1

Preparation and Characterization of 7075

Aluminum Alloy Reinforced with Nano
Particles of Alumina





A Thesis
Submitted To College of Engineering
Alnahrain University in a Partial Fulfillment
Of the Requirements for the Degree of Master Science
In
Mechanical Engineering





By:
Ibrahim Rahman Ibrahim
(B.Sc. 2006)




Thi Al Qida 1434
September 2013
2



Chapter One
Introduction
1.1 Background
The first focused efforts to develop Metal-Matrix Composites MMC's
originated in the 1950s and early 1960s. The principal motivation was to
dramatically extend the structural efficiency of metallic materials while retaining
their advantages, including high chemical inertness, high shear strength, and good
property retention at high temperatures. Early work on sintered aluminum powder
was a precursor to discontinuously reinforced MMCs. The development of high-
strength monofilamentsfirst boron and then silicon carbide (SiC)enabled
significant efforts on fiber-reinforced MMCs throughout the 1960s and early 1970s.
Issues associated with processing, fiber damage, and fiber-matrix interactions were
established and overcome to produce useful materials. Although these were very
expensive and had marginal reproducibility, important applications were
established, including 243 structural components on the space shuttle orbiters.
Recession in the early 1970s produced significant research and development
funding cuts, leading to an end of this phase of MMC discovery and development.
In the late 1970s, efforts were renewed on discontinuously reinforced MMCs using
SiC whisker reinforcements. The high cost of the whiskers and difficulty in
avoiding whisker damage during consolidation led to the concept of Particulate
reinforcements. The resulting materials provided nearly equivalent strength and
stiffness, but with much lower cost and easier processing. A renaissance in both
discontinuous and fiber-reinforced MMCs continued through the 1980s. Major
efforts included particle-reinforced, whisker-reinforced, and tow-based MMCs of
aluminum, magnesium, iron, and copper for applications in the automotive, thermal
management, tribology, and aerospace industries. In addition, monofilament-
3


reinforced titanium MMCs were developed for high-temperature aeronautical
systems, including structures for high-mach airframes and critical rotating
components for advanced gas turbine engines. Significant improvements in
performance and materials quality were matched by an increasing number of mostly
small businesses that were specialized in the production of MMC components for
target markets.
In the early 1990s, a U.S. Air Force Title III program provided a significant
investment to establish an MMC technology base for the aerospace industry in the
United States. This program produced several landmark military and commercial
aerospace applications of discontinuously reinforced aluminum (DRA). In addition
to these dramatic successes, new MMC insertions in the ground transportation,
industrial and thermal management electronic packaging industries far exceeded the
growth in the aerospace industry. Thus, the insertion of new materials in military
and commercial aircraft has actually lagged behind the industrial sector, reversing
the trend of earlier years for the insertion of new materials. The MMC market for
thermal management and electronic packaging alone was five times larger than the
aerospace market in 1999, and this gap is expected to increase in the coming years,
due to aggressive growth in the ground transportation and thermal management
markets [1].
For many researchers the term metal matrix composites is often equated with the
term light metal matrix composites (MMCs).Substantial progress in the
development of light metal matrix composites has been achieved in recent decades,
so that they could be introduced into the most important applications. In traffic
engineering, especially in the automotive industry, MMCs have been used
commercially in fiber reinforced pistons and aluminum crank cases with
strengthened cylinder surfaces as well as particle-strengthened brake disks. These
innovative materials open up unlimited possibilities for modern material
science and development; the characteristics of MMCs can be designed into the
material, custom-made, dependent on the application. From this potential, metal
matrix composites fulfill all the desired conceptions of the designer. This material
4


group becomes interesting for use as constructional and functional materials, if the
property profile of conventional materials either does not reach the increased
standards of specific demands, or is the solution of the problem. However, the
technology of MMCs is in competition with other modern material technologies, for
example powder metallurgy. The advantages of the composite materials are only
realized when there is a reasonable cost performance relationship in the
component production. The use of a composite material is obligatory if a special
property profile can only be achieved by application of these materials. The
possibility of combining various material systems (metal ceramic nonmetal)
gives the opportunity for unlimited variation. The properties of these new materials
are basically determined by the properties of their single components [2].

1.2 Metal Matrix Nanocomposites

Metal matrix composites (MMCs) such as continuous carbon or boron fiber
reinforced aluminum and magnesium, and silicon carbide reinforced aluminum
have been used for aerospace applications due to their lightweight and tailorable
properties. There is much interest in producing metal matrix nanocomposites that
incorporate nanoparticles and nanotubes for structural applications, as these
materials exhibit even greater improvements in their physical, mechanical and
tribological properties as compared to composites with micron-sized
reinforcements. The incorporation of carbon nanotubes in particular, which have
much higher strength, stiffness, and electrical conductivity as compared to metals,
can significantly increase these properties of metal matrix composites.
Nanocomposites are being explored for structural applications in the defense,
aerospace and automotive sectors. Concurrent with the interest in producing novel
nanocomposites materials is the need to develop low cost means to produce these
materials. Most of the prior work in synthesizing nanocomposites involves the use
of powder metallurgy techniques, which are not only high cost, but also result in the
5


presence of porosity and contamination. Solidification processing methods, such as
stir mixing, squeeze casting and pressure infiltration are advantageous over other
processes in rapidly and inexpensively producing large and complex near-net shape
components, however, this area remains relatively unexplored in the synthesis of
nanocomposites. Stir mixing techniques, widely utilized to mix micron size
particles in metallic melts, have recently been modified by dispersing small volume
percentages of nanosize reinforcement particles in metallic matrices. Although there
are some difficulties in mixing nanosize particles in metallic melts resulting from
their tendency to agglomerate, a research team in Japan has published research on
dispersing nanosize particles in aluminum alloys using a stir mixing technique.
Researchers at the Polish Academy of Science have recently demonstrated the
incorporation of greater than 80 volume percent nanoparticles in metals using high-
pressure infiltration with pressures in the GPa range. Composites produced by this
method possess the unique properties of nanosize metallic grains.
Recently, metal matrix nanocomposites were synthesized at the University of
Wisconsin, Milwaukee using aluminum alloy A206 and nanoparticles of alumina
(Al
2
O
3
).TEM samples of the cast Al-A206/Al
2
O
3
clearly show nanoparticles present
within the metal matrix (Figure 1.1). SAD patterns show the pattern of the matrix as
well as the nanoparticles (Figure 1.2). EDX indicates that the grains are composed
of aluminum, which contains nanosize alumina particles. The distribution of
particles throughout the grains of the matrix with an absence of large concentrations
at the grain boundaries suggests wetting of the alumina by the liquid metal. In this
case the nanoparticles did not appear to act as nucleation sites for nanosized grains
[3].

1. 3 Material Used to Reinforce Aluminum Alloys
The most common DRMMC materials systems used for current aerospace structural
applications are silicon carbide (SiC) and boron carbide (B4C) particulate
reinforcement in an aluminum alloy matrix. Aluminum oxide particles are a lower
6


cost alternative most commonly used for casting applications. Titanium carbide is
being investigated for high-temperature applications [1].
Among the ceramic reinforced materials, SiC is the most common used in MMCs.
The second most used reinforcement is Al
2
O
3
. Compared with SiC it is more stable
and inert and has better corrosion and high temperature resistance. The influence of
these reinforcements to aluminum alloys has been the subject of a significant
amount of research work [5].
Because of its extreme hardness and temperature resistant properties, Al
2
O
3
ceramic
particles are often used as reinforcement within the aluminum matrix. This type of
composite is more frequently used in the automotive industry today, particularly in
various engine components as well as brakes and rotors [2].

1.4 Stir Casting

Melting metallurgy for the production of MMCs is at present of greater technical
importance than powder metallurgy. It is more economical and has the advantage
of being able to use well proven casting processes for the production of MMCs.For
melting metallurgical processing of composite materials there are three procedures
mainly used :
compo-casting or melt stirring
gas pressure infiltration
squeeze casting or pressure casting.

