Beruflich Dokumente
Kultur Dokumente
Department of Materials Science and Engineering, University of Ioannina, Ioannina 45110, Greece
Physical Metallurgy Department, Materials Science Institute, The University of Miskolc, H-3515 Miskolc-Egyetemvaros, Hungary
a r t i c l e
i n f o
Article history:
Received 11 June 2014
Accepted 14 August 2014
Available online 27 August 2014
Keywords:
Aluminium Matrix Composites
WC/TiC nanoparticles
Melt inoculation
Sliding wear
Cyclic polarization
Dilute Harrisons Solution
a b s t r a c t
In the present effort, Aluminium Matrix Composites (AMCs) were produced by the addition of submicron
sized TiC and WC particles of low (up to 1.0 vol%) content into a melt of Al1050. Casting was assisted by
the use of K2TiF6 as a wetting agent and mechanical stirring to limit particle clustering. An extensive
presence of intermetallic phases was observed in the cast products, as a result of both the inoculation
by K2TiF6 and the intensive mainly due to the ne carbide particle size reactivity of the carbides with
the molten matrix. Particle distribution was reasonably uniform comprising both clusters and isolated
particles. The intermetallic particle dispersion has changed the intended nature of the composites.
Instead of one type of reinforcement, that of carbide particles, the aluminium matrix contained two main
types of reinforcement: (a) in-situ intermetallic particles and (b) carbide nanoparticles, as such, or more
often as clusters of remaining carbide nanocores and aluminide particles. The reinforced materials
exhibited a notably improved sliding wear performance over that of the alloy owing to the benecial
effect of both the carbide and the intermetallic phase dispersion. A wear mechanism was formulated
based on microstructural features of the wear surface (repeated hill-valley morphology, surface oxide
layers, crack formation and grooving). Cyclic potentiodynamic polarization in Dilute Harrisons Solution
(DHS) revealed that the corrosion behaviour of the reinforced materials was mainly controlled by the
corrosion of the alloy matrix. As such, the predominating form of corrosion was intergranular corrosion
(IC) of Al associated with the presence of alloy matrix impurities. Carbide nanoparticles, aluminide phase
associated with them and their Al-matrix remained essentially intact of corrosion. IC progress was often
inhibited by the presence of clusters of aluminide and carbide particles.
2014 Elsevier Ltd. All rights reserved.
1. Introduction
Due to properties, such as high specic strength and stiffness,
low density and low thermal expansion coefcient, Aluminium
Matrix Composites (AMCs) have attracted great scientic attention
as candidate materials for high-tech, structural and functional
applications including aerospace, defense, automotive, electronic
packaging, precision instruments, thermal management areas,
sports equipment and recreation. Among them, particulate
reinforced AMCs (PRAMs) have extensively been investigated
owing to their low production costs and versatility in employing
conventional techniques for their production and shaping [13].
Recent evidence has shown that the mechanical response of AMCs
can further be improved if submicron- and nano- sized particles
Corresponding author. Tel.: +30 26510 07309; fax: +30 26510 07034.
E-mail address: alekatou@cc.uoi.gr (A. Lekatou).
http://dx.doi.org/10.1016/j.matdes.2014.08.040
0261-3069/ 2014 Elsevier Ltd. All rights reserved.
1122
Regarding the second drawback, in conventional casting processes, the particle-molten Al wetting behaviour is the most crucial
factor for a successful particle insertion in the melt. Towards this
direction, ceramic phases with a strong metallic character, such
as TiC and WC, may ensure enhanced particle liquid metal wetting compatibility [17]. Besides, TiC and WC exhibit very high
hardness and modulus of elasticity, excellent wear and high temperature properties and good corrosion resistance, properties of
great industrial signicance. Nevertheless, research efforts on WC
and TiC cast reinforced AMCs are limited and they, in their vast
majority, concern microsized TiCp reinforced AMCs. These works
have produced promising results as far as the wetting behaviour
of the melt, the dispersion uniformity, as well as the strength
and wear resistance are concerned [1825]. Additionally, the particle insertion can further be assisted by the use of uxing agents,
such as halide salts that dissolve the oxide layer formed on the
surface of the molten alloy; thus, the involved phases are allowed
to express their net wetting characteristics and enhance particle
incorporation [21,22,24,2629].
