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Materials Science and Engineering A 551 (2012) 5966

Contents lists available at SciVerse ScienceDirect

Materials Science and Engineering A


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

Inuence of forging on mechanical properties of NiP coated Si3 N4 reinforced


Al6061 composites
C.S. Ramesh a,b, , R. Keshavamurthy a
a
b

Department of Mechanical Engineering, PES Institute of Technology, Bangalore, India


School of Design, Engineering & Computing, Bournemouth University, United Kingdom

a r t i c l e

i n f o

Article history:
Received 13 January 2012
Received in revised form 10 April 2012
Accepted 16 April 2012
Available online 1 May 2012
Keywords:
Al6061
Hot forging
Silicon nitride

a b s t r a c t
NiP coated silicon nitride reinforced Al6061 composites were fabricated by liquid metallurgy route.
The percentage of silicon nitride as a reinforcement was varied from 4 wt% to 10 wt% in steps of 2. The
developed cast composites were hot forged at a temperature of 500 C. Both as cast and hot forged alloy
and their composites were subjected to microstructural studies, micro hardness and tensile strength tests.
Results reveal that, microhardness, yield and tensile strength of the developed composites are higher
when compared with that of matrix alloy under both as cast and hot forged conditions. Increased content
of silicon nitride in the matrix alloy leads to enhancement in micro hardness yield and tensile strength of
the composites. However, the ductility of the cast and forged composites decreases with increased content
of silicon nitride in the matrix alloy. Hot forged alloy and its composites possess higher microhardness,
tensile strength and ductility when compared with the cast composites for a given reinforcement content.
2012 Elsevier B.V. All rights reserved.

1. Introduction
Discontinuously reinforced aluminum based metal matrix composites (DRAMMCs) are the class of materials that have been
widely used in many engineering applications owing to their several improved mechanical properties such as excellent strength
to weight ratio, good wear resistance, isotropy, low cost and better reproducibility [1]. All the engineering properties of aluminum
composites do depend mainly on the quality of the processed composites which in turn depend on the processing routes adopted to
develop them [2]. In this regard, major focus is on synthesis of high
quality aluminum based MMCs developed by liquid metallurgy
route which is the most sought after and well accepted technique
owing to its simplicity and cost effectiveness [3]. However, composites developed by this technique cause interfacial reaction between
the matrix and the reinforcement. Further, poor wetting of the
ceramic particles in liquid aluminum results in weakening the bond
between the matrix and the reinforcement. A possible approach to
overcome this problem is to adopt use of metallic coated ceramic
particulate powders as reinforcement. It has been reported [4] that
metallic coating of ceramic particles enhances their wettability in
liquid aluminum and also minimizes the interfacial reaction. These
factors result in improved bond between the matrix and reinforcement.

Corresponding author. Tel.: +91 80 2672 1983; fax: +91 80 2672 0886.
E-mail address: csr gce@yahoo.co.in (C.S. Ramesh).
0921-5093/$ see front matter 2012 Elsevier B.V. All rights reserved.
http://dx.doi.org/10.1016/j.msea.2012.04.081

It is well known fact that the secondary processing of composites


by extrusion, rolling and forging can lead to improved mechanical properties, tribological behavior and corrosion resistance of
the primarily processed cast composites [5]. Khalifa and Mahmoud
[6] have reported on the tensile properties of as cast and extruded
Al606310 wt%SiC composites. They have observed that increased
content of SiC particles increases the strength up to 10 wt% in both
as cast and extruded conditions. The strength of extruded composites was higher than that of cast composites. Zhang et al. [7] have
reported that extruded Al6092/B4 C composites exhibited improvement in strength when compared with cast ones. Kang et al. [8] have
reported that the interfacial bond is a very important factor in dictating the tensile strength of Al alloy Al2 O3 short bre composites.
Lam et al. [9] have observed a marginal improvement in the tensile
strength of the cast composites with increased volume fraction of
SiCP reinforcement in the Al6061 matrix alloy. Ceschini et al. [10]
have studied the benecial effects of forging on tensile strength
of AA2618/20 vol%Al2 O3 composites. Thimmarayan and Thanigayarasu [11] have carried out studies on cast and forged Al6082/SiCp
composites. They have reported that the tensile strength of forged
composites is higher when compared with cast ones.
From the literature survey it is evident that most of the
researchers have focused on studying the mechanical behavior of
extruded aluminum based composites. However, meager information is available as regards the study on hot forging of aluminum
based metal matrix composites. Currently, in industries forging has
emerged as one of the important secondary processing route in
view of its several advantages. A near net shaped high strength

