TECHNICAL PAPER

Wear Behavior of Plasma Sprayed Nanostructured Al–SiCp

Composite Coatings: A Comparative Study

Satish Tailor1 • R. M. Mohanty2 • P. R. Soni3 • A. V. Doub1

Received: 3 June 2015 / Accepted: 20 August 2015

� The Indian Institute of Metals - IIM 2016

Abstract Powders of AlSi, 2024Al and 6061Al were

separately ball milled with 15 wt% SiC reinforcement in a

high-energy attrition ball mill using stainless steel balls for

8 h. The ball milled powders were plasma sprayed on the

weathering steel (Cor-Ten) substrates to get Al–SiC com-

posite coating with as much high volume fraction as pos-

sible of SiC. The microstructure characteristics of coatings

were examined by SEM, XRD and image analyzer. XRD

studies showed SiCp embedment in the Al matrix after ball

milling, and nano grains in the ball milled powder and

coatings. The thickness of coating and hardness were

measured. The high adhesion-strength of the coatings

observed might be attributed to higher degree of diffusion

at the interface. The wear behaviors of the coatings were

carried out under pin-on-disc wear test machine for 50 N

load. Results showed that hardness and wear resistance of

coatings depended on SiCp fraction and crystallite size in

the matrix. The results of mechanical and wear tests also

indicated that high-energy attrition ball milling and addi-

tion of SiC particles increased the strength, hardness and

wear resistance of the coatings.

Keywords High-energy attrition ball milling �2024Al, 6061Al, AlSi alloys �Plasma spray coatings, adhesion, wear

1 Introduction

SiCp reinforced ‘‘aluminum based metal matrix composite’’

(Al-MMCs) are widely used in aerospace, transport, and

electronic industries because they provide excellent

specific properties such as low density (2.95–3.00 g/cm3),

high bending strength (350–500 MPa), high stiffness, good

wear resistance, low thermal expansion coefficient (tailor-

made from 6.5 to 9.5 E-6 K-1), high elastic modulus

(200–300 GPa), high damping capacity and excellent high

temperature properties which are the key factors of

industrial interest [1–4]. The high wear resistance is cred-

ited to the presence of the hard silicon particles distributed

throughout the matrix [3, 5]. Plasma sprayed Al-MMCs

coatings are regularly used for wear resistance, thermal

barrier applications, aerospace, defence and selected

automotive applications such as high performance racing

applications [3, 4]. Due to the low density of aluminum,

2024Al and 6061Al (as a matrix) have long been used in

synthesis of Al-MMCs [6, 7]. But the major drawback of

Al-alloys is its low wear resistance. Numerous attempts

have been made to overcome this draw back. The ceramic

particles as a reinforcement phase in Al-MMCs is the most

commonly used form due to their easier production process

and with isotropic properties in the composite [8, 9]. So

ceramic reinforced Al-MMCs have collected significant

attention due to the integration of their tribological prop-

erties without dropping the corrosion properties of Al-al-

loys [10, 11]. Al2O3 [12], TiN [13], B4C [14], SiC [15],

MgO [16], MoSi2 [17] etc. are the most commonly used

& Satish Tailor

dr.saty@yahoo.in

1 National University of Science and Technology ‘‘MISiS’’,

Leninsky Prospect-4, Moscow 119049, Russia

2 Council of Scientific and Industrial Research, CSIR-HQS,

Rafi Marg, New Delhi 110001, India

3 Department of Metallurgical and Materials Engineering,

Malaviya National Institute of Technology, Jaipur 302017,

India

123

Trans Indian Inst Met

DOI 10.1007/s12666-015-0692-8

ceramic particles used in the production of Al-MMCs.

