not have enough adhesion to the
during the wear test. For the SS 316 and SS 316 rich coating (Fig. 12 (a) substrate causing cracks and abrasive third body particles. Fig. 13(b)

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H. Hamedi and T. Isfahani Results in Engineering 24 (2024) 102966

Fig. 14. The (a) Tafel polarization curve of the coatings and (b) corrosion current density (icorr) and corrosion rate for the different samples.

abrasive grooves are less shallow but several cracks and third body TiC
Table 5
particles are still present. Fig. 13(d) shows the worn surface of the 20 %
The result of the Tafel polarization corrosion test applied to the coated samples.
TiC sample which has the highest wear resistance compared to all the
Sample code E (i = 0) icorr (μA/ βa βc (mV) Corrosion (μm/ samples. The worn surface shows a smoother surface with a few shallow
(mV) cm2) (mV) Y)
abrasive grooves along with some small debris and worn particles. In
20%TiC − 476.1 0.3939 134.8 − 90.8 4.9358 Fig. 13(e) the worn surface of the 100 % SS 316 coated layer is presented
50%TiC 466.9 1.0855 200.0 389.2 15.871
− −
as can be seen it has some ductile elongated SS 316 debris and shallower
80%TiC − 474.4 0.9930 295.7 − 371.7 17.286
100 % SS − 377.4 0.4945 198.6 − 321.4 5.6386
abrasive grooves compared to the other samples along with areas
316 showing a peel-off mechanism (see Fig. 13).
100%TiC − 461.9 1.0029 177.9 − 377.0 11.436
4. Corrosion test

shows the worn surface of the 80%TiC sample. This sample shows a
In Fig. 14 (a) the Tafel polarization curve of the samples and in
completely different wear behavior. As can be seen besides TiC particle
Fig. 14 (b) the corrosion current density (icorr) and corrosion rate for the
detachment; the plastic flow of the ductile SS 316 phase along with
different samples are presented. The corrosion parameters extracted
several deep abrasive grooves are present. In Fig. 13(c) the worn surface
from the curves are shown in Table 5. It is well known that factors such
of the 50 % TiC sample is presented in this sample it is obvious that the

Fig. 15. SEM image of the (a) 20 % TiC, (b) 80 % TiC, and (c) 100 % TiC samples.

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H. Hamedi and T. Isfahani Results in Engineering 24 (2024) 102966

as the corrosive media and materials composition affect the corrosion coefficient of friction was the least for the 20 % TiC and 100 % SS 316
resistance of materials [50–52]. In this research, the 3.5 % NaCl solution samples which were around 0.3 and 0.52, respectively. Moreover, the
as a corrosive environment is the same for the different samples but as lowest wear rate was obtained for the 20 % TiC coated sample to be
can be seen, the corrosion resistance and corrosion current density of the around 0.36 × 10− 6 (mm3/Nm) which is 50 times more resistant than
coatings are different which is due to the different compositions of the the 100 % SS 316 sample. It can be concluded from the Tafel test that the
samples. As can be seen, the 20 wt% addition of TiC as reinforcement introduction of TiC as reinforcement improved the corrosion resistance
improves the corrosion resistance having the least amount of corrosion and exhibited the lowest value of current density and corrosion rate.
current density and corrosion rate to be 0.3939 μA/cm2 and 4.9358 However, the increase of TiC content from 20 to 50 and 80 wt% caused
μm/Y, respectively. Moreover, increasing the amount of TiC reinforce­ an increase in the current density and corrosion rate. Whereas the
ment to 50 and 80 wt% was not beneficial in increasing the corrosion corrosion rate of the 20 % TiC sample was 3.5 times less than the 80 %
resistance because it led to an increase in the corrosion current density TiC sample. This confirms that the 20 % TiC sample has the highest
to around 1 μA/cm2 and the corrosion rates of 15.871 and 17.286 μm/Y, corrosion resistance.
respectively. This result is in agreement with Wu et al. [53,54] which
studied the effect of TiC addition on the corrosion behavior of SS 304 Funding
and SS 2Cr13. They showed that the addition of TiC to these steels re­
sults in an increase of corrosion resistance at lower amounts of TiC and a The authors declare that no funds, grants, or other support were
decrease in the corrosion resistance at high amounts of TiC. In this received during the preparation of this manuscript.
research, the 20 % TiC composite sample obtained the lowest value of
corrosion current density and corrosion rate between all the samples.
CRediT authorship contribution statement
This means that this material has the highest corrosion resistance.
Furthermore, the 100 % SS316 coating compared to the 20 % TiC has
Hesamoddin Hamedi: Writing – original draft, Validation, Meth­
slightly higher amounts of corrosion current density and corrosion rate
odology, Formal analysis, Data curation. Taghi Isfahani: Writing – re­
probably due to the smaller grain size, the presence of porosity in the
view & editing, Writing – original draft, Visualization, Validation,
coating, and the plastic deformation and increase in the dislocation
Supervision, Software, Resources, Project administration, Methodology,
density of the coating and also the higher corrosion resistance of the
Investigation, Funding acquisition, Formal analysis, Data curation,
ceramic TiC reinforcements present in the 20 % TiC coating. The lower
Conceptualization.
corrosion resistance of the 100 % TiC coating compared to the 20 % TiC
and 100 % SS 316 samples is due to the porosity and pores present in the
coating [55–57].
The SEM images of the 20 % TiC, 80 % TiC, and 100 % TiC samples Declaration of competing interest
after the corrosion test are shown in Fig. 15. As can be seen compared to
the 80 % TiC and 100 % TiC samples the 20 % TiC coating has a uniform The authors declare that they have no known competing financial
coating and less evidence of corrosion is present. However, the 80 % TiC interests or personal relationships that could have appeared to influence
coating is severely corroded with several corrosion pits present in the the work reported in this paper.
SEM image. Furthermore, the 100 % TiC sample is uniform with some
pores and cracks (shown by arrows) present from the coating before the Data availability
corrosion test. These pores and cracks result in the penetration of the 3.5
% NaCl solution to the substrate which increases the corrosion rate. Data will be made available on request.

5. Conclusions References

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