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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
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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
1
2
3
4
5
30
10
20
10
0.02
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
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. 5. Variation of microhardness of Al6061 alloy and its composites with reinforcement.
3.4. Microhardness
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
350
Hot Forged
250
200
150
100
50
0
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.
14
As Cast
12
Hot Forged
10
Duclity (%)
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
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
Fig. 11. SEM of fractured surfaces of as hot forged Al606110 wt%Si3 N4 composite.
66
[21]
[22]
[23]
[24]
[25]
[26]
[27]
[28]
[29]
C.S. Ramesh, R. Keshavamurthy / Materials Science and Engineering A 551 (2012) 5966
F.J. Humpherys, Acta Metall. 25 (1977) 1323.
V.V. Ganesh, C.K. Lee, M. Guptha, Mater. Sci. Eng. A 333 (12) (2002) 193198.
Z.F. Moustafa, Wear 185 (1995) 189195.
Z.F. Zhang, L.C. Zhang, Y.W. Mai, J. Mater. Sci. 30 (1994) 19611966.
Y.L. Shen, Chawla, Mater. Sci. Eng. A 297 (2001) 44.
K.S. Foo, R.A.L. Drew, Composites 25 (1994) 677683.
K.F. Ho, M. Gupta, T.S. Srivatsan, Mater. Sci. Eng. A 369 (12) (2004) 302308.
T.P.D. Rajan, R.M. Pillai, B.C. Pai, J. Mater. Sci. 33 (1998) 491.
M. Vogellany, R.J. Arsenault, R.M. Fisher, Metall. Trans. 17 (1986) 379389.
[30]
[31]
[32]
[33]
[34]