These particles can be used in nano and micron scales. But

some specific properties of SiC (i.e. high melting point

(2730 �C), high modulus (250 GPa), good thermal stabil-

ity, good hardness, high wear and impact resistance, high

chemical resistance and high density—3.21 g/cm3) makes

it an appropriate reinforcing material for producing Al-

MMCs. By decreasing the size of ceramic particulates and/

or matrix grains to the nanometer level using high-energy

attrition ball milling technique, the mechanical properties

such as adhesion strength, hardness and wear resistance of

Al-MMCs can be further enhanced [15, 18–20]. Some

researchers have reported that, ductility of nanocomposites

is better than that of microcomposites [21–23]. This par-

ticular finding makes it important for structural

applications.

As a method for uniform dispersion of reinforcing par-

ticles in the matrix, ball milling is well recognized [24–27].

The Al-MMC powders prepared by high-energy attrition

ball milling can be deposited on the surfaces of engineering

parts using thermal spraying techniques. Low porosity,

high hardness and good bonding to the substrate are attri-

butes of the coatings developed by this method. In com-

parison to available all thermal spray methods, plasma

spray technique is capable of producing coatings with low

porosity and superior tribological properties [24, 26–28].

The strength of the interface between matrix and rein-

forcement particles decide the wear behavior of Al-MMCs

[15]. Weak interface strength between the matrix and

reinforcement material leads to high wear rate [29]. The

effect of reinforcing particles on wear behavior of a com-

posite depends on powder preparation method. In the

composites synthesized by ball milling, reinforced particles

are well distributed and produce very fine particles, thus

improving the wear resistance [30].

The effect of reinforced particles and different grain size

of alloys on wear properties have been studied by several

researchers. They have reported that finer grains lead to

increased hardness and reduced wear rate [31–36]. Wang

SG, Liu Y et al. [37] observed that wear rate is higher in

nanoparticles compared to coarse grained iron and they

have attributed this decrease in wear resistance to a sharp

decrease of flexibility in a nanostructured sample. The

effect of ball milled processed feedstock powder on ther-

mal spray coatings is not well established. Yet several

studies have been done on composite coatings with micro-

sized hard particles [38–40]. However, limited studies have

been reported on wear and mechanical properties of the

SiCp reinforced 2024Al MMCs. Reason may be the high

strength and low compressibility of this alloy [41].

In the present work, ball milled AlSi–SiC, 2024Al–SiC

and 6061Al–SiC coatings are deposited on weathering steel

(WS; which is also known as Cor-Ten steel) substrate using

the air plasma spraying (APS) technique. Properties of

plasma sprayed coatings like microstructure, crystallite

size, deposition efficiency, porosity and hardness have been

studied. Adhesion strength and wear properties of AlSi–

SiC coatings have also been evaluated. An attempt has

been made to optimize the plasma spray conditions, based

on the current density and spray distance to get better wear

properties.

2 Experimental

2.1 Materials Used

Al–13Si powder was supplied by The Metal Powder

Company Limited Thirumangalam, Madurai, India with an

average particle size of 199.65 lm. 2024Al and 6061Al

alloys powders, supplied by the EKCA Granulate Veldem

GmbH, Germany with an average particle size of 31.63 and

43.43 lm, respectively were used as matrix material. The

reinforcement SiC powder was also supplied by The Metal

Powder Company Limited Thirumangalam, Madurai, India

with an average particle size of\40 lm. Scanning electron

micrographs of as-received materials are shown in Fig. 1.

2.2 Feedstock Powder Preparation and APS

Processing

The powder mixtures of aluminum with 15 wt% SiC

reinforcement, that is, Al–13Si–15SiC, 2024Al–15SiC and

6061Al–15SiC powder, were ball milled and used as

plasma spray feedstock. The powders were mechanically

alloyed in an indigenous high-energy attrition ball mill, in

purified nitrogen (99.99 %) atmosphere for 8 h. The mil-

ling media consisted of 12.2 mm sized hardened steel balls.

Ball to powder weight ratio and rotational speed were 10:1

and 350 rpm, respectively. The composite powder mixture

was processed in a batch size of 100 g along with 1 wt %

Acrawax carbon (supplied by Lonza Inc., NJ.) as process

control agent (PCA). The ball milled powder was then

degassed for 1 h at 200 �C in a vacuum of 1 9 10-2 torr.