Both the terms compo-casting and melt stirring are used for stirring particles into
a light alloy melt .The particles are often tend to form agglomerates, which can be
only dissolved by intense stirring[2]. Out of the available methods of producing
these composites, Stir casting route is most promising and economical for
synthesizing the particle reinforced AMCs and is not only simple, but is easy to
obtain shape castings[6].
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Among discontinuous metal matrix composites processes , stir casting is generally
accepted as a particularly promising route, currently practiced commercially. Its
advantages lie in its Simplicity, flexibility and applicability to large quantity
production. It is also attractive because, in principle, it allows a conventional metal
processing route to be used, and hence minimizes the final cost of the product. This
liquid metallurgy technique is the most economical of all the available routes for
metal matrix composite production, and allows very large sized components to be
fabricated. The cost of preparing composites material using a casting method is
about one-third to half that of competitive methods, and for high volume
production, it is projected that the cost will fall to one-tenth . In general, the
solidification synthesis of metal matrix composites involves producing a melt of the
selected matrix material followed by the introduction of a reinforcement material
into the melt, obtaining a suitable dispersion [7].
However, stir casting has inherent problems such as good wetting between the
particulate reinforcement and the liquid aluminum alloy melt. Moreover the
problem with finer reinforcement particles especially nano particles would be
agglomeration. If these challenges could be overcome, then stir casting would be a
commercially viable technology for producing AMCs especially nano particle
reinforced AMCs. A few researchers have made attempts to develop stir casting
setup that can overcome these problems and they have been quite successful. Most
of the researchers have focused on using micron sized reinforcement particles and
not much research has been done using nano size reinforcement particles.
Hashim et al., have identified four technical difficulties in stir casting: difficulty of
achieving a uniform distribution of the reinforcement material; wettability between
the two main substances; porosity in the cast metal matrix composites; and chemical
reactions between the reinforcement material and the matrix alloy. These difficulties
need to be overcome in order achieve a MMC with a broad range of mechanical
properties. They have also identified the important process variables that affect the
mechanical properties of MMC. The holding temperature, stirring speed, size of the
8


impeller and the position of the impeller in the melt are to be considered in the
production of cast metal matrix composites (quoted in 8).



Figure 1-1 Schematic showing the mechanical stirring device used in the vortex technique of
dispersing particles in melts [9].



Objective of this study

The aim of this study is to prepare and characterize the 7075alluminum alloy after
reinforcing it by alumina nano powder based on stir casting technique taking into
consideration the following :

1- Investigation into the improvement in mechanical properties of 7075 Aluminum
alloy reinforced with 20 nm alumina particles.
2- Obtaining best result from wt. % of reinforcement within 0.5%, 1.0% and 1.5%
wt. fraction of alumina particle as a reinforcement in Aluminum metal matrix.
3- Pointing out to utilization of addition of particles by capsules and how suitable it
is with stir casting technique to get regular distribution in the structure of the
AMC.


9


Chapter Two
Literature Survey
2.1 Introduction
Many studies dealt with synthesizing and composing metal matrix composites .
Next studies which will be surveyed are focusing on preparation of MMC's,
especially AMC's reinforced by ceramic particles and nano particles . Different
techniques had been experimented as a route of formation and preparation of
MMC's For example: mechanical alloying, ultrasonic ,In situ ,stir casting and
powder metallurgy . The Following researches are surveyed:
2.2 Metal Matrix Composites
Tong and Ghosh, 2001[10] : evaluated high-strength Al-Si/TiC and the
elevated temperature-resistant Al-Fe(-V-Si)/TiC composites . The microstructural
characteristics of ingot metallurgy (IM) or rapid solidification (RS) Al-Si/TiC and
Al-Fe(-V-Si)/TiC composites could be thought of as a combination of the related
alloy matrix microstructures and the IM or RS Al/Tic composites. Included Orowan
strengthening, grain-size and substructure strengthening, and solid-solution
strengthening. Used RS technique, fine, uniform particle size distribution; a high
interfacial strength; control of particle shape; and a ductile matrix to maximize
strength and ductility for particular volume fraction, and influence the degree of
flexibility available.

Kim, et al, 2001[11]: described the optimum condition for synthesis of
Al2O3/Cu nanocomposites. Discussed the effects of Cu dispersion on the
microstructure and fracture toughness. Concluded that Al
2
O
3
/Cu nanocomposites
can be fabricated by a controlled powder preparation and sintering process with a
relatively simple and cost-effective method. Successfully synthesized the
11


nanocomposites powders with crystallite size of about 25 nm by a high-energy ball
milling process. Sintered the composites at 1250C for 5 min which showed a
relative density above 97% and enhanced fracture toughness of 4.51 MPa.m1/2.
Microstructural observation of the sintered composites\revealed that the nano-sized
Cu particles are uniformly distributed and situated on the grain boundaries of Al
2
O
3

matrix.

Koch , 2003[12] :reviewed the 'top-down 'methods for synthesis of nano
structured or submicron grain size material which utilize sever plastic deformation
along with thermal process. Of the variety methods he discussed , appeared that
only ball milling ,high pressure torsion and accumulative roll bonding can regularly
produce average grain size below100nm .By examples of combining conventional
deformation methods with annealing ,showed the possibility of forming
nanocrystalline/submicrom grain sizes that can optimize mechanical properties in
practical ways .

Miyajima and Iwai ,2003[13] : investigated effects of reinforcements on
the wear behavior of aluminum matrix composites by pin-on-disk tests. The matrix
materials were 2024 and ADC12 aluminum alloys. The volume fractions of SiC
whiskers (Vfw) were 529% (MMCw), Al
2
O
3
fibers (Vff ) were 326% (MMC
f
),
and SiC particles (Vfp) were 210% (MMCp). The MMCs were rubbed against a
carbon steel pin under a load of 10N at a sliding velocity of 0.1ms1. The degree of
improvement were investigated By summarizing the results, they concluded that
particles are most beneficial for improving the wear resistance of MMC.

Bajaj ,2004[14]: His work focuses on the study of the behavior of Aluminum
cast alloy (LM6) with SiC and AL
2
O
3
composites produced by the stir casting
technique .Different % age of reinforcement were used .Tensile test ,hardness test,
impact test were performed on the samples obtained by the stir casting process.X-
11


ray diffraction was performed to find the presence of the phases of reinforcement
material .SEM was done to find the distribution of the SiC/Alumina particles in
Aluminum alloy . He concluded that stir casting ,stirrer design and position ,stirring
speed and time, particle preheating an temperature ,particle incorporation rate .etc.
are the important process parameters.

Xia, et al, 2005[15]: studied the structural evolution of an Al/BN mixture
during mechanical alloying (MA) using a planetary ball mill systematically. The X-
ray diffraction (XRD) patterns showed that the diffraction peaks of hexagonal boron
nitride (h-BN) disappeared. Characterization of the milled samples was also carried
out by means of differential scanning calorimetry (DSC), Fourier transform infrared
spectroscopy (FTIRS), and scanning electron microscopy (SEM). Experimental
results revealed that most h-BN gradually decompose into boron and nitrogen
atoms as MA proceedes . They conclude that no new phase is formed directly
during MA from Al/BNmixture in our experiments, but AlN and AlB2 are formed
when the milled samples were annealed at 773K for 2 h. AlN and AlB2 deposited
out from the solid solution of AlBN during annealing.

Hassan and Gupta, 2005 [16]: fabricated magnesium based composites
with three different volume percentages of nano-sized Al
2
O
3
particulates
reinforcement using blend-press-sinter methodology avoiding ball milling.
Microstructural characterization of the materials revealed reasonably uniform
distribution of nano size Al
2
O
3
reinforcement and presence of minimal porosity.
Mechanical properties characterization revealed that the presence of nano-Al
2
O
3

particulates as reinforcement leads to a simultaneous increase in hardness, elastic
modulus, 0.2% yield strength, UTS and ductility of pure magnesium. The results
reveal that the 0.2% yield strength, UTS and ductility combination of the
magnesium nanocomposites containing 0.66 and 1.11 vol.% of alumina remained
higher when compared to high strength magnesium alloy AZ91 reinforced with
12


much higher amount of micrometer size SiC particulates. An attempt is made in the
present study to correlate the effect of presence of nano-Al
2
O
3
as reinforcement and
its increasing amount with the microstructural and mechanical properties of
magnesium.

Kurzydlowski, 2006[17]: studied the microstructure and mechanical
properties of nanomaterials (Al, Al-alloys, Cu, Ni, Ti, and stainless steel) and
nanocomposites (Al
2
O
3
/ Ni P) by the methods of transparent and scanning
electron microscopy, X-ray diffraction analysis, and micro hardness and tensile
tests. The experimental methods included the procedures of measuring the electric
and corrosion resistances. Prepared the materials a by using contemporary methods,
namely, by hydrostatic extrusion (nanometals) and by sintering ceramic powders
covered with NiP nanoparticles under high pressure by using the procedure of
nonelectric chemical metallization (Al
2
O
3
/ Ni P nanocomposites).

Espinoza, et al 2007[18]: studied the microstructure, electrical conductivity
and hot softening resistance of two alloys (G-10 and H-20), projected to attain Cu
2.5 vol.% TiC2.5 vol.% Al
2
O
3
nominal composition, and prepared by reaction
milling and hot extrusion. The alloys were characterized by many analysis
techniques. They concluded that the H-20 alloy is a good candidate
for engineering applications at high temperature.

Tavoosi , et al 2007[19]: investigated fabrication and characterization of
alumina particles reinforced aluminum-based metal matrix nanocomposite by
mechanical alloying. Aluminum and zinc oxide powders mixture were milled by a
planetary ball mill in order to produce Al13.8 wt.% Zn/5 vol. % Al
2
O
3

nanocomposite. The structural evaluation milled and annealed powders were
studied by X-ray diffraction, SEM observation and hardness measurement. The
aluminum crystallite size was estimated with broadening of XRD peaks by
13


WilliamsonHall formula. The results show that milling of aluminum and zinc
oxide for 60 h leads to displacement reaction of the zinc oxide and aluminum to
produce Zn and Al
2
O
3
phases. The milled powder had a microstructure consisting of
nanosized Al
2
O
3
particles in an AlZn solid solution with a nanoscale grain size of
40 nm. Micro hardness of this nanocomposite was found to be about 190 HV.