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C.S. Ramesh, R. Keshavamurthy / Materials Science and Engineering A 551 (2012) 5966

Table 1
Bath composition for electroless nickel deposition.

Table 2
Forging conditions.

Sl. No.

Bath constituents

Quantity (g/l)

Type of forging

Open die forging (upsetting/attening)

1
2
3
4
5

Nickel chloride, hexahydrate (NiCl2 6H2 O)


Sodium succinate, hexahydrate (Na2 C4 H6O4 6H2 O)
Sodium hypophosphite, monohydrate (NaH2 PO2 , H2 O)
Glycin (H2 NCH2 COOH)
Lead Nitrate (Pb(NO3 )2 )

30
10
20
10
0.02

Initial billet temperature


Initial die temperature
Die type
Average deformation ratio
Initial billet height
Final billet height
Average strain
Average strain rate

500 3 C
300 C
Flat die
6.5:1
80 mm
12 2 mm
0.85
0.0107 mm s1

component within a short duration and without incurring any damage are the characteristic features of hot forging. Silicon nitride
possesses very high hardness and excellent strength over a wide
range of temperature, superior wear resistance and antifriction
properties coupled with good corrosion resistance [12]. These properties make Si3 N4 an ideal choice as reinforcement in aluminum
alloys to produce MMCs. In the light of the above, the present investigation deals with the study on mechanical properties of hot forged
Al6061Si3 N4 composites processed by liquid metallurgy route.
2. Experimental details
2.1. NiP coating of silicon nitride particles
Silicon nitride (-acer) in powder form having average particle
size of 2040 m was obtained from M/s ACE Rasayan, Bangalore. Electroless coating technique was used to nickel coat silicon
nitride particles. Electroless nickel bath using sodium hypophosphite as a reducing agent was prepared to deposit thin adherent
nickelphosphide coating on silicon nitride particles. The details
of the bath composition used for electroless nickel deposition are
given in Table 1 [1214].
Silicon nitride particles taken in a beaker was soak cleaned
by immersing in toluene and propane followed by acetone wash.
Cleaned powder were vibrated by immersing in nitric acid to
roughen the surface, for further sensitivity and activation followed
by distilled water rinse. The surfaces of silicon nitride powder were
sensitized for further activation in a solution of stannous chloride and hydrochloric acid followed by distilled water rinse. Thus,
roughened and sensitized silicon nitride particles were treated
with palladium chloride solution for activating its surfaces prior
to nickel coating. Palladium activated silicon nitride particles were
then cleaned in distilled water and allowed to dry in air for 2 h. The
palladium activated silicon nitride particles were allowed to stay in
the freshly prepared electroless nickel bath. The temperature of the
bath was maintained at 85 C. The duration for coating was 30 min.
The pH of the bath was maintained at 4.5. NiP coated silicon nitride
particles were then thoroughly cleaned in distilled water and dried
by heating in oven at temperature of 50 C for 60 min.
2.2. Composite preparation and hot forging
NiP coated Si3 N4 reinforced Al6061 composites were fabricated by liquid metallurgy route. Percentage of NiP coated Si3 N4
particles was varied from 4 wt% to 10 wt% in steps of 2 wt%. The
cast Al6061 alloy and Al6061Si3 N4 composites were machined
to cylindrical shape of diameter 80 mm and height 80 mm. The
machined billets were subjected to hot forging process using a 300 T
hydraulic hammer at Fitwell Forgings Pvt. Ltd., Tumkur, Karnataka,
India. Table 2 shows the forging conditions adopted in this study.
2.3. Microstructure, porosity and grain size analysis
Both cast and hot forged Al6061 alloy and Al6061Si3 N4 composites were subjected to SEM using JSM 840a Jeol scanning
electron microscope at Indian Institute of Science, Bangalore, India.

