Manufacturing of Aluminum Matrix Composites Reinforced

with Iron Oxide (Fe3O4) Nanoparticles: Microstructural

and Mechanical Properties
EMIN BAYRAKTAR, FAYZA AYARI, MING JEN TAN, AYSE TOSUN-BAYRAKTAR,
and DHURATA KATUNDI

The purpose of this paper is to demonstrate the low-cost manufacturing of aluminum matrix
composites reinforced with nano iron oxide as light and efficient materials for engineering
applications. It is very desirable to use reinforced aluminum matrix composites in structural
applications (automotive, aeronautical, etc.) because of their outstanding stiffness-to-weight and
strength-to-weight ratios. In modern industry, it is increasingly important to develop new
composites as alternative materials to fabricate multifunctional pieces. Detailed information is
presented on the manufacturing process of this composite, and a preliminary study was per-
formed on the cryogenic-cycling behavior to evaluate the interface between the matrix and the
reinforcement. Microindentation tests were carried out to evaluate the micromechanical prop-
erties of these materials; a simple and practical finite element model is proposed to predict
certain parameters related to the composition of the composite.

DOI: 10.1007/s11663-013-9970-1
Ó The Minerals, Metals & Materials Society and ASM International 2013

I. INTRODUCTION The microindentation technique is often used to

THE worldwide popularity of powder