Eschbach, et al 2007[20]: presented the fabrication and characterization of
nanocomposite materials based on crystalline nanoparticles dispersed in an
oligomer matrix . Two types of nanoparticles were used. They described the
nanocomposites fabrication process and underlined the dispersion step and the
problems inherent to clusters destruction. Explored Mechanical properties of the
nanocomposites based on Al
2
O
3
by Brillouin spectroscopy. An enhancement of the
Young's modulus was observed with a very weak mass percentage of nanoparticles
(3%). . This result is of great importance in order to achieve piezoelectric and
ferroelectric applications.

Ahmad, et al 2007[21]: report the effect of weight percentage on the
microstructure and properties of alumina particle reinforced aluminum metal matrix
composite and the microstructure, bulk density and hardness value of the
composites . They concluded that the production of Al
2
O
3
particle reinforced
aluminum matrix composites in the form of net shape component can be achieved
by use of conventional P/M route, cold uniaxial pressing and sintering processing
technology. The hardness values and density of the composites increase with the
increasing percentage of Al
2
O
3
.

Rafaja, et al 2007[22]: illustrate the capability of the combination of the X-
ray diffraction and the transmission electron microscopy for the Microstructure
investigations on thin film and bulk nanocomposites of three experimental
examples: two Cr-Al-Si-N coatings with different chemical compositions and one
14


BN bulk nanocomposites. They used a modified kinematical diffraction theory that
describes and explains the phenomenon of the partial crystallographic coherence of
crystallites, they could show that the analysis of the X-ray diffraction line
broadening is able to reveal nanocrystalline domains organized in semi-coherent
clusters, to determine the size of the nanocrystalline do mains and the clusters, and
to quantify the mutual orientation of the partially coherent crystallites within these
clusters.


Ren , 2007[23]: The aim of his project was to fabricate SiC (50nm)/7075
aluminium composites via a modified powder metallurgy and extrusion
route.Ageing treatment was used to increase the strength of the composites and
mechanical tests, including tensile test and abrasive wear test. He studied the
effects of nanometric silicon carbide particulates to the ageing behaviors and
mechanical properties of the composites by optical metallography, scanning
electron microscopy and transmission electron microscopy. He found that the
dispersion of nanometric silicon carbide is not homogeneous, but tends to disperse
along grain boundaries. He also found that of these nano-reinforcements cluster
within the grains. He concluded the addition of a small amount of SiC
nanoreinforcements has a high potential to further strengthen 7xxx aluminum alloy.
He suggested that by improving the dispersion of nanometric reinforcements, as
well as putting in reinforcements with different sizes, the mechanical properties and
wear resistance can both be increased.
Reddy, et al 2008[24]: prepared aluminum-based metal matrix composites
reinforced with in situ Al3Ni and Al
2
O
3
hybrid reinforcements prepared by the
mechanically activated, self-propagating, high temperature synthesis (MASHS).
They demonstrated that the composite properties can be tailored by altering the
stoichiometry of reactants and concluded that the formation of different types of
nickel aluminides depending on the excess aluminum demonstrates the
compositional versatility of the MASHS process. Results they obtained have a
15


good agreement with the thermodynamic predictions of the displacement reaction
between aluminum and NiO. This can be utilized for the in situ synthesis of the
composite materials of AlAl
2
O
3
AlxNiy system at the processing temperatures
where the nanostructure is retained successfully.


Lin, et al 2008[25]: fabricated nanostructured metal matrix composites
(NMMCs) in large-dimension billets by hot isotactic pressing (HIPing) of
cryomilled powders consisting of AA2024 alloy reinforced by 25 wt.% SiC
particles and concluded that the presence of micro-voids/porosity in the large bulk
billet is believed to be the failure source leading to a less strengthening effect
anticipated from the grain refinement in nanometer to sub-lm scale. Further
optimization of consolidation process and/or using a proper secondary consolidation
process such as extrusion or forging would further improve the strength.

Mula, et. al. 2009[26]: investigated the structure of an ultrasonically cast
nanocomposite of Al with 2 wt.% nanosized Al
2
O
3
(average size _10 nm)
dispersoids and showed that the nanocomposite consists of nearly continuous nano-
alumina dispersed zones (NDZs) in the vicinity of the grain boundaries
encapsulating Al
2
O
3
depleted zones (ADZs ) and the mechanical properties by
nanoindentation and tensile tests . They found that The nano-sized dispersoids
causes a marginal increase in the elastic modulus, and a significant increase in the
hardness (~92%), and tensile strength (~48%).
Li, et al 2009[27]: investigated systematically the microstructural origins and
the strengthening mechanisms, including HallPetch, Orowan and Taylor, as
appropriate to each phase constituent and calculated overall strength using rule-of-
mixtures.They modified shear-lag model, and MoriTanaka method to provide
insight into the relative contributions of above mentioned mechanisms.

16


Singla, et al 2009[7]: attempted to develop aluminum based silicon carbide
particulate MMCs with the objective to develop a conventional low cost method of
producing MMCs and to obtain homogenous dispersion of ceramic material. Two
step-mixing method of stir casting technique and subsequent property analysis had
been made to achieve these objectives. They chose aluminum (98.41% C.P) and SiC
(320-grit) as matrix and reinforcement material respectively. Experiments were
conducted by varying weight fraction of SiC (5%, 10%, 15%, 20%, 25%, and 30%),
while keeping all other parameters constant. Their results indicated that the
developed method is quite successful to obtain uniform dispersion of
reinforcement in the matrix. They observed an increasing trend of hardness and
impact strength with increase in weight percentage of SiC.

Flores-Campos, et al 2010[28]: prepared composites of 7075 aluminum
alloy (Al7075) with carbon-coated silver nanoparticles (Ag-C NP) by the
mechanical milling process and found that Ag-C NP has an effect on refining the
powder and in the crystal size. The Vickers microhardness (HVN) values were
higher at higher Ag-C NP contents and a saturation point exists where
microhardness does not present variation. They concluded that concentrations
higher than 2wt.% do not have an important effect on microhardness.

Wang, et al 2010[29]: fabricated In situ formation of Al
2
O
3
SiO2SnO2
composite ceramic coating on Al20%Sn alloy in aqueous Na2SiO3 electrolyte by
microarc oxidation technology successfully and studied in detail the compositions,
structure, mechanical and tribological properties of the composite by scanning
electron microscope, energy dispersive spectroscopy, X-ray diffraction, hardness
tester and ball-on-disc friction tester. They found that the species originating from
the Al20%Sn alloy substrate and the electrolyte solution both participate in
reaction and contribute to the composition of the coating, which results in the
generated coating firmly adherent to the substrate. They conclude that considering
17


the convenience on preparation and attractive performance acquired in the final
products, the Al
2
O
3
SiO2SnO2 composite coating could be a promising way to
extend the applications of AlSn alloy in industry.

Khorshid, et al 2010[30]: prepared aluminum matrix composites reinforced
by two sizes of alumina particles (35 nm and 0.3 lm) wet attrition milling and hot
forward extrusion processes and evaluated the effect of the ratio of the nano- to
submicron-sized particles (2:8, 3:7, 4:6, 5:5, and 6:4 in weight percent) on
mechanical properties of the composites by micro-hardness and tensile tests. They
found that by increasing the nanoparticles content, the hardness and strength of the
composites first increase and then decrease when the amount of the nanoparticle
exceeds 4 wt.%. The tensile fracture surfaces are also observed by scanning electron
microscopy.

Monazzah , et al 2010[31]: produced alumina dispersion strengthened
aluminum powder by mechanical milling of a commercial gas-atomized aluminum
powder in a planetary ball mill under an argon atmosphere for 12 h. They explained
the creep behavior according to the invariant substructure model and dislocation
glide process and concluded that the nanometric alumina particles actively pin the
substructure and limit the deformation of the aluminum matrix.

Mirzadeh and Zomorodian , 2010[32]: modeled the effects of the
annealing temperature and time, cryomilling in liquid nitrogen, and the addition of
aluminum powder on the thermal stability and grain growth behavior of
nanocrystalline iron using the Artificial Neural Network (ANN) technique .The
developed model can be used as a guide for the quantification of the grain growth
by considering the effects of annealing temperature and time. The model also
quantifies the effect of Al on the thermal stability of cryomilled nanocrystalline Fe.
18


The model results show that the cryomilling of Fe has a tangible effect on the
stabilization of the nanostructure.

Hoobi, et al 2011[33]: studied some of mechanical properties such as Brinell
hardness (BHN) and compression strength of aluminum matrix composite material
that reinforced was by (3, 6 , 9 , and 12 wt.% ) Al
2
O
3
particles. Powder technology
technique was used in samples prepared. Their result show that an advancement in
the Brinell hardness (BHN) and compression strength especially at 12 wt.% - Al
2
O
3
.
The development in the Brinell hardness (BHN) and compression strength were
found to reach 89% and 54% respectively from the initial properties of unreinforced
aluminum samples.