The ball milled processed composite powders were then

deposited on the grit-blasted weathering steel (Cor-Ten

A242) (Table 1) substrates using Sulzer Metco plasma

spray equipment NY 3 MB gun under the conditions as

presented in Table 2. The plasma coatings were developed

on the substrates with different spray distances and current

intensities for optimization as in (Tables 3, 4). The whole

concept of 2024Al–SiCp composite powder by ball milling

process and its spraying using APS is schematically shown

in Fig. 2.

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Fig. 1 SEM of as-received powder particles. a AlSi, b 2024Al, c 6061Al and d SiC

Table 1 Chemical composition of weathering steel substrate

Cor-ten Chemical contents/%

C Si Mn P S Cr Cu V Ni

A 0.12 0.25–0.75 0.20–0.50 0.07–0.15 0.030 0.50–1.25 0.25–0.55 – 0.65

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2.3 Characterizations

The phase composition of the as-received and as-milled

powders were analyzed with a Philips X’Pert-X-ray

diffractometer using Cu Ka radiation (k = 0.15406 nm).

The XRD patterns were recorded in the 2h range of 20�–100� (step size of 0.05� and time per step of 1 s). The

crystallite size of powder particles and coatings were

estimated using the Williamson–Hall method by analysing

the following equation [42]:

b cos h ¼ KkD

þ 2Affiffiffiffi

e2p

sin h ð1Þ

where h is the Bragg angle, k the radiation wave length, K

the Scherrer constant (0.9), D the crystallite size, e the

average internal strain, b the diffraction peak width at half

maximum intensity, and A is the coefficient (depending on

strain distribution; it is near to unity) [15].

The morphology of powder particles and as-sprayed

coatings were investigated using a scanning electron

microscope (TESCAN VEGA LSII, Brno, Czech). Particle

size analyses were carried out using laser particle size

analyzer (CILAS 1064, Marcoussis, France).

Microhardness measurement was performed (ten indenta-

tions for each value) using a Vickers microhardness tester

under a load of 4.9 N for 20 s. The porosity and SiCp

fractions in coatings (five measurements for each value)

were analysed using image analyser. The adhesion strength

of the coating was measured (ten indentations for each

value) by interfacial indentation tests [43] using Vickers

indenter under the loads of 0.98, 1.96, 2.94 and 3.92 N.

Surface roughness of the coatings were measured using

a Mitutoya Sj-301 profilometer. The average roughness,

Ra, was used to quantify the surface roughness of the

coatings. The wear behavior of the coatings were studied

under dry-sliding conditions using DUCOM pin-on-disk

type TR-20-M100 machine with the pin diameter of min-

imum 3 mm and 12 mm Maximum (Ducom Instruments-

Asia, Bangalore). Tests were conducted at 50 N applied

loads at a sliding speed of 1 m/s and a sliding distance of

2 km. The counterpart material was a cold work hardened

AISI D2 tool steel disk with a hardness of 730 VHN. Care

was taken to continuously clean the specimens during the

test with woolen cloth to avoid the entrapment of wear

debris to achieve uniformity in experiments. Scanning

electron microscopy was performed to analyze the mor-

phology of the worn surfaces. Sample weight loss due to

wear was measured using an electronic balance with a

resolution of 0.01 mg. The wear rate was calculated by

dividing the weight loss by the sliding distance. The wear

debris generated at the substrate was also collected to

ascertain the type of wear mechanism.