Grain size analysis were performed at Advanced Metallurgical Laboratory, Peenya Industrial Area, Bangalore on polished samples
using Clemex Image Analyzer software as per ASTM 112-96 standard test method.
The apparent porosity of both as cast and hot forged alloy and
their composites was estimated using following relation [15]
W W1
100 (%)
W W2
W is the constant weight (obtained after heating the specimen in an
oven for a duration of 3 h at a temperature of 100 C); W1 is weight
of sample in hot water (obtained after heating the specimen in an
hot water for duration of 30 min); W2 is the weight of sample in
cold water.
Tests were carried out for 3 different samples in each composition and an average of all three results was considered as porosity
of the composite.
2.4. Microhardness
Hardness test was performed on polished samples of cast and
forged alloy and its composites using Vickers microhardness tester.
Tests were performed with a load of 100 g for duration of 10 s. The
test was carried out at ve different locations in order to contradict
the possible effect of indentor resting on the harder particles. The
average of all the ve readings was taken as hardness of the sample.
2.5. Tensile properties
Tensile tests of developed composites were evaluated as per
ASTM A370 standards at M/s. Sri Ram Institute of Industrial
Research, Whiteeld, Bangalore.
3. Results and discussion
3.1. Microstructure
Fig. 1(a)(f) shows SEM photos of Al6061 alloy and
Al6061Si3 N4 composites in as cast and hot forged conditions. It is
observed that the extent of distribution of reinforcement particle
in forged composites is more homogeneous than the cast ones,
indicating rearrangement and recrystallization during hot forging.
Further, there exists a good bond between the matrix and the
particle reinforcement even after forging as evidenced in Fig. 1(e)
and (f). No pullout, and fracture or damage of silicon nitride
particles is noticed in the forged composites. The particle size of
silicon nitride reinforcement in the forged composites for a given
reinforcement content is smaller than those in corresponding
as cast composites. The size of Si3 N4 particles before and after
forging was in the range of 3040 m and 1020 m, respectively.
This can be attributed to the high compressive stresses on the
ceramic reinforcement particles during hot forging. Further, it is
observed from the microphotographs of forged composites, that

C.S. Ramesh, R. Keshavamurthy / Materials Science and Engineering A 551 (2012) 5966

61

Fig. 1. SEM of as cast and hot forged Al6061Si3 N4 composites.

the reinforcement particles are oriented in the direction of metal


ow during forging.

solidication of composites [15]. The improved grain renement


on forging of alloy and all the developed composites can be mainly
attributed to the dynamic recrystallization during forging which is
effectively a thermo mechanical process [16].

3.2. Grain size analysis


Fig. 2 shows the micrographs of as cast and hot forged Al6061
alloy and Al606110 wt%Si3 N4 composites. Fig. 3 shows the variation of grain size in as cast and hot forged Al6061 matrix alloy
and the developed composites. It is observed that with increase in
the percentage of silicon nitride particles in matrix alloy, there is a
reduction in the average grain size of the composites in both as cast
and hot forged conditions. However, a larger extent of grain renement in hot forged composites is observed when compared with
cast composites for a given reinforcement content. A maximum
of 31% and 51% reduction in the average grain size are observed
for as cast and hot forged Al606110 wt%Si3 N4 composites respectively when compared with as cast matrix alloy. This reduction in
grain size may be attributed to fact that, presence of ceramic particles in the molten aluminum alloy acts as nucleation sites during