Zhang, et al 2011[34]: fabricated in situ Al composites by selection of Al and
TiO2 powders via multiple pass friction stir processing (FSP) based on the
thermodynamic analysis. The microstructural investigations indicate FSP would
induce reaction between Al and TiO2. Al3Ti and Al
2
O
3
. Tensile tests indicate that
the in situ nanocomposites exhibits pronounced work hardening behavior and a
good combination of strength and ductility.

Choi, et al 2011[35]: used an ultrasonic cavitation based dispersion technique
to fabricate Al-7Si- 0.3Mg alloyed with Cu and reinforced with 1 wt. pct. Al
2
O
3

nanoparticles, in order to investigate their influence on the mechanical properties
and microstructures of Al-7Si-0.3Mg alloy. They concluded that that the
combination of 0.5 pct. Cu and 1 pct. Al
2
O
3
nanoparticles results in a significant
increase in ultimate tensile strength (22 pct.). It is noticed that the ductility is
improved from 1.7 to 10.4 pct. (increased by 512 pct). The significant enhancement
of properties is attributed to the decrease in porosity (from 2.1 to 0.5 pct.) and
modification of eutectic Si phases due to the addition of Al
2
O
3
nanoparticles. The
enhancement of yield strength in T6 heat-treated Al-7Si-0.3Mg-0.5Cu-1 wt pct
19


Al
2
O
3
nanocomposite was limited by the reaction between Mg and Al
2
O
3

nanoparticles during the heat treating process.

Law, et al 2011[36]: analyzed the mechanical response of aluminum matrix
reinforced with nanosized silicon carbide using plane strain, discrete dislocation
plasticity. In the simulations, plasticity arises from the collective motion of
dislocations within an elastic medium. They prescribed constitutive rules for
nucleation, motion and annihilation of the dislocations. Performed calibration of
various parameters or quantities which affect these processes .The numerical results
show improvements in the mechanical strength of the nanocomposite material with
increasing particle volume fraction and decreasing particle size.

Mazahery and Ostadshabani 2011[37]: incorporated 0.75, 1.5, 2.5, 3.5,
and 5 vol.% of alumina nanoparticles into the A356 aluminum alloy by a
mechanical stirrer and then, cylindrical specimens were cast at 800_C and 900_C.
It was observed a uniform distribution of reinforcement, grain refinement of
aluminum matrix, and presence of the minimal porosity by microstructural
characterization of the composite samples. They reveal that the presence of nano-
Al
2
O
3
reinforcement leads to significant improvement in 0.2% yield strength and
ultimate tensile stress while the ductility of the aluminum matrix is retained.
Fractography examination shows relatively ductile fracture in tensile-fractured
samples.

Sajjadi, et al 2011[38]: used a novel three step mixing method in order to
improve the wettability and distribution of reinforcement particles within the
matrix. The process included heat treatment of micro and nano Al
2
O
3
particles,
injection of heat-treated particles within the molten A356 aluminum alloy by inert
argon gas and stirring the melt at different speeds. Investigated The influence of
various processing parameters such as heat treatment of particles, injection process,
21


stirring speed, reinforcement particle size and weight percentage of reinforcement
particles on the microstructure and mechanical properties of composites was studied
. The use of heat-treated particles, injection of particles and the stirring system
improved the wettability and distribution of the nano particles within the aluminum
melt. They revealed that the amount of hardness, compressive strength and porosity
increases as weight percentage of nano Al
2
O
3
particles increases.

Sivasankaran, et al,2011[39]: synthesized nanocrystalline AA 6061 alloy
reinforced with alumina (0, 4, 8, and 12 wt.%) in amorphized state composite powder by
mechanical alloying and consolidated by conventional powder metallurgy route. They
concluded that The lattice parameter of as milled powders is decreased with percentage of
reinforcement due to dissolution of some atoms in the Al lattice, whereas it is increased
with the percentage of reinforcement in the sintered pellets due to segregation of some
elements. elements. Their analysis can be used for understanding the stress and the strain
present in the nanocomposite through mechanical alloying.

Parvin and Rahimian, 2011[5]: investigated the influence of Al
2
O
3
particle size on the density, hardness, microstructure, yield stress, compression
strength, and elongation of the sintered AlAl
2
O
3
composites. They used 10 wt. %
of Al
2
O
3
powder with three different particle sizes (3, 12 and 48 m) in the
production of the samples. Results show that the relative density of the composite is
initially increased with decreasing particle size and pointed out that the mechanical
properties of the specimens is increased with decreasing particle size. The grain size
and particle distribution homogeneity is decreased with raising the particle size.


Suresh, et al 2011[8]: produced LM25 aluminum alloy metal matrix
composites (MMCs) reinforced with weight fractions of micro and nano Al
2
O
3
particles up to 10 wt. % by stir casting. The produced composites for their
mechanical properties such as hardness and tensile strength as well as for the
21


dispersion of the micro and nano Al
2
O
3
particles were characterized. Their results
reveal that stir casting could be an economical route for the production of nano
composites. Nano particle reinforced MMCs exhibit better hardness and strength
when compared to micro particles reinforced composites. Scanning electron
microscopic observations of the microstructures reveal that the dispersion of the
micron size particles is more uniform while nano particles lead to agglomeration of
the particles.

Hosseini, et al 2012[40]: investigated wear behavior of nanostructured
Al6061alloyand Al6061Al
2
O
3
nanocomposites produced by milling and hot
consolidation. They showed that Nanocomposites containing 3vol%Al
2
O
3
a had
maximum hardness of 235HV and optimum wear rate of 4x10
-3
mg/m. Increasing
the amount of Al
2
O
3
up to5vol%resulted in decreaseing hardness values(112
HV)and a sharp rise in wear rate(18 x10
-3
mg/m). It should be mentioned that in
best case, the relative density of nanostructured and nanocomposite samples was
9798% which is not high enough for industrial applications.

Murthy, et al 2012[41]: made an attempt to modify the micro sized fly ash
into nano structured fly ash using high energy ball mill. Produced Alfly ash nano
composites by ultrasonic cavitation route successfully. And found that as the
amount of nano fly ash is increasing the hardness of the composite also increass and
the nano fly ash addition leads to improvement in the compression strength of the
composites.

Flores-Campos, et al 2012[42]: produced nanostructured composites
of 7075 aluminum alloy and carbon coated silver nanoparticles by mechanical
milling and indirect hot extrusion. The experimental results demonstrate that the
Al7075AgC NP's nanostructured composites can be produced by mechanical
milling and subsequent hot-extrusion processes. Both milling time and silver
22


nanoparticles have a positive effect on the mechanical properties. It was observed
that the dispersion of the nanoparticles does not affect the ductility.

El-Daly, et al 2012[43]: used pulse echo overlap method (PEO) which is a
non-destructive technique for evaluating the mechanical properties of Al/SiC
nanocomposites. The nano-sized AI/SiC powders were prepared by mechanical
alloying method.It is concluded that mechanical alloying appears to be an ideal
method to synthesize nanocomposites in a variety of systems. And the elastic
moduli can be correlated well with the additions of SiC reinforcements in various
amounts to the Al matrix.

Deshmanya and Purohit, et al 2012[6]: presented the details of
developing a mathematical model to predict the tensile behavior like ultimate tensile
strength (UTS) and percentage elongation of the as-cast Al7075/Al
2
O
3
in terms of
size and % fraction of Al
2
O
3
, holding temperature and holding time; using factorial
design of experiments. Adequacy of the models was tested using Fishers F-test.
UTS of the composite were increased by 20%compared to that of matrix and %
elongation which was reduced by around 30%.


2.3 Summary

From the previously surveyed researches, It is clear that the MMC's, specially
AMC's are promising field for research but still needs additional discovering and
experiments. Since no reliable standards had been recorded yet for nano AMCs'
properties and evaluation, the traditional routes and test are still used. Industrial
production of mentioned composites is still relatively coasty and almost restricted
to labor level. What is aimed in this study is contributing to making production of
AMC's possible by simpler method. This is, addition of particles to the molten
23


metal using aluminum capsules. This technique has not been widely used. Yet, no
reliable standards had been recorded. From the researches that have been surveyed
the following point could be summarized:
1-Generally, ceramic particle reinforcement could enhance mechanical properties
of the metal matrix composites.
2- The main challenge in nano MMC's production is how to achieve regular
distribution of the particles throughout the material structure.
3- In production of the AMC's, best results are obtained by using in situ, stir
casting, powder metallurgy and ultrasonic techniques.
4-The mechanical properties increase with as used particle size decreases.
5- Among properties enhanced using particle reinforcement, wear rate resistance
is the most enhanced property.

