3 Results and Discussion

3.1 Characterization of Ball Milled Powder

Figure 3 shows the particle size distribution in ball milled

powders. It also shows the morphologies and distribution

of SiC particles in ball milled AlSi–SiC, 2024Al–SiC and

6061Al–SiC composite powders. During high-energy mil-

ling, the morphology of powder particles changes as a

result of repeated deformation, fracturing, and welding

processes [44]. It can be seen that SiCp particles are uni-

formly distributed and the initial AlSi–SiC and 2024Al–

SiC powders acquire irregular shape while 6061Al–SiC

powder take the shape of flakes. The SiC particles (smaller

as well as larger) distribution in the Al matrix powder can

be confirmed by back scattered mapping of SiCp using

EDX (corresponding micrographs in Fig. 3 shows the back

scattered mapping of SiC).

XRD patterns of powder particles as-received, blended

and after milling for 8 h are shown in Fig. 4. It can be seen

that after milling for 8 h the intensity of Al–Si, 2024Al and

6061Al alloys and SiC diffraction peaks decreases and

Table 2 Optimized plasma spray parameters

Parameters Values

Current, A 500

Voltage, V 50

1st gas, Ar, SCFH 70

2nd gas H2, SCFH 10

Carrier gas Ar, SCFH 20

Powder feed rate, RPM 20

Spray distance, mm 100

Table 3 Spraying at fixed current

Substrates WS

Condition code A1 A2 A3 A4

APS conditions

Spray distance (D) mm 50 100 150 200

Current (I) amp 500 500 500 500

Table 4 Spraying at fixed distance

Substrates WS

Condition code B1 B2 B3 B4

APS conditions

Spray distance (D) mm 100 100 100 100

Current (I) amp 200 300 400 500

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their width increases as a result of decrease of crystallite

size and increase of lattice strain. A decrease in peak

intensities may be attributed to embedment of SiCp in the

matrix after ball milling processing. With the decrease in

the amount of free SiC particles, the intensity of SiC peak

decreases (Fig. 5) indicating embedment of SiC particles in

the Al alloy matrix. A small displacement in diffraction

peaks can also be observed. Shifting of the 2h angle to a

high value indicates strain in the ball milled matrix powder.

The ball milling materials undergo extensive plastic

deformation before they get the shape and the strain

hardening coefficient can be assumed to be zero [44].

Moreover, the peak broadening of the main peak indicates

a reduction in grain size due to ball milling [44].

After 8 h of milling, the mean powder particle size of

AlSi–SiC, 2024Al–SiC and 6061Al–SiC become about 37,

14 and 31 lm respectively (Fig. 6). The milling is inter-

rupted at this stage because longer milling time lead to

finer powder particles that are unsuitable for spraying [3,

15]. A fine particle size causes several problems in APS,

including non-uniformity in the powder feed rate and a

decrease in powder flux, leading to increased porosity and

poor adhesion [3, 5, 15]. On the other hand with increase in

time of milling, the Al particles may begin to cold weld

which increases its size, resulting a decrease in the amount

of fines and formation of agglomerated or cold welded Al

particles. As the Al particles are cold welded, the SiC

particles are embedded within the MMC particles. Thus the

process of cold welding is dominant compared to the rate

of fracture. An increase in the particle size of the MMC

also causes several problems in APS and it is unsuitable for

spraying. Thus 8 h mechanical alloyed processed powders

are found to be suitable for spraying.

3.2 Characterization of the Coating

The microstructure and cross section of AlSi–SiC, 2024Al–

SiC and 6061Al–SiC composite coatings are shown in

Fig. 7. The coating thickness has been in the range of

250–300 microns in all three cases. Cross sections of the

coatings show that the interface is free of cracks and the

SiC particles are homogeneously dispersed and well inte-

grated inside the matrix. The SiC particles exhibit an uni-

form distribution in the matrix in all three cases. The SiCp

area fraction, porosity, microhardness and crystallite size

of sprayed coatings are listed in Table 5.

Fig. 2 Concept of powder production and air plasma spraying

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Fig. 3 SEM images of powder

morphology and distribution of

SiC particles in the ball milled

powders. a AlSi–SiC,

b 2024Al–SiC and c 6061Al–

SiC (corresponding micrograph

showing back scattered

mapping of SiC)

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123

The deposition efficiency of powder on substrates at

spray distance (D) of 100 mm is greater than other spray

distances in all three cases. So, 100 mm has been selected

as the optimum spray distances. It can also be noted that

these composite powders milled for 8 h gives good coating

deposition on substrates for spraying distance (D) of

100 mm and current (I) of 500 amp.