Regarding the third drawback, it is well established that the
aqueous corrosion behaviour of AMCs can be affected by many
AMC features. The matrix-reinforcement interface, the matrix/
secondary phase interface, the secondary phase nature and content,
the reinforcement/secondary phase interface, the electrolyte active
ion concentration, the production route, the heat treatment, the surface treatment can signicantly affect the corrosion resistance and
mechanisms [3034]. Owing to these too many factors, conicting
data and interpretations exist regarding fundamental issues, such
as corrosion resistance and corrosion initiation sites [35]. Several
studies have reported lower corrosion resistances for AMCs in comparison with the respective monolithic alloys. Various reasons have
been considered responsible for this deterioration of corrosion resistance in AMCs: (a) breakdown of a continuous passive lm at the
matrix/reinforcement interfaces [36]; (b) galvanic coupling of aluminium and reinforcement [37]; (c) voids at the reinforcement/
matrix interface [38]; (d) an increase in the dislocation
density around particle clusters [39]; (e) interfacial layers around
particulate reinforcements that promote galvanic corrosion [30];
(f) formation of intermetallic phases by reaction of the reinforcement with the matrix due to heat treatment [34] or precipitation
of intermetallic phases enhanced by the presence of particulates
[33]. More recently, Pardo et al. [40] noted that the corrosion damage in AA360/SiCp and AA380/SiCp composites in (13.5) wt% NaCl
was caused by pitting attack mainly at the reinforcement/matrix
interface.
However, Grifths and Turnbull [41] did not notice any apparent effect of SiC reinforcement on the electrochemical behaviour
of Al6061 in aerated 3.5 wt% NaCl. They concluded that the effects
of reinforcement on the corrosion of Al cannot be generalized and
are specic functions of the environmental conditions and the processing route. The following works tend to support this claim:
Trowsdale et al. [38], whilst nding no signicant galvanic action
between SiC and Al, noticed that 20 wt% incorporation of SiC (of
particle size of 3 lm) in Al1050 led to a slight reduction of the pitting resistance of the alloy. However, large particle sizes (20 lm)
led to intensication of pitting due to cracking during the fabrication process. Kiourtsidis et al. [42] stated that the SiCp presence
does not accelerate failure of the passivation oxide lm, whereas
pitting corrosion potentials in aerated 3.5 wt% NaCl are not
considerably affected by the SiCp content at a given aging condition; nevertheless, alteration in aging kinetics due to SiCp presence
is responsible for the differentiation in the pitting corrosion
behaviour among the composites. Alaneme and Bodunrin [43]
claimed that unreinforced AA6063 exhibited slightly superior corrosion resistance than the AA6063/Al2O3p composites in NaCl and
NaOH media; however, the composites showed better corrosion
2. Experimental procedure
AMCs were prepared by the addition of sub-micron sized WC
particles (of approximate particle size of 200400 nm) and TiC
particles (of approximate particle size of 400700 nm) into
Al1050 (Al of 99.5% commercial purity). The compositions
employed were: Al-0.7 vol% TiC, Al-1.0 vol% TiC, Al-0.5 vol% WC
and Al-1.0 vol% WC. Wetting and homogenization were assisted
by two approaches: Fluxing and mechanical stirring. K2TiF6 (10 g
K2TiF6/190 g Al1050) was utilized as a uxing salt for removing
the oxide phase from the surface of the aluminium melt [26,29].