24


Chapter Three
Theoretical Aspects
3.1 Aluminum-based Metal Matrix Composites
Aluminum-based metal matrix composites (AMCs) are ideal materials for
structural applications in the aerospace and automotive industries due to their high
strength-to-weight ratio. Reinforcing the ductile aluminum matrix with stronger and
stiffer second-phase reinforcements such as oxides, carbides, borides, and nitrides
provides a combination of properties of both the metallic matrix and the ceramic
reinforcement components. This may result in improvement of physical and
mechanical properties of the composite. In recent years, many researchers have paid
attention to new fabrication techniques for making aluminum matrix composite.
High-energy ball milling can be named as one of the most important of such
techniques. Mechanical alloying (MA) is a solid-state powder processing technique
involving repeated deformation, welding and fracturing of powder particle. MA has
been widely used to synthesize a variety of materials, such as amorphous alloys ,
Nano crystalline materials , intermetallic compounds , borides, carbides , nitrides
and composites. In almost all cases, the final product has nanosized structure which
exhibits better properties and performance compared to the conventional coarse-
grain materials[19].

3.2 Mechanisms of Strengthening in MMCs
The characteristics of metal matrix composite materials are determined by their
microstructure and internal interfaces, which are affected by their production and
thermal mechanical prehistory. The microstructure covers the structure of the matrix
and the reinforced phase. The chemical composition, grain and/or sub-grain size,
texture, precipitation behavior and lattice defects are of importance to the matrix.
The second phase is characterised by its volume percentage, its kind, size,
25


distribution and orientation. Local varying internal tension due to the different
thermal expansion behavior of the two phases is an additional influencing factor.
With knowledge of the characteristics of the components, the volume percentages,
the distribution and orientation it might be possible to estimate the characteristics of
metallic composite materials. The approximations usually proceed from ideal
conditions, i.e. optimal boundary surface formation, ideal distribution (very small
number of contacts of the reinforcements among themselves) and no influence of
the component on the matrix (comparable structures and precipitation
behavior)[44].
Early materials studies led to the computation of the theoretical strengths of perfect
crystals, which were many times greater than those actually measured. During the
1930s it was theorized that this discrepancy in mechanical strengths could be
explained by a type of linear crystalline defect that has since come to be known as a
dislocation. It was not until the 1950s, however, that the existence of such
dislocation defects was established by direct observation with the electron
microscope. Since then, a theory of dislocations has evolved that explains many of
the physical and mechanical phenomena in metals.
Metallurgical and materials engineers are often called on to design alloys having
high strengths yet some ductility and toughness; ordinarily, ductility is sacrificed
when an alloy is strengthened. Several hardening techniques are at the disposal of
an engineer, and frequently alloy selection depends on the capacity of a material to
be tailored with the mechanical characteristics required for a particular application.
Important to the understanding of strengthening mechanisms is the relation between
dislocation motion and mechanical behavior of metals. Because macroscopic plastic
deformation corresponds to the motion of large numbers of dislocations, the ability
of a metal to plastically deform depends on the ability of dislocations to move.
Since hardness and strength (both yield and tensile) are related to the ease with
which plastic deformation can be made to occur, by reducing the mobility of
dislocations, the mechanical strength may be enhanced; that is, greater mechanical
forces will be required to initiate plastic deformation. Virtually, all strengthening
26


techniques rely on this simple principle: restricting or hindering dislocation motion
renders a material harder and stronger [45].

3.3 Strengthening by Particles

Metals and metal alloys may be strengthened and hardened by the uniform
dispersion of several volume percents of fine particles of a very hard and inert
material. The dispersed phase may be metallic or nonmetallic; oxide materials are
often used. the strengthening mechanism involves interactions between the particles
and dislocations within the matrix[45].The strengthening of particulate MMCs may
be due to different mechanisms[46]:
* Orowan strengthening
* grain and sub-structure strengthening
* quench strengthening
* work hardening
Orowan strengthening theory could explain the strengthening mechanism of metal
matrix composites. The mechanism is shown schematically in Figure (3-1) below.
According to this mechanism the yield stress is determined by the stress required for
a dislocation line to pass by the two particles shown. The dislocation line is bowed
around the two particles as the applied stress is increased until the dislocation line
reaches a critical curvature (stage 2). When this critical curvature is reached the
dislocation line can then move forward without increasing its curvature (stage 3).
The segments of dislocation line on either side of each particle then join, and a
dislocation loop is left around each particle. As each dislocation line moves past a
particle the dislocation cell structure around the particle builds up.
27



Fig. 3-1 Orowan Strengthening Theory [46]

By scaling down the particle size from micro-meter to nano-meter, better material
properties could be obtained. It has been reported that with a small fraction of nano-
sized reinforcements, nano-size dispersion composite could obtain comparable or
even far superior mechanical properties than those of micro-metric dispersion
strengthened MMCs. For example, the tensile strength of 1 vol% Si3N4(10nm)-Al
composite which is fabricated by powder metallurgy method, is comparable to that
of a 15 vol% SiCp(3.5 m)-Al composite fabricated by the same technique[24]. The
yield strength of the nano-metric dispersion composite is much higher than that of
the micro-metric dispersion reinforced composite [45].
Summary of characteristic properties of particle reinforcements is given below [47]:
1 when strength is not main objective
2 improved stiffness
3 reduced wear
4 controlled thermal expansion
5 increased service temperature

3.4 Liquid State Route of AMMCs
Liquid state route involves the incorporation of reinforcement into a liquid
aluminum alloy or the infiltration of a preform (e.g. pressure or vacuum infiltration,
28


squeeze casting). These routes are very attractive because they are simple, cheap
and can be applied for the production of complex three-dimensional compounds. It
is also feasible to produce parts with local reinforcements. Basic foundry
technologies can easily be adapted for the fabrication of discontinuously reinforced
aluminum composites. The main drawbacks of the liquid state routes are the lack of
wetting of the reinforcements (mainly ceramics) by liquid aluminum, the
development of casting defects (shrinkage, gas holes) in the final product, the
insufficient bonding between reinforcement and the matrix or/and the degradation
of the reinforcement by excessive reaction[44].



29


Fig. 3-2 Liquid state Process [44]


3.5 Stir Casting Process
One of significance is the difficulty of achieving a homogeneous distribution of
reinforcement in the matrix, essential for optimum mechanical properties. This
problem is common to most production routes, including the stir casting process
which, using particulate reinforcement, offers the possibility of producing relatively
complex shaped composites. It is important to identify and control casting process
parameters relevant to reinforcement distribution in order to achieve a good quality
composite.
There are however problems associated with the production of reinforced
composites, one of significance being the difficulty of achieving a homogeneous
distribution of reinforcement in the matrix, essential for optimum mechanical
properties . This problem is common to most production routes, including the stir
casting process which, using particulate reinforcement, offers the possibility of
producing relatively complex shaped composites. It is important to identify and
control casting process parameters relevant to reinforcement distribution in order to
achieve a good quality composite. In general stir casting of MMCs involves
producing a melt of the selected matrix material, followed by the introduction of a
reinforcement material into the melt, obtaining a suitable dispersion through
stirring. The next step is the solidification of the melt containing suspended particles
under selected conditions to obtain the desired distribution of the dispersed phase in
the cast matrix. The emphasis has been given to MMCs fabricated by the stir casting
technique. In order to design a process to give a homogeneous distribution of
reinforcement the following factors need to be understood [48]:
1- Particle density, size, shape and volume fraction will influence the reinforcement
settling rate,
2- Surface properties of particles will affect the ease or difficulty with which
wetting is achieved.
31


3- The rheological behavior of the matrix alloy melt and reinforcement slurry is
influenced by the reaction of particles with the liquid, and with each other.
4- Gas entrapment during particle incorporation or mixing will lead to poor
distribution as particles attach to gas bubbles, and porosity is also increased.
5-Mixing parameters must be such as to produce a uniform particle distribution in
the radial and axial directions.
6- During solidification settling time must be minimized.
7- In general the reinforcement particles occupy inter-dendritic or between
secondary dendrite arm spacing; therefore the finer the spacing or the finer the
matrix grain size, the better the particle distribution.


3.6 Differentiation between Microscale and Nanoscale
Reinforcement Particles

Large-particle and dispersion-strengthened composite are the two sub classifications
of particle-reinforced composites. The distinction between these is based upon
reinforcement or strengthening mechanism. The term is used to indicate that
particlematrix interactions cannot be treated on the atomic or molecular level;
rather, continuum mechanics is used. For most of these composites, the particulate
phase is harder and stiffer than the matrix. These reinforcing particles tend to
restrain movement of the matrix phase in the vicinity of each particle. In essence,
the matrix transfers some of the applied stress to the particles, which bear a fraction
of the load. The degree of reinforcement or improvement of mechanical behavior
depends on strong bonding at the matrixparticle interface.
For dispersion-strengthened composites, particles are normally much smaller,
having diameters between 0.01 and 0.1 m (10 and 100 nm). Particlematrix
interactions that lead to strengthening occur on the atomic or molecular level. The
mechanism of strengthening is similar to that for precipitation hardening. Whereas
31


the matrix bears the major portion of an applied load, the small dispersed particles
hinder or impede the motion of dislocations. Thus, plastic deformation is restricted
such that yield and tensile strengths, as well as hardness, improve [45].

