April 2002

Materials Letters 53 (2002) 244 – 249

www.elsevier.com/locate/matlet

Copper matrix SiC and Al2O3 particulate composites by powder

metallurgy technique
S.F. Moustafa a, Z. Abdel-Hamid a,*, A.M. Abd-Elhay b
a
Central Metallurgical Research and Development Institute, P.O. Box 87, Helwan, Cairo, Egypt
b
Faculty of Engineering, Helwan University, Cairo, Egypt
Received 16 October 2000; received in revised form 28 June 2001; accepted 3 July 2001

Abstract

Copper matrix reinforced with either Ni-coated or uncoated SiC and Al2O3 particulate composites were made by means of
the powder metallurgy route. The reinforcement particles of SiC and Al2O3 were coated with a thin layer of nickel by electroless
method. The coated or uncoated reinforcement particles of either SiC or Al2O3 were added to copper metal powders with
nominal loading of 20 wt.%, mixed in a mechanical mixer having 360 rpm for a period of 10 min. Each mixture of the
investigated powders was cold compacted at 600 MPa, and sintered at 900 BC, in hydrogen atmosphere.
The electroless coating process of the investigated reinforcements is given. Micrographs of Ni-coated particles of SiC and
Al2O3, and the microstructure of the sintered composites are also provided. Some physical and mechanical properties of the
copper matrix Ni-coated and uncoated particulate composites are measured and explained with regard to its structure. D 2002
Elsevier Science B.V. All rights reserved.

Keywords: Copper matrix; SiC; Al2O3; Powder metallurgy technique

1. Introduction two main routes depending on the state of matrix

Metal matrix composites (MMCs), reinforced with
particulate or discontinuous fibres of SiC or Al2O3,
are potential candidate materials for a variety appli-
cations. The importance of these composites could
be attributed to their high stiffness, superior room
and elevated temperature strengths, improved wear
resistance and low coefficient of thermal expansion
[1– 3].
Several processing techniques could be used for the
production of MMCs, which could be grouped into
*
Corresponding author. Fax: +20-2-5010-639.
E-mail address: rucmrdi@rusys.eg.net (Z. Abdel-Hamid).
during the fabrication process, either liquid or solid
routes [4 – 7]. The production of MMCs by liquid
metal processing are receiving a great deal attention
because of their low cost, but they suffer from the fol-
lowing drawbacks: (i) nonuniform distribution of
ceramic particles or fibres due to the agglomeration
and dendritic segregation, and (ii) undesirable chem-
ical reaction at the interface due to the high temper-
ature of the melt.
These drawbacks could be minimized using pow-
der metallurgy route. Powder metallurgy process
(PM) lends itself well for economical mass production
components. Different metal matrix composites are
manufactured by this PM route [8 – 10]. However,
relatively poor physical and mechanical properties

0167-577X/02/$ - see front matter D 2002 Elsevier Science B.V. All rights reserved.
PII: S 0 1 6 7 - 5 7 7 X ( 0 1 ) 0 0 4 8 5 - 2
 S.F. Moustafa et al. / Materials Letters 53 (2002) 244–249
are obtained due to the existence of a large amount
of residual porosity due to the nonwetting character-
istics between metal matrix and SiC and Al2O3
particles [11].
The objectives of the present investigation are: (i)
to prepare Cu-matrix composites reinforced with 20
wt.% of either Ni-coated or uncoated powders of SiC
or Al2O3, and (ii) to demonstrate the superiority of Ni-
coated powders reinforcements over the uncoated
powders reinforced composites. The reason of select-
ing Ni as a coating material instead of Cu-coating is
that Ni-coating has better adhesion on SiC and Al2O3
powders than Cu-coating. Also, nickel forms a solid
solution with copper, i.e. nickel is compatible with
both reinforcement materials and Cu-matrix.
2. Experimental
2.1. Materials
The materials used in this investigation were
highly pure SiC powders of a-type made by Carbor-
undum, Perth Amboy, NJ, and Al2O3 powder of a-
Fig. 1. Variation of dimensional change as a function of sintering time of: Cu – 20% coated SiC, Cu – 20% SiC, Cu – 20% coated Al2O3, and
Cu – 20%Al2O3 composites.
245
type of high purity made by Aldrich, Brockmann 1,
STD grade, CA. The copper powders used in this
investigation were of electrolytically precipitated
powders and made by Ecko, Germany. The powder
sizes were nominally minus 200 mesh. Powders of
SiC and Al2O3 were etched in nitric acid, washed with
distilled water and dried.
2.2. Coating of powders
Powders of SiC and Al2O3 were coated sepa-
rately with nickel by electroless method. The surface
of the investigated powders were sensitized and acti-
vated prior to nickel coating. The treatment consists
of the following steps: (1) cleaning the surface of
powders in an organic solvent such as acetone for 15
min, (2) sensitization in an aqueous solution consists
of 10 g/l SnCl2
H2O and 30 ml/l HCl for 15 min,
(3) then activated in an aqueous solution of 0.25 g/l
PdCl2 and 3 ml/l HCl for 15 min, and (4) rinsing
the activated powders in boiling water, and drying
[12]. The dried powders were gently dispersed in an
electroless bath containing a solution of 45 g nickel
chloride, 8 g sodium hypophosphite, 100 g sodium
246 S.F. Moustafa et al. / Materials Letters 53 (2002) 244–249