3.3. Porosity
Fig. 4 shows the variation of porosity of Al6061 matrix alloy
and Al6061Si3 N4 composites in as cast and hot forged conditions
respectively. It is observed that with increased content of silicon
nitride there is an increase of porosity in the developed composites
under both cast and forged conditions. Cast Al606110 wt%Si3 N4
composite and its alloy exhibited porosity levels of 2.2% and 1.5%
respectively. It is observed that on forging, there is a signicant
decrease in the porosity of cast matrix alloy and its composites.
Hot forged Al606110wt%Si3 N4 composite and its alloy exhibited
porosity levels of 1.1% and 0.75% respectively. This can be attributed
to the fact that hot forging leads to higher densication and grain
renement of the matrix material [1719].

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C.S. Ramesh, R. Keshavamurthy / Materials Science and Engineering A 551 (2012) 5966

Fig. 2. Optical micrographs illustrating the variation of grain size of as cast, hot forged alloy and its composites.

Fig. 3. Variation of grain size of Al6061 alloy and its composites.

Fig. 5. Variation of microhardness of Al6061 alloy and its composites with reinforcement.

3.4. Microhardness

Fig. 4. Variation of porosity of Al6061 alloy and its composites.

Fig. 5 shows the variation of microhardness with increase in percentage weight of silicon nitride particles in Al6061 alloy in as cast
and hot forged conditions. It is observed that there is a signicant
improvement in microhardness with addition of silicon nitride particles in matrix alloy. An improvement of 83% and 92% increase is
noticed with addition of 10 wt% silicon nitride particles in matrix
alloy in as cast and hot forged composites respectively.
This drastic improvement in the hardness value of matrix alloy
may be attributed to the fact that, silicon nitride being hard reinforcement do exhibit greater resistance to indentation of hardness
tester, by rendering its inherent property of hardness to matrix
alloy [20].
It is also reported that addition of hard reinforcement in soft
ductile matrix always enhances the bulk hardness of matrix material [21]. Further, there is a large difference in co-efcient of thermal
expansion of Al6061 alloy and silicon nitride particles, which will

C.S. Ramesh, R. Keshavamurthy / Materials Science and Engineering A 551 (2012) 5966

63

Ulmate Tensile Strength (MPa)

350

3.5. Yield strength


Fig. 6 shows the variation of yield strength of as cast and hot
forged Al 6061 matrix alloy and its composites. It is observed with
increase in percentage of reinforcement there is an increase in yield
strength for both as cast and hot forged composite. A maximum
improvement of 50.58% and 107.44% for has been observed in as
cast and hot forged Al606110 wt%Si3 N4 composites respectively
when compared with their matrix alloys.

Hot Forged
250
200
150
100
50
0

Fig. 6. Variation of yield strength of Al6061 alloy and its composites.

lead to thermal mismatch between matrix alloy and reinforcement.


This factor increases the density of dislocations in the material
resulting in higher hardness value [22]. It is also evident from SEM
that lesser extent of porosity is observed in both as cast and hot
forged composites. It is reported that higher hardness is always
associated with lower porosity of metal matrix composites [2224].
On the other hand, silicon nitride particles are NiP coated prior to
addition in molten metal, as a benecial result of it, the interface is
free from the reaction products as discussed earlier and even good
bond exists between matrix alloy and reinforcement. Thus, the load
transfer capability of matrix to the reinforcement is expected to be
more which may be another reason for higher hardness value.
Further, in all the cases studied hot forged composites posses
higher hardness when compared with cast ones. The higher hardness of the forged matrix alloy and the forged composites can be
reasoned to the fact that during forging process, some of the existing minor aws in casting get healed up there by contributing
to further improvement in the hardness of forged samples when
compared with the cast ones. In addition to this, signicant grain
renement is noticed in both matrix alloy and composites after
forging. This reduction in average grain size will result in more
obstacles for dislocation motion, thereby enhancing the resistance
to plastic deformation resulting in higher hardness.