XRD patterns of APS coatings at optimum conditions

have been shown in Fig. 8. These XRD patterns show no

oxide peaks as well as no new phases. In the plasma spray

coatings, molten particles solidify with a very high rate

(approaching 107 K/s). Probably due to the high tempera-

ture and diffusion, the reaction between the phases present

can not take place, and consequently no new phase can

form.

The crystallite size of the coatings are calculated from

broadening of XRD peaks using the Williamson–Hall

method. The results shows that the crystallite size decrea-

ses to 15, 17 and 32 nm for ball milled AlSi–SiC, 2024Al–

SiC and 6061Al–SiC coatings respectively. This may be

attributed to the process of continuous fracturing and

welding of the Al-matrix powder particles during the high

energy milling and this process is facilitated by the pres-

ence of angular shaped hard particles of SiC [5, 15].

Microhardness for AlSi–SiC is higher than the coatings

of 2024Al–SiC and 6061Al–SiC, which can be credited to

higher volume fraction (30–50 %) of SiC particles. This

nano-grain size, high dislocation density because of ball

milling and dispersed oxides and carbides may be the

possible reasons for high hardness in the coatings [15]. The

measured porosity is surface connected open porosity. In

view of the homogeneous coating, it is presumed that it

will be same throughout the coating.

Surface roughness results obtained from coating mate-

rial are given in Table 5. Surface roughness is highest for

6061Al–SiC coatings. The amount and size of reinforce-

ment have no significant effect on surface roughness of

material.

3.3 Wear Behavior of As-Sprayed Coatings

Figure 9 shows the wear rates at loads of 50 N of the AlSi–

SiC, 2024Al–SiC and 6061Al–SiC composite coatings

applied on weathering steel substrate. The composite

coatings display a significant improvement in wear resis-

tance ([100 %) by the addition of SiC particles in the

matrix. Plasma sprayed ball milled AlSi–SiC composite

coatings shows the lowest wear rate, which can be attrib-

uted to homogenous distribution and slightly higher frac-

tion of SiC particles with hard Si particles in matrix, low

porosity level and a nanosized crystallite size.

Fig. 4 Effect of the ball milling on the powders. a AlSi–SiC,

b 2024Al–SiC and c 6061Al–SiC

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bFig. 5 XRD patterns of the powders. a AlSi–SiC, b 2024Al–SiC and

c 6061Al–SiC

Fig. 6 The particle size distribution in ball milled powders. a AlSi–

SiC, b 2024Al–SiC and c 6061Al–SiC

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123

Figure 10 shows the SEM of worn surfaces and corre-

sponding debris of the ball milled AlSi–SiC, 2024Al–SiC

and 6061Al–SiC composite coatings. A large numbers of

dimples have been formed on the surface with the grooves.

It appears that some SiC particles on the worn surface has a

micro cutting effect on the counter face and acts as a load

Fig. 7 The microstructure and

cross sections of coatings.

a AlSi–SiC, b Cross section of

AlSi–SiC, c 2024Al–SiC,

d Cross section of 2024Al–SiC,

e 6061Al–SiC and f Cross

section of 6061Al–SiC

Table 5 SiCp fraction, porosity, microhardness, crystallite size and surface roughness in the coatings at optimum spray condition

Material SiC fraction (%) Porosity (%) Microhardness (HV) Crystallite size (nm) Surface roughness (Ra 0.001 mm)

AlSi–SiC 30–50 1 351 15 9

2024Al–SiC 35–45 1–2 334 17 11.8

6061Al–SiC 35–45 2 232 32 12.2

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supporting element without serious fragmentation. It can be

seen in Fig. 10 that the debris is powder-like and reveals a

dark contrast in the image. The worn surfaces of the

specimen and the debris generated are found to contain

Al2O3 and Fe2O3 (Fig. 11). This shows a typical charac-

teristic of oxidative wear. Therefore, the oxidative wear is a

dominant wear mechanism in these composite coatings.