Table 1 Microstructural investigation was performed using

Values of relative density and porosity % of: Cu – 20% coated SiC, optical and scanning electron microscopy. Property
Cu – 20% SiC, Cu – 20% coated Al2O3, and Cu – 20% Al2O3 com-
posites measurements included density and porosity. Com-
pression strengths of these composites were meas-
Material composition Relative density Porosity (%)
ured using Schematzu testing machine at strain rate
Cu – 20% coated SiC 0.95 5
of 0.2 mm/mm min. Samples were compressed
Cu – 20% SiC 0.87 13
Cu – 20% coated Al2O3 0.975 2.5 between graphite-lubricated steel disks at room tem-
Cu – 20% Al2O3 0.92 8 perature.

citrate, 50 g ammonium chloride dissolved in 1 l 3. Results and discussion

distilled water [13].
After the nickel deposition, the powders were
washed with cold water, dried in air, and weighed.
2.3. Composites fabrication
Powders of 20 wt.% of SiC or Al2O3 (coated or
uncoated) were each mixed with Cu-metal powder in
conical flask using a mechanical stirrer of 360 rpm
for 6 min. Four mixtures were obtained, namely Cu –
20% coated SiC, Cu – 20% SiC, Cu – 20% coated
Al2O3, and Cu – 20% Al2O3. Each mixture was cold
compacted in a floating die using hydraulic press at
compaction pressure of 600 MPa. The compacts
were in the shape of cylinders of 8 mm in diameter
and 12 mm in length, with tolerances of 0.1 mm in
length direction. The compacts were sintered in a
horizontal tube furnace at 900 BC in pure hydrogen
atmosphere.
3.1. Densification process
Fig. 1 compares compact shrinkage as a function
of time for Cu – 20% coated SiC, Cu – 20% SiC,
Cu – 20% coated Al2O3, and Cu – 20% Al2O3 com-
posites. It is observed that coated powders containing
composites shrink during sintering and reach an al-
most dimension stability after about 24 min sintering
time. However, in the case of uncoated powders
containing composites the samples exhibit swelling
during sintering. Dimensional stability during sinter-
ing of uncoated composites reached after about 60
min. It is evident that the densification of compacts
made from Ni-coated powders are much faster than
those made from regular powder mixtures by about
2.5 times. Lack of both wettability and solubility of
SiC and Al2O3 (uncoated powders) with copper
prevent densification by grain shape accommodation

Fig. 2. Micrographs of powders of: (a) Ni – coated SiC, (b) Ni – coated Al2O3.
 S.F. Moustafa et al. / Materials Letters 53 (2002) 244–249 247

and solution-reprecipitate. Therefore, for such sys-
tems, the contribution to densification by coalescence
of Cu-powder become very significant [14]. The
uncoated powder composites are characterised by
solid-state sintering between the Cu-particles during
heating which results in a copper skeletal structure.
Contrary to that, Ni-coated powders containing com-
posites sintered by heterodiffusion mechanism. In such
blends, the heterodiffusion takes place at the Cu – Ni
contacts, and the Cu-skeleton shrinks because of the
shrinkage at the Cu – Cu contacts is high. Table 1
reports the values of relative density and porosity
content of the investigated composites. It is clear that
uncoated powders of either SiC or Al2O3 have higher
porosity content due to the lack of wettability.
3.2. Microstructure
Fig. 2a and b shows micrographs of Ni – coated SiC
and Ni– coated Al2O3 powders. The coating procedure
used in this study resulted in a batched Ni-precipita-
tion on the surfaces of either SiC or Al2O3 particles.
The phosphorous concentration was very limited and
it was less than 0.03%.

Fig. 3. Microstructures of: (a) Cu – 20% coated SiC, (b) Cu – 20% SiC, (c) Cu – 20% coated Al2O3, and (d) Cu – 20% Al2O3 composites.
248 S.F. Moustafa et al. / Materials Letters 53 (2002) 244–249