As Cast

300

Al6061

Al6061-4Wt%
Si3N4

Al6061-6Wt%
Si3N4

Al6061-10Wt%
Si3N4

Fig. 7. Variation of ultimate tensile strength of Al6061 alloy and its composites with
reinforcement.

aws/defects in the composites will be very less and will result in


increased ultimate tensile strength [2931].
In increasing the strength of the composite material a critical
role has been played by the clean interface that exists between
matrix material and reinforcement. It is reported that the moderate interfacial reaction and enhanced interfacial bonding between
matrix and reinforcement results in improved bulk mechanical
properties. It is also reported that, when the reaction free interface
exists between matrix and reinforcement, the load transfer efciency of matrix to the reinforcement is high. Thus, higher stress is
required to initiate the crack between matrix alloy and reinforcement resulting in higher tensile strength [25]. Further, hot forged
composites possess higher tensile strength when compared with
cast ones. The improvement in tensile strength of hot forged Al6061
matrix alloy and Al6061Si3 N4 composites can be attributed to
their increased hardness. The other factor that may contribute to
the enhancement in strength of the hot forged composites is the
result of the consolidation route and thermo mechanical treatment.
The hot forging process generates substantial plastic work as well
as some plastic anisotropy. The enhancement in the strength on hot
forging can be due to the absence of micro porosity, better interfacial bond between matrix and reinforcement. Grain renement
on hot forging is also one of the factors in improving the tensile
strength of forged composites.

14

3.6. Ultimate tensile strength (UTS)

As Cast
12

Hot Forged

10

Duclity (%)

Fig. 7 shows variation of ultimate tensile strength with increase


in percentage of silicon nitride particles in as cast and hot forged
conditions. The ultimate tensile strength of the composite material
increases by an amount of 99% and 203% in as cast and hot forged
Al6061Si3 N4 composites respectively when compared with as
cast matrix alloy. This trend is similar to results of other researchers
[2527]. Addition of silicon nitride particles induces strength to
matrix alloy thereby causing increased resistance to tensile stresses
resulting in enhanced ultimate tensile strength. Further, the generation of high dislocation densities due to difference in co-efcient
of thermal expansion between matrix and reinforcement may also
be responsible for improved tensile strength [28]. In addition, the
particle size of the silicon nitride particles is very small of range
between 20 and 30 m. The chances of having strength limiting

Al6061-8Wt%
Si3N4

8
6
4
2
0
Al6061

Al6061-4Wt%
Si3N4

Al6061-6Wt%
Si3N4

Al6061-8Wt% Al6061-10Wt%
Si3N4
Si3N4

Fig. 8. Variation of ductility of Al6061 alloy and its composites with reinforcement.

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C.S. Ramesh, R. Keshavamurthy / Materials Science and Engineering A 551 (2012) 5966

Fig. 9. (ad) SEM of fractured surfaces of as cast and hot forged Al6061Si3 N4 composites.

3.7. Ductility
Fig. 8 shows variation of ductility of Al6061 alloy Al6061Si3 N4
composites in both as cast and hot forged conditions. It is observed
that addition of Si3 N4 leads to the drastic reduction in ductility
of Al6061Si3 N4 composites for both as cast and hot forged conditions. The reduced ductility of Al6061Si3 N4 composites with
increased content of Si3 N4 particles in both as cast and hot forged
conditions can be attributed to the stress concentration effects at
the interface of the matrix and Si3 N4 particles.
The presence of intrinsically brittle phases and presence of additional secondary or intermetallic phases serve as potential sites
for early crack nucleation resulting in reduction in ductility under
quasi-static loading [26]. However, when compared with cast alloy
and cast Al6061Si3 N4 composites, the hot forged alloy and its composites show signicant improvement in the ductility. The ductility
values of cast Al6061 alloy and cast Al606110 wt%Si3 N4 composites are 6.9% and 1.9% respectively. In case of forged Al6061
alloy and forged Al606110 wt%Si3 N4 composites the ductility values are 11.2% and 5.7% respectively. It can be clearly observed
that upon forging there is signicant increase in ductility when
compared with cast ones. This can be mainly due to recrystallization and grain renement in matrix material during forging of
alloy and developed composites. The improvement in the ductility after forging can also be attributed to porosity reduction and
homogenization of reinforcement distribution, and also an extensive rened microstructure obtained. All these factors together

improve the interfacial strength and ductility of the matrix and


composites [32].