This is not consistent with the observations on some other

aluminum alloys [45–47] and aluminum based MMCs [48,

49]. It has been reported that iron oxides have a low

coefficient of friction [50], and therefore, lubricate the

worn surface and reduce the wear rate.

On the other hand, some platelets in the debris and dim-

ples on the worn surface can be observed. These platelets in

the debris must have been created due to subsurface crack

formation and propagation in the specimen (Fig. 12).

Nucleation may have occurred in subsurface cracks in the

form of microstructural defects or embracement in the

material. It gives rise to characteristic pitting fatigue that

results in generation of wear or debris particles. These par-

ticles are equiaxed, where the friction forces are enough to

damage the surface layer. This results in the loss of material

in the form of thin flakes. This type of wear is called

delamination wear. In such type of wear, subsurface plastic

shear plays an important role in generation and spreading of

cracks in the material structure. [51, 52]. The wear thickness

(typically few microns) depends on the position of cracks

generation. Therefore, the wear process of the composite

coating is delamination as well as of oxidative type.

4 Conclusions

Microstructure, adhesion and wear behavior along with

mechanical properties of the nanostructured AlSi–SiC,

2024Al–SiC and 6061Al–SiC alloys produced by ball

milling, were investigated by means of coatings deposited

on weathering steel (Cor-Ten A242) substrate using an

APS process. Ball milling was used to synthesize the

nanostructured AlSi–SiC, 2024Al–SiC and 6061Al–SiC

powders in high energy attrition mill under pure nitrogen

(99.99 %) atmosphere up to 8 h. Using ball milled pro-

cessed feedstock powders for air plasma spraying, a good

quality nanostructured coatings were obtained. Crystallite

size of matrix indicated that severe plastic deformation of

powder particles during high-energy attrition ball milling

decreased the crystallite size of matrix down to the order of

nm resulting the base grain size in coatings to decrease to

15, 17 and 32 nm for ball milled AlSi–SiC, 2024Al–SiC

and 6061Al–SiC coatings respectively. Results of particle

Fig. 8 X-ray diffraction

patterns of as sprayed coatings

at optimum spray conditions

Fig. 9 Wear histograms of the as-sprayed coatings on WS substrate

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size analysis and SEM showed that the addition of SiCp-

reinforcement influenced the matrix grain size and mor-

phology. XRD studies showed the embedment of SiCp in

the ball milled processed composite powder, and

nanocrystals in the ball milled powder and in the coatings.

Microstructural studies confirmed the uniform distribution

of SiC-reinforced particles in the coatings. The coatings

were found to have 30-50 % fraction of SiC particles, low

porosity level of about 1–2 %, hardness to the level of 351

HV. Adhesion strength of the coatings with the substrates

Fig. 10 Scanning electron

micrographs of worn surfaces

and their corresponding debris.

a AlSi–SiC, b 2024Al–SiC and

c 6061Al–SiC, at a load of 50 N

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123

was also excellent due to increased degree of diffusion at

the interface. The wear rate in the coatings was evaluated

using a pin-on-disk type tribometer under a 50 N load and

found to decrease by 60 % as compared to the basic matrix

coatings. The wear mechanism in the coating was found to

be delamination and oxidative type.

Acknowledgments The authors gratefully acknowledge the finan-

cial support of the Ministry of Education and Science of the Russian

Federation in the framework of Increase Competitiveness Program of

NUST «MISiS» (Grant § R4-2014-081) and financial & experi-

mental support of Malaviya National Institute of Technology Jaipur,

India and Council of Scientific and Industrial Research, CSIR-HQS,

Rafi Marg, New Delhi-110001, India.

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