The microstructures developed in the sintered Table 2

composites reveals the differences in their process- Compression properties of: Cu – 20% coated SiC, Cu – 20% SiC,
Cu – 20% coated Al2O3, and Cu – 20% Al2O3 composites
ing parameters. Fig. 3a – d show micrographs of Cu –
Materials 0.2% proof Fracture Elongation
20% coated SiC, Cu – 20% SiC, Cu – 20% coated
composition stress (MPa) strength (%)
Al2O3, and Cu – 20% Al2O3 composites, respectively. (MPa)
Fig. 3a shows a very good adhesion between SiC
Cu – 20% coated SiC 83 344 43.6
particles and Cu-matrix, but uncoated SiC graph, Fig. Cu – 20% SiC 16 135 30.4
3b, reveals that the adhesion between SiC particles Cu – 20% coated Al2O3 62 285 48.4
and Cu-matrix is poor, due to the presence of gaps Cu – 20% Al2O3 14.1 112 33.2
and porosity between SiC and Cu-matrix. Almost no
detectable porosity and very good adhesion between
particles and Cu-matrix are observed in Cu-coated
Al2O3 composite, as indicated in Fig. 3c. In the case was noticed that all compressed samples, either coated
of Cu-uncoated Al2O3 composite, Fig. 3d, gaps or uncoated, were fractured at an inclined angles of
between Al2O3 particles and Cu-matrix are observed. 45B, which means that fracture is taking place by a
Metallographic observation of composites produced shear mode.
by uncoated reinforcement of both cases of SiC and The results compiled in Table 2 demonstrate that
Al2O3, as those shown in Fig. 3b and d, revealed that the yield and breaking (fracturing) strengths of the
both closed and interconnected porosity are present. coated composites are much higher than those of
The presence of porosity in the case of Cu-uncoated uncoated composites. Also, it is noted that the com-
reinforcement composites could be attributed to the pression strains of coated composites are higher than
masking or at least partially masking of Cu powder those of uncoated composites. The improvements of
with fine dust of SiC or Al2O3 which was generated compression properties of the coated composites
during the mixing process of uncoated reinforcement could be attributed to the good adhesion between
and Cu due to the wear abrasion of reinforcements coated particles and the Cu-matrix, in addition to the
during their contacts with each other or with the wall higher density and lower porosity.
of the mixer. When these Cu-powders which covered
with dust were investigated using scanning electron
microscope, the dust powders were seen at the start 4. Conclusions
of investigation, but after few seconds they fly like
ashes and disappeared. The emitted electrons of the This investigation provides insights into densifica-
microscope hit the dust, and due to the absence of tion and compression properties in Cu – 20% coated
adhesion or bonding between copper powders and SiC, Cu – 20% SiC, Cu – 20% coated Al2O3, and Cu –
the dust of SiC or Al2O3, they fly in the evacuated 20% Al2O3 composites. The Cu-composites fabri-
chamber of the microscope. During sintering, the Cu/ cated by mixing uncoated powders of SiC or Al2O3
Cu contacts became less, but SiC/SiC or Al2O3/ exhibit swelling during sintering at constant tempe-
Al2O3 contacts increased due to the partially covered rature of 900 BC. However, Ni-coated powders
Cu powder with reinforcement dust, which resulted a containing composites shrink during sintering. The
weak interfacial bonding between SiC or Al2O3 and densification of compacts fabricated from coated
Cu-matrix. powders is much faster with 2.5 times than those
made from uncoated powders. The Cu matrix Ni-
3.3. Compression strength coated reinforced composites have higher relative
density and lower porosity content than the uncoated
Compression strengths were determined at 20 BC composites, due to the good adhesion between the
on samples of Cu – 20% coated SiC, Cu – 20% SiC, reinforcements and the Cu-matrix. Yield and breaking
Cu –20% coated Al2O3, and Cu – 20% Al2O3 compo- compression strengths of coated reinforcement pow-
sites. The yield stress measured as 0.2% proof stress ders containing composites are superior than those of
for all composites, either coated or uncoated ones. It uncoated ones.
 S.F. Moustafa et al. / Materials Letters 53 (2002) 244–249
References
[1] J. Lui, A. Upadhyaya, R.M. German, Metall. Trans. 30A
(1999) 2209.
[2] S.M. Devincent, G.M. Michal, Metall. Trans. 24A (1993) 53.
[3] A. Yeoh, C. Persad, Z. Eliezer, Scr. Mater. 37 (3) (1997) 271.
[4] S. Ho, E.J. Lavernia, Metall. Trans. 27A (1996) 3241.
[5] P.K. Rohatgi, R. Asthana, S. Das, Int. Met. Rev. 31 (3) (1986)
115.
[6] S.J. Harris, Mater. Sci. Technol. 4 (1988) 231.
249
[7] T. Chou, T. Oki, Mater. Sci. Technol. 3 (1987) 378.
[8] M. Inal, M. Alam, Metall. Trans. 30A (1999).
[9] C.M. Friend, J. Mater. Sci. 22 (8) (1987) 3005.
[10] T.W. Chou, A. Kelly, A. Okura, Composites 16 (3) (1985) 187.
[11] G. Ramani, T. Ramanohan, R. Pillai, B. Pai, Proceedings of
International Seminar on Interfacial Phenomenon in Compo-
site Materials, Sheffield, UK, 1989, pp. 246.
[12] M. Patel, B. Padhi, Powder Metall. Int. 24 (10) (1992).
[13] T.Y. Chan, S.T. Lin, J. Mater. Eng. Perform. 6 (5) (1997).
[14] J.L. Johnson, R.M. German, Metall. Trans. 23A (1996) 1455.