3.7 Weight Volume Conversion

Most of the rules that deal with composites are in term of volume fraction V
f
rather
than weight fraction W
f.
, it is worthy to estimate volume in term of weight. It should
be known that:
Density = W/ V, So:
V = W/ .. (3-1)




3.8 Method Used to Determine the Volume Fraction of the
Matrix and Reinforcement


Many researchers carried out studies about this type of reinforcement and they all
agreed about the methods to calculate the moduli of elasticity and rigidity [49],
assuming that:
1- The particles are randomly distributed in the matrix.
2- The particles are of the same size.
3- The particles are bonded with the matrix strongly.
4- Each of the particles and the matrix is isotropic.
The law of mixture [50]: -
The mass (Mc) of composite is made up of the masses of the matrix (m) and the
filler particle M
r
M
c
= M
m
+ M
r
. (3-2)
Since the mass is volume times density then equation can be written as below: -
V
c

c
=V
m

m
+ V
r

r

32

... (3-3)
where

is the volume fraction of the matrix and

volume fraction of fiber

c
=
m
V
m
+
r
V
r
...(3-4)
noted that since V
m
= V
c
V
r
it must have:
Vm = 1-V
f
.. (3-5)
Also the mass of the matrix and the mass of reinforcement material can be
calculated as follows: -
Since V
f
=

Then M
r
= Vc V
r
P
r

And M
m
= Vc P
m
(1-Vr) .(3-6)


3.9 Law of Mixture
The mass (M
c
) of composite is made up of the masses of the matrix (M
m
) and the
filler particle (M
r
),
M
c
= M
m
+ M
r
.. (3-2)
Since the mass is volume time's density then
equation (3-3),for density , can be written as follows[46,49]: -

c
=
m
V
m
+
r
V
r
.(3-4)

3.10 Principles and Properties of Dislocation Reinforcement
Composite materials technologies offer a unique opportunity to tailor the properties
of aluminum. This could include increased strength, decreased weight, higher
service temperature, improved wear resistance, higher elastic modulus, controlled
coefficient of thermal expansion, improved fatigue properties, etc.
33


It is of utmost importance to have rules or models in order to predict or to calculate
the expected properties of the composite. As a first estimation, the rule of mixtures
can be helpful. That is[46]:
Pc = PmVm + P
r
V
r
(3-10)
with P = property
V = volume fraction
and subscript c, m and r indicate resp. composite material, matrix and
reinforcement.
Youngs modulus (E) is an elastic property which is well bracketed
by two models. Figure (3-3)illustrates the evolution of the Young's modulus of an
Al-SiC

composite as a function of the volume fraction of SiC.


Fig. 3-3 The evolution of the Young's modulus of an Al-SiC[46]

Linear bound in fig (3-3) is defined by the simple rule of mixtures:
Ec = Em Vm + ErVr ,,,,,,,,.(3-11)
The nonlinear bound (see dotted line in 3-3) is given by a more complex expression
(valid for discontinuously reinforced composite with spherical particles as
reinforcement) :
34



(3-12)


3.11 Basics of Wettability
Basically the wettability of reinforcement with a metal melt can be shown by the
edge angle adjustment of a molten droplet on a solid base as the degree of
wettabilityaccording to Young:
SA LS = LA cos
where LA is the surface energy of the liquid phase,SA the surface energy of the
solid phase, LS the interface energy between the liquid and solid phases and is
the edge angle.
Figure (3-4) shows the edge angle adjustment of a molten droplet on a solid base for
different values of the interface energy. At an angle of > /2 a nonwettable system
is described and for an angle limit of < /2 a wettable system. With decreasing
angle the wettability improves. In Table 1.3 the surface and interface stresses of
selected metal ceramic systems at different temperatures are summarized. Of
special relevance is the system Al/SiC, since it is the basis for the melting
metallurgy of particle reinforced aluminum composite materials.
As the contact develops, for example at the beginning of an infiltration, adhesion
occurs. The adhesion work WA for separation is [46]:
WA = SA LA =LS
WA = LA (1 + cos)
35


In the case of immersion the interface between the solid and the atmosphere
disappears, while the interface between the solid and the liquid forms. The
immersing work WI is:
WI = LS SA
In the case of spreading the liquid is spread out on a solid surface. During this
procedure the solid surface is reduced as well as a new liquid surface being formed
and hence a new solid/liquid interface is formed. The spreading work WS is:
WS = SA LS LA
The wetting procedure is kinetic and is dependent on time and temperature.
Therefore, the kinetics can be affected by the temperature.

Fig. 3-4 Edge angle adjustment of a melt drop on a solid base for various values of the interface energy
.
3.12 7000 Serious Aluminum Alloys as Matrix Reinforced with
Ceramic Particles

Among all the commercial aluminum alloys, the 7000 series aluminum alloys
exhibit the highest mechanical properties. They are used for high strength structural
36


applications such as aircraft parts and sporting goods. The desirable properties of
these alloys are: low density, high stiffness, specific strength, good wear resistance
and creep resistance [42].
Aluminum metal matrix composites (MMCs) with 7075alloy as matrix reinforced
with ceramic particles are finding application in aerospace, automobile and farm
machinery equipment because of their improved mechanical and tribological
properties . In particular, Al
2
O
3
particles mixed with Al7075 matrix in appropriate
proportions are reported to exhibit improved tensile properties because of the higher
modulus of elasticity and strength of the alumina [6]. However, it is difficult to
reach the same strength in the composite as in the monolithic alloy, for 2xxx, 6xxx
and 7xxx based composites[46,47].Existence of Mg in 7075 composition make it
good candidate for particle reinforcement since Mg is considered a wetting
agent[51,52]


3.13 Features of AlAl
2
O
3
System

The system shows high stability at elevated temperatures. It resists softening at
high temperatures. Alumina does not react with matrix at high temperature and does
not create any undesired phase and the system has superior properties such as
hardness, fracture toughness as compared to the native material. High thermal
stability of alumina particles prevents the particles from ripening and
dissolving[55].


3.14 Addition of Particles using Aluminum Capsules
One of the common challenges in preparing AMC's is the addition of the second
phase of the composite, i.e. the reinforcement. The basic issue is how to get regular
distribution. In practical work of this thesis, an Aluminum capsulated Al
2
O
3
powder
37


will be used as a route of addition. Using aluminum capsules is not a commonly
route. It has three main encouraging advantages:
1-It has no significance in the alloy composition since it is made from pure
Aluminum (only balance of the composition slightly increases).
2- It allows preheating of the particles (with relatively high conductivity of alumina
32.6 W/m K [3] and their high surface area).
3- Allows good accuracy of weight fraction control (no loss of particles caused by
stream convection of air or gas).
An optimization between first two points must be taken in mind by adjusting the
volume and the shape of the capsule .In other term, less weight of capsules for less
significance in composition, and a shape that allows slow melting for longer
preheating by conductance through capsule wall.
On the other hand , agglomeration of particles is a disadvantage of mentioned route
.This disadvantage can be overcome by reducing the capsule charge and by leaving
a space in the capsule to allow gases to expand inside the capsule consequently
defuse the particles by convection streams specially with light weight of the
particles ( 20 nm sized).
The feeding efficiency of capsule which is ratio of the incorporating particles to remaining
particles is about 56 % [49].






38


Chapter Four
Experimental Work
4.1 Introduction

In this chapter, the Experimental procedure is explained. These steps are based
on previously investigated researches and studies.
4.2 Preparations of Basic Materials
A 7075 aluminum shafts were chosen. Their surface was cleaned by Iron brush to
remove any undesired oxides and containments. It was washed with alcohol then
with Acetone. The alloy chemical composition was examined using SPECTRO
metal analyze. The composition is given in table (4-1).
Table 4-1 Chemical composition
Ni Cr Mg Mn Cu Fe Si
0.0036 0.190 2.11 0.0244 1.73 0.295

0.0756

Al Zr V Pb Be Ti Zn
balance 0.0014

0.0101 0.0093

0.0042 0.0293 5.53


The shaft was cut to smaller pieces for easier melting and to meet crucible size.
The pieces were weighted to know melting charge according to desired weight
fraction of each cast as in figure (4-1).
39



Fig. 4-1 7075 alloy scrap
The Al
2
O
3
powder is Gamma white 20 nm in size with specific surface area of 230-
400 m
2
/g ( SSNano,USA). The powder was charged in known weight commercial
aluminum foil with known weight. In first trial the capsule weight was 1g and filled
with 1g of alumina powder. A 0.01 g accuracy balance was used to prepare alumina
capsules as in figure (4-2).



Fig. 4-2 Capsule preparation
41





4.3 Furnace Description


The furnace used in experiment is constructed from graphite crucible and heater
element controlled by K type thermal controller + stirring system.(figure 4-3).The
stirrer has four blades with 45
o
inclination [56] rotated by hand drill electrical
motor and its speed set at 300 rpm [15, 53, 56]. A K-type thermocouple is attached
to the crucible base to give accurate temperature feedback to thermal controller .the
temperature was set at 700 C
O
[57, 37].