3.8. Fractography
Fig. 9(a)(d) shows the tensile fractured surfaces of as cast
and hot forged Al6061 alloy and its composites. It is evident
from the microphotographs that the base matrix alloy exhibits
larger and uniform voids indicating the ductile fracture, whereas
Al6061Si3 N4 composites show voids of size smaller than that of
base alloy, indicating macroscopically brittle fracture and microscopically ductile fracture. The observation made on the fractured
surface of the composites indicates several common features as
reported by many researchers [33,34]. SEM micrographs of fractured surfaces show symptoms of possible de-cohesion at the
interface between matrix, void nucleation and reinforcement and
fracture of reinforced phase. Fig. 10 shows fractured surface of
cast Al606110 wt%Si3 N4 composite. Several non-uniform voids
are observed, which can be attributed to debonding/de-cohesion
of reinforced particles from matrix material. Some of the damages
noticed on the fractured surface are located away from deep voids,
which reveal the greater ductility of matrix material.
Fig.
11
shows
fractured
surface
of
hot
forged
Al606110 wt%Si3 N4 composites. It is observed that small sized
reinforced silicon nitride particles ow along with the matrix
material until the debonding occurs.

C.S. Ramesh, R. Keshavamurthy / Materials Science and Engineering A 551 (2012) 5966

65

few agglomerations of the reinforced silicon nitride particles on


the fractured surfaces while there is elimination of the same after
forging.
The fracture of the reinforced phase may be due to the excellent
bond that exists between the matrix alloy and the reinforcement as
a result of metallic coating of reinforcement. With the increase in
load during tensile loading, the larger particle will undergo fracture
rst, followed by fracture of small sized particles. The maximum
intensity of particle fracture is observed in the region of particle
clustering. The crack initiation in the matrix as observed in Fig. 12
shows the limited ductility of matrix material in the presence of
reinforcing phase. The fracture of the reinforced phase and the failure of the surrounding matrix result in the formation of ne voids
at the particle/matrix interfaces [35,36].
4. Conclusion

Fig. 10. SEM of fractured surfaces of as cast Al606110 wt%Si3 N4 composite.

Microstructure studies on Al6061Si3 N4 composite clearly


reveal uniform distribution of silicon nitride particles in both as
cast and hot forged conditions with excellent bond between the
matrix and the reinforcement.
Appreciable reduction in the grain size of forged composites has
been observed when compared with cast composites.
Microhardness, yield and tensile strength of composites are
higher when compared with that of matrix alloy for both as cast
and hot forged composites. Increased content of silicon nitride
in the matrix alloy leads to enhancement in microhardness, yield
and tensile strength of the composites. Ductility of the composites
decreases with increased content of reinforcement in the matrix
alloy for both as cast and hot forged condition. However, hot forged
composites possess higher ductility when compared with the cast
composites.
Acknowledgements

Fig. 11. SEM of fractured surfaces of as hot forged Al606110 wt%Si3 N4 composite.

Further, it is also noticed that, most of the dimples/voids seem


to be formed in the direction of tensile loading rather than the lateral in both as cast and hot forged composites. Some of the hollow
dimples contain reinforced particles indicating good bond between
the matrix and the reinforcement. The cast composite exhibits a

Fig. 12. SEM of cast Al606110 wt%Si3 N4 composite.

The authors would like to acknowledge their sincere thanks to


Naval Research Board (NRB), India, for nancial support provided
for this research work under grant in aid scheme (Project No. NRB111/MAT/06-07).
The authors would like to express their deep sense of gratitude
to Prof. D. Jawahar, CEO, PES Group of Institutions and Dr. K.N.B.
Murthy, Principal and Director, PESIT, Bangalore.
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