First, mixing of the reinforcement and the salt was carried out. Then,
this mixture was added into the alloy melt (830 C). The salt was
allowed to react with Al, a slag was formed, the carbide particles
inltrated into the melt and the slag was removed by a ladle. Rigorous stirring was then applied for homogenization and breakage of
any initial particle clusters. Stirring was conducted by an in-house
made apparatus based on an AEG SB2E 700R power drill, with a
graphite rod being adapted and a four branch stirring shaft being
assembled at the end of the rod. The stirring speed was kept
constant at 3200 rpm. The stirring duration was 20 s. A nal slag
cleaning was performed prior to casting into cylindrical, steel
moulds of 1.5 cm inner diameter and 15 cm height.
Specimens were cut from each cast bar, mounted and prepared for
metallographic examination. Standard metallographic procedures
Temperature (K)
1123
Al
Ti
Al (mole fracon)
Temperature (K)
liquid
Al2W
bcc
Al7W3
Al
Al4W
fcc
Al12W
Al5W
Al77W23
W (mole fracon)
Fig. 1. Phase diagrams of the systems: (a) TiAl [68], e(l) = Al3Ti; and (b) AlW [69].
1124
0.5 vol% WC
1.0 vol% WC
Fig. 2. Microstructures of the cast composites (backscattered electron-BSE mode). Isolated and clustered carbide particles are noted by arrows and circles/ellipses,
respectively.
Al3Ti
Al3Ti
Al3Ti
Al3Ti
Fig. 3. Intermetallic compound particles observed in the TiCp/Al materials (a & b: Secondary Electron-SE mode, c: BSE mode). Spot EDX analyses in (at%): (a) spectrum 8:
76.97 Al-23.03 Ti, spectrum 9: 76.89 Al-23.11 Ti, spectrum 10: 75.97 Al-24.03 Ti, spectrum 11: 76.56 Al-23.44 Ti; (b) spectrum 18: 76.16 Al-23.84 Ti, spectrum 19: 76.06 Al23.94 Ti, spectrum 20: 76.68 Al-23.32 Ti; (c) Al3Ti formation associated with TiC nanoparticles (in circle).
The origin of the Al3Ti formation can be twofold: (a) due to reaction between K2TiF6 and molten Al [72,73] and (b) due to reaction
between molten Al and TiC. Taking into account the TiAl (Fig. 1a)
and AlC phase diagrams, the following reactions may account for
the presence of Al3Ti particles in the TiCp reinforced materials:
At the temperature of the melt (830 C):
1125
1126
0.5 vol% WC
0.5 vol% WC
Al3Ti
Al5W
Al3Ti
WC
Al3Ti
Al3Ti
Al12W
1.0 vol % WC
Al3Ti
Al5W
Al3Ti
WC
Al5W
Fig. 4. Intermetallic compound particles observed in the WCp/Al materials (SE mode). Spot EDX analyses in (at%): (a) spectrum 12: 91.73 Al-7.64 W-0.63 Ti, spectrum 13:
76.01 Al-18.47 Ti-5.52 W, (b) spectrum 29: 83.88 Al-15.55 W-0.57 Ti, and (c) spectrum 2: 75.44 Al-19.05 Ti-5.51 W, spectrum 3: 75.23 Al-18.95 Ti-5.82 W, spectrum 5: 83.86
Al-15.03 W-1.11 Ti.
Al-1.0 vol% WC
Al-0.5 vol% WC
30
25
Al1050
20
15
10
5
0
200
400
600
800
1000
1200
Fig. 6. (a) Mass loss versus sliding distance during dry ball-on-disk testing, for Al
1050, monolithic and reinforced by TiC and WC submicron particles; (b) the wear
rate of the different materials.
1127
1128
monolithic
valley
hill
valley
hill
hill
valley
0.5 vol% WC
1.0 vol% WC
hill
valley
valley
hill
Fig. 7. Panoramic views of the wear track morphologies of the monolithic alloy and the different composites produced (SE mode), illustrating the hill-valley landscape.
1.0 vol% WC
Al
Al
O
Ti
Fig. 8. Wear track morphologies in BSE mode and EDX spectra from hill (dark contrast) areas. (a) and (c) Al-1.0 vol% TiC and EDX spectrum from a hill, respectively; (b) and
(d) Al-1.0 vol% WC and EDX spectrum from a hill, respectively.