Fig. 4-3 furnace
4.4 Mold

The mold was manufactured of stainless steel with ability of disassemble to prevent
cast sticking or entrapment .Its dimensions are 120 x 100x 14 mm vertically stand
with open upper side to be a raiser as in fig(4-4) .

41



Fig. 4-4 Mold

4.5 Casting Procedure
1 -First Trial
The furnace with the crucible was preheated for 1 hour with aluminum scrap charge
to remove undesired moisture, then temperature was raised up to 700 C
o
.When the
all scrub melt first alumina capsule was introduced and stirrer was lowered for
stirring .Introducing of other capsules was in rate of 1 capsule per min. until the
desired amount was completely introduced .The stirring continued for total time of
5 min [57] and AlCl
3
was used

to degas the melt .Then the melt was poured slowly
in the mold .
After the cast was cooled, it was machined to examine interior places of the cast.
Agglomerations of alumina powder were observed by macro examination.
2 -Second Trial
First trial procedures were repeated but with capsules of thicker foil and less powder
weight .The stirring time was 20 min.[37] machining the sample showed no
agglomeration of particles on macro level.
In the first trial capsules were: 1g Al + 1g alumina powder
In the second trial capsules were 3g Al + 0.5 alumina powder
42



3- Last Trial
In the last trials the charges (Aluminum scrub +alumina capsules ) were prepared as
following in table (4-2) .Each capsule contained 0.5g of alumina.
Table 4-2 sample charges
Aluminum Capsules
weight x No.
Alumina weight 7075 alloy scrub weight Sample
4 x 3g =12 g 2g 386 g 0.5 %
8 x 3g = 24g 4g 372 g 1%
12 x 3g = 36g 6g 358g 1.5%

The final cast specimen was machine cut to visually examine porosity and
agglomeration as in figure (4-5).


43



Fig. 4-5 Sample machining and cut
Then the samples were heat treated at 200
o
for 12 hour and then quenched in cold
water from about 200C
O
cooling rate for internal stress relief and grain refinement
[58].
4.6 Preparing samples and tests
4.6.1Impact test:
Samples were prepared for impact test by machining to dimensions of 10 x10 x 50
mm with thin saw was cut in the middle with 8m height under the saw cut
(charpy)[45] . The tests were carried out using BROOKS charpy Impact test
machine as shown in figure (4-6). Two readings were taken for each sample.

44



Fig. 4-6 Impact test specimen [45] and Impact test instrument
4.6.2 Wear Rate Test:
Dry sliding wear resistance test was carried out on all samples according to ASTM
G99[59]with sample of 10mm in diameter and 16.5 mm in length, taking the load as
the alternative parameter with (500,1000 and 1500 gram) [60]and a rotating speed
of disc was set to 500 RPM. The pin was located at a radial distance of 60 mm from
the rotating axis, for each 8000 revolution the sample was taken out, cleaned and
weighted with 0.0001 g accuracy balance.
Two readings were taken for each case to plot the mass loss against the load. Figure
(4-7) shows the pin on disc and testing of samples.

Fig. 4-7: Sample in pin on disc device
45


4.6.3 Tensile Test:
Tensiletest samples were prepared according to ASTM -E 8M sub sized specimen
[61].The specimens were made using wire cut CNC machine.The test was carried
out in Al-Nahrain University-Applied Mechanics Laboratory using GUNT WP310
instrument at speed of 0.1mm/s as shown in figure(4-8).

(a)


(b)
46


Fig.4-8 Tension test, (a) samples preparing,(b) apparatus
4.6.4Hardness Test:
Brinel hardness testing device which is located in State Company for Inspection and
Engineering Rehabilitation (SIER) had been used, shown in figure (4-9) with a 50
gram load. The tests were carried out on all samples with a holding time of 2
second. Six readings of hardness were taken for each sample to get the mean value.
The values were then converted to Vickers hardness by using standard chart of the
device.

Fig. 4-9 Hardness instrument
4.7 Physical Tests
Porosity of each sample was calculated by comparing theoretical and apparent
density .Theoretical density was calculated using law of mixture and apparent
density was measured using Archimedes law.
Three similar samples were prepared for X-ray diffraction (XRD), Optical
Microscope, Atomic Force Microscope (AFM) and scanning electron microscope
(SEM). To prepare the samples for the test, samples of (SEM) and Optical
Microscope were cut and mounted using acrylic material for easy handling in
grinding and polishing stage.
47


An etching process was done to reveal the grain boundary using two kinds etching
solutions which were HNO
3
+H
2
O and NaOH [62].
Scanning Electron Microscope (SEM) and X-Ray Differaction (XRD) tests were
carried out in the Ministry of Sciences and Technology / Material Science
department. 40 kV with Cu K radiation (=0.15406 nm) was used for XRD
measurements. The XRD patterns were recorded in the 2 range of 3080 (step
size 0.05 and speed 5 degree/min.). Microstructure Image analysis and (AFM)
were carried out In Al-Nahrain University /Mechanical engineering Department
Laboratories . Microstrucure images were obtained using Olympic type optical
microscope with a max magnification of 1000X. Fig (4-10) shows the optical
microscope.
Atomic Force Microscopy (AFM) was used to capture the surface topography and
the surface and measure the materials AFM topographic images were obtained in
air at room temperature 25 and 27% relative humidity. Images were acquired and
processed with the NanoScope 531r software.

Fig. 4-10 Optical microscope




48


Chapter Five
Results and Discussion

5.1 Introduction
In this chapter results of physical and mechanical tests results of all samples will
be illustrated and discussed.

5.2 Physical Results
The results of Physical properties and their discussion can be given as follows:

5.2.1 Density and Porosity Measurement

The experimental density of the composites was obtained by the archimedean
method by weighing small pieces cut from the composite cylinder first in air and
then in water. In addition, the theoretical densities were calculated using the mixture
rule.
Density of Al
2
0
3 =
3.92

g/ cm
3
[3]
1 g of

Al
2
0
3 =
1/ 3.92 = 0.2551 cm
3

Porosity = (Theoretical Density Apparent Density)/Theoretical Density


The Al 7075 and the reinforcement Al
2
O
3
particles have the densities of 2.7 and 3.9
g/cm
3
, respectively [22]. In order to determine the porosity content, density
measurements were conducted on unreinforced and composites reinforced with 0.5,
1 and 1.5 wt. % nano-Al
2
O
3
particles. The difference between the theoretical
densities and calculated densities which were obtained are given in table (5-1) .

49



Table 5-1 porosity
Sample Theoretical
density(g/cm
3
)
Apparent or practical
density (g/cm
3
)
Porosity %
0.5 % 2.7880 2.7810 0.251
1 % 2.7925 2.7768 0.562
1.5 % 2.7921 2.7748 0.6196


Fig. 5-1 The variation of porosity
The variation of porosity with volume percent with nano alumina volume percent is
shown in fgure (5-1) The figure shows that increasing porosity volume percent has
occurred with increasing alumina weight fraction . This is due to the effect of low
wettability and agglomeration at high content of reinforcement and pore nucleation
at the matrixAl
2
O
3
interfaces. Moreover, decreasing liquid metal flow associated
with the particle clusters leads to the formation of porosity , and also the hydrogen
content of molten increasing viscosity due to particle addition and entrap gassed
inside the melt and prevent them from floating before it solidify. Porosity highly
effect the mechanical properties by decreasing them.
0
0.1
0.2
0.3
0.4
0.5
0.6
0.7
1 2 3
51



Fig, 5-2 Variation of porosity with the nano alumina content [38]


5.2.2X-ray Diffraction Results
The XRD spectrum of Al 7075 with 0.5wt.%, 1% and 1.5%Al
2
O
3
nanocomposite
powder is shown in figure (5-3) The diffraction patterns of the nanocomposite
exhibit various peaks corresponding to the face centered cubic phase of Al. It
appears that the addition of ultra-fine Al
2
O
3
resulted in further broadening of Al
peaks. X-ray diffraction peaks, which increased with an increase of fine Al
2
O
3

content. The peak width of 1.5 wt.% Al
2
O
3
nanocomposite was increased by around
25% higher than unreinforced nanocrystalline alloy. This indicated the formation of
fine grain. Further, a minor shift (towards smaller angle) in the position of the XRD
peaks was also noticed and this could be related to the dissolution of little oxygen
atoms from alumina and other atoms like Mg, Cu etc. related to minor matrix
alloying elements in the lattice of aluminum.
51



(a-0.5%)

(b-1%)
52



(c-1.5%)


Fig 5-3 a, b and c shows XRD for different wt. fractions
It is shown that difference in intensity not in 2 dfferaction this is perhaps due to
small additives from Al
2
O
3
and alloying elements which are not clear affected in the
differaction of

X-ray.