1129
monolithic
0.5 vol% WC
Fig. 9. Wear track morphologies of different materials produced (SE mode), illustrating a high extent of plastic deformation for the monolithic alloy and the formation of ne
and dense grooves on the wear surface of the AMCs.
monolithic
0.5 vol% WC
Al
O
W
Fig. 10. (a)(c): Crack formation in oxide layer areas (SE mode); (d) EDX analysis in the vicinity of the cracks revealing Al-based oxide presence (Al-0.5 vol% WC).
Figs. 9a and b, Fig. 10c with Figs. 10a and b). This observation is
compatible with the relatively extensive (ne and dense) grooving
along the wear track of the WC-reinforced alloy (compare Fig. 9c
with Figs. 9b and a).
EDX analysis of debris particles from the wear surface of the
WC reinforced alloy (Fig. 11a) revealed two types of materials:
(a) bright contrast particles of high W content (e.g. spectra 13
and 15) and darker contrast oxide particles of relatively low W
content (spectra 14, 16). It is indicated that the former ones
originated from oxidized broken particles of W-aluminides (most
1130
Al
1.0 vol% WC
Spectrum 13
W
W
Al
Spectrum 16
Ti
Spectrum 8
Ti
Fig. 11. Debris particles on the wear surface of the AMCs. (a) 1.0 vol% WC reinforced alloy and EDX spectra of brighter contrast particles (Spextrum13) and darker contrast
particles (Spectrum16); and (b) 1.0 vol% TiC reinforced alloy and EDX analysis from a debris particle (spectrum 8).
1131
1500
(v) The abrasive action of debris (TiCp/Al: oxides mostly originating from the matrix; WCp/Al: oxides originating from
mixtures of Al matrix and W-, Ti- aluminides and oxides
originating from fragments of large Al12W particles) caused
the formation of shallow, ne and dense grooves along the
wear tracks.
1000
500
0
-500
-1000
-1500
-2000
0.00001
0.0001
0.001
0.01
0.1
10
100
10
100
10
100
10
100
1500
1000
500
0
-500
-1000
-1500
-2000
0.00001
0.0001
0.001
0.01
0.1
1500
1000
500
0
-500
-1000
-1500
-2000
0.00001
0.0001
0.001
0.01
0.1
1000
500
0
-500
-1000
-1500
-2000
0.00001
0.0001
0.001
0.01
0.1
1132
-300
AlFe or Al and AlFeSi (even with the lm on the intermetallic phase), localized dissolution of the anodic Al (in or
adjacent to the eutectic microconstituent) occurred and
small pits were formed.
(3) As the pits were getting deeper, differential aeration cells
were formed between the bottom of the pits and the pit
walls.
(4) Pitting was evolved to intergranular corrosion at the boundaries where the Al-Fe intermetallics exist.
-500
-700
-900
-1100
-1300
-1500
-1700
0.0001
Forward Al 1050
Forward Al-1.0 vol%TiC
Forward Al-1.0 vol%WC
0.001
0.01
0.1
10
-300
-500
-700
-900
-1100
-1300
-1500
-1700
0.0001
(a) The fact that corrosion was mainly associated with the intergranular iron aluminide phase (a feature of the monolithic
alloy), whilst features associated with the carbide reinforcement have remained essentially free of corrosion traces support the claim deriving from the similar polarization
behaviour in Fig. 12 and formulated in Section 3.3.1: the
corrosion behaviour of the tested materials was mainly
controlled by the corrosion of the monolithic alloy.
(b) The only notable evidence of corrosion associated with the
reinforcement is the anodic dissolution of Al around A12W
indicating a cathodic role for the large surface of Al12W
particles. This evidence correlates well with the relatively
high cathodic currents recorded during polarization of the
WC reinforced AMCs (in comparison with the TiC-AMCs,
Forward Al 1050
Forward Al-0.5 vol%WC
Forward Al-1.0 vol%WC
0.001
0.01
0.1
10
1.0 vol% WC
1.0 vol% WC
1.0 vol% WC
Fig. 14. SEM micrographs of AMCs after cyclic polarization in DHS, 25 C (cross-sections). (a) and (b): extensive intergranular corrosion associated with the AlFe/Al and
AlFeSi/Al eutectic microconstituent; (c) evidence that Al12W particles have acted as cathodic surfaces. (d) WC & aluminide clusters and their matrix appear corrosion-free.
Black outlined ellipses: intergranular clusters of aluminides (Al5W, Al3Ti)/carbides and their matrix have remained free of corrosion signs. White arrows: aluminide (Al5W,
Al3Ti) and carbide clusters have acted as physical barriers to IC progress. White outlined ellipses: clusters of aluminides/carbides and their matrix have remained free of
corrosion signs.
Fig. 12a and d and Fig. 13a) and the 1.0 vol% WC-AMC (in
comparison with the 0.5 vol% WC-AMC, Figs. 12c and 13b).
According to Birbilis and Buchheit [94], the size of intermetallic particles plays an important role on the kinetics of
cathodic reactions, as this will govern the amount of current
the intermetallic can support.
1133
Acknowledgements
It should also be noted, that although clusters of aluminide particles and carbide nanocores do not appear to have acted as cathodic sites (even in the case of large surface area occupation, as in
Fig. 14ac), it is reasonable to assume that the entire volume of
high conductivity may have also contributed a cathodic inuence
on the matrix in compatibility with Deuis et al. [95].
The above observations suggest that the matrix/primary reinforcement interface was not the main factor in the corrosion
behaviour of these composites. The fact that the Al/WC and the
Al/TiC interfaces have remained unaffected in conjunction with
the sliding wear response, indicate the existence of clean and
strong reinforcement-matrix interfaces.
4. Conclusions
Aluminium Matrix Composites (AMCs) were produced by the
addition of sub-micron sized WC and TiC particles (61.0 vol%) into
a melt of Al1050. Casting was assisted by the employment of K2TiF6
as a wetting agent and mechanical stirring. The main conclusions
drawn from the study of the microstructure, wear performance
and corrosion performance of the cast materials are:
The AMC contained two main types of reinforcement: (a) in-situ
Al3Ti and (Al5W + Al12W + Al3(Ti,W)) intermetallic particles in
the cases of TiCp-AMC and WCp-AMC, respectively; (b) carbide
nanoparticles, as such, or more often as clusters of carbide
nanocores and aluminide particles.
Particle distribution was considered as reasonably uniform
comprising both clusters and isolated particles. Carbide nanocores, in clusters with aluminides or isolated were mainly
located at grain boundaries and the areas of the lastly solidied
liquid.
The sliding wear performance of the alloy was markedly
improved by the addition of the carbide phase through a direct
effect stemming from the TiC and WC particles, as such and as
clusters with intermetallic phase, and an indirect effect originating from the intermetallic hard particles.
WCp-AMCs presented higher wear resistance than TiCp-AMCs.
A wear mechanism was formulated including four steps: (a)
plastic deformation of the Al-matrix leading to a repeated
hill-valley morphology of the wear surface; (b) formation
of surface alumina based oxide layers due to frictional heating; (c) crack formation due to friction, fatigue and brittleness
of the oxide surface layers; (d) ne groove formation along
the sliding direction. The wear mode was characterized as
mild.
The corrosion behaviour of the reinforced materials in DHS,
at 25 C, was mainly controlled by the corrosion of the
alloy matrix. As such, the predominating form of corrosion
was intergranular corrosion (IC) of Al in the Al/iron aluminide eutectic microconstituent or adjacent to the grain
boundaries.
Features associated with carbide reinforcement (clusters of
aluminide and carbide nanoparticles) along with their Almatrix have remained intact of corrosion, whilst in several
cases, they have acted as physical barriers to the IC progress.
However, a cathodic action of large Al12W particles was
observed.
1134
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