5.2.3 Microstructure Observation

A-Optical Microscope
Fig (5- 4) shows Micro structures of different wt. fractions as well as the scale.
53



(a)

(b)

(c)
Fig 5-4: Microstructures, (a) 1.5%, (b) 1%, (c) 0.5 %
Optical micro structures show that there are several areas in the cast for three samples. It
could be said that practically, porosity appears even with smallest fraction of alumina
addition. 7075 AL alloy is very sensitive to cooling stage in heat treatment [58].It is clear
that the grain size range is about 70-200 m .Considering it is not cold worked and
assuming there is no porosity ,this grain size range indicates good mechanical properties ,
54


However ,mechanical properties do not depend on grain size only, but also on the bonding
between them[45].Grain boundaries tend to enlarge with increasing Al
2
O
3
wt. fraction due
to movement of particles (if it is dealt with as impurities out of the grain) during
solidification stage [63].
B- Scanning Electron Microscope
Figure( 5-5) shows the (SEM) images for the three samples

(a)

(b)
55




(c)
Fig.5-5 :( SEM) micrographs,(a)0.5%,(b)1%,(c)1.5%
It is clear from micrographs above that the alumina particles are distributed. The
particles cannot be considered as distributed regularly all over the matrix since these
micrographs represent a small portion of the material. However, as stir casting
technique is used , it can be successful technique applicable to industrial purposes
and mass product . For more regular distributed and efficient particles, ultrasonic
technique showed better result [27]. This technique is still costly high to be
applicable in industrial and mass productions. Figure (5-4) shows SEM micrographs
of the as-cast Al2%Al
2
O
3
nanocomposites synthesized using ultrasonic technique.
In 0.5% a pitting like point appears .It is expected to be formed during
solidification process as a result of clustering of alumina and entrap of gasses by
it,as well as the deference of thermal expansion between it and Al matrix . In 1.5%
image it is clear that there are eutectic zones caused by precipitation of alumina
particles on grain boundary during grain growth stage.

56



Fig.5-6: (SEM )micrographs of the as-cast Al2%Al
2
O
3
nanocomposites synthesized using
ultra sonic technique [27].
C- Atomic Force Microscope



Fig.(5-7)AFM images of ceramic nanocomposite on aluminium 0.5%
57


The morphological changes of the metal nanocomposite investigated by From Fig.
1, it can be observed that the morphology Surface roughness is also an important
parameter composite application. surface roughness of the composite increase with
increasing the volume fraction of the reinforcement. These results are further
confirmed by AFM images, which show a increases in RMS roughness of the
nanocomposite It is widely established that addition of a nanocrystalline phase
affects the rod-like structure and crystallite size, which determine the surface
morphologies of the nanocomposite [63].Figure (5-7) for Aluminum with 0.5%
20nm alumina, figure (5-8) pure Aluminum and figure (5-9) Aluminum reinforce
with micro size Alumina.




Fig. 5-8 Atomic force microscopy (AFM) images of aluminum
58





Fig.5-9 (AFM) images of aluminum reinforce with micro alumina [57]


5.3 Mechanical Results
Mechanical results and their discussion can be given as follows:


5.3.1 Hardness
Table (5-2) shows hardness results of the original alloy and different wt. fractions. This
change can be stated as the particle was reinforcing the structure by preventing the lattice
movement and also it indicates the good binding force between the particle and the
structure. This is not to be explained for 1.5% which, as previously mentioned, has weak
grain boundary .These results are a little higher than 100 micron SiC /LM6 Al alloy but
with higher wt. % [14] .
Table (5-2): Vickers hardness for all samples

sample Hv
0.5% 134.33
1% 105.6
59


1.5% <50



Fig. 5-10 Hardness variation ,
Porosity does not affect so much the hardness measurement since it is measured
locally .Therefore ,six readings were taken in different points in the sample.Results
show improvement in Hardness upon O tempered 7075 Al alloy [4] except for 1.5
% sample which showed decreased hardness due to high.


5.3.2 Sliding Wear Resistance

Table (5-3) shows mass loss in g against applied load. The result shows increasing wear
resistance with fraction increase. These results can be confirmed by previous researches
surveyed in chapter two. In fact the most enhancements in mechanical properties can be
observed in wear resistance. This is valid for almost all AMCs reinforced with ceramic
particles. Theoretically, according to law of mixture as general rule, property changes and
the properties of alumina it is not surprise to obtain same results.


0
20
40
60
80
100
120
140
160
1 2 3
61





Table 5-3 mass loss against applied load

Sample load 500g 1000g 1500g
0.5% 0.0225 0.0404 0.8715
1% 0.085 0.0206 0.0225
1.5% 0.0053 0.0100 0.015


(a)


(b)
0
0.2
0.4
0.6
0.8
1
1 2 3
0
0.02
0.04
0.06
0.08
0.1
1 2 3
61



(c)
Fig. 5-11mass loss against load ,(a)0.5%,(b)1%,(c) 1,5%
Above results agree with those of CNT reinforced 6061 Al alloy [64](figure 5-12)



Fig.5-12 1%CNT/6061 wear rate[65]

5.3.3 Fracture Toughness Results

Table (5-4) shows the fracture toughness of the samples. It is clear that there is
improvement in 1 and 1.5 wt fractions. But for 1.5 sample ,again, the voids caused a
reduction in fracture toughness .Brittleness behavior increased with increasing wt. fraction.
0
0.005
0.01
0.015
0.02
1 2 3
62


Voids (flaws) contribute in increasing stress intensity factor that can directly affect the
fracture toughness [65].
K
I
=1.14(a)
0.5

where K
I
is fracture toughness and is stress and a is flaw radius .
Table (5-4) Impact test results
Sample Trial 1(Nm) Trail 2 (Nm)
0.5% 7.4 7.7
1% 8.3 8.4
1.5% 6.9 6.7


above results agree with those of 100 micron Al
2
O
3
/LM6 al alloy (table 5-5)[14]
Table 5-5 alumina/LM6 impact load[14]

%alumina/LM6 Al alloy Average force (Nm)
2.5% 6.62
5% 6.88
7.5 7.04


5.3.4 Tensile Test Results
Table (5-6) shows ultimate tensile stress and maximum elongation
Table (5-6) tensile test results

sample Ultimate tensile Maximum elongation %
0.5% 190 MPa 2.9
1% 155 MPa 2.1
1.5% 108 MPa 1.8

63


If the high porosity is kept in mind ,above results agree with those of 35nm
Al
2
o
3
/pure Aluminum 2,3,4 wt.%[29] .As mentioned before the initial strength of
7075 Al alloy cannot be easily enhanced[52,46].
Tensile test specimens showed Brittle Failure .Therefore, there is no clear
measurement for yield strength. The Results showed a small increase upon o-
tempered 7075 Al alloy[3].
Generally , when talking about enhancement effect of particle reinforcement and
comparing different researches, It is noticed that there is an efficiency for
strengthening .That is the finer the particles the higher enhancement . It is also
noted that there is some kind of relation between different particle sizes and
increase in mechanical property . For example , the effect of 2.5 wt% of 100 micron
Al
2
O3 is very close or equivalent to 1wt.% of 20 nm[14].

Chapter Six
Conclusions and Recommendations

6.1 Conclusions
It is clear that the addition of ceramic nanoparticles to the Aluminum alloy
generally enhances its properties. However, the main challenge is How to achieve
regular or good distribution of particles across the matrix (The Aluminum
alloy).Not only this, But also how to produce final composite. The routes of
production Is very similar to those in ordinary composites. For example, achieving
good porosity for the material which has an important role in production of any
MMC. For this thesis, conclusions could be summarized with following points:
1- The best results regarding enhancement of mechanical properties are wear
resistance, fracture toughness and micro hardness but not tensile strength.
2- Increasing stirring time can reduce agglomeration of added particles.
64


3- Heat treatment refines grain size and consequently enhances mechanical
properties
4- Reducing capsule particle content and increasing its thickness lead to reduction
in particles agglomerations.
6.2 Recommendations for Future Work

it is obviously known that subject of reinforcement of Aluminum using ceramic
nanoparticle is very promising and can be applied in wide fields of application
Although It is not standardized yet . It is very fertile subject for researches; however
it is divergent, especially in routes and materials. May be in future new routes will
be applied. Industrial application and mass production of AMCs reinforced with
ceramic nanoparticles are still limited. So, it is more useful for researchers to find or
Investigate methods and techniques that are easier to be utilized in industrial level
of production. There should be an optimization between production quality and its
cost. Regarding present thesis and starting from the availability of initial materials
following recommendations are put forward:
1- Repeat the stir casting under inert gas flow, for example: Argon.
2- Enhancement capsule addition method by focusing and improvement of used
capsules.
3- Using more than one particle size for same fraction.
4-Designing and modeling more molds and cast techniques.
5- Reinforcement of more than Aluminum alloy for same particle kind and size.
6- Study the effect of work hardening on produced AMC .

65


And for far future standardization the following flow chart is designed to clarify the
recommendations for Industrial applications:























AMC using
Nanopoweder
Matrix alloy
Reinforcement
Production method
Liquid state
or casting
Powder
metallurgy
Size
kind
Squeez casting
Investment or
Sand
casting
Introduction of
reinforcement
66















Fig (6-1) recommendations flow chart


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75





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Al
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.

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, 4.7 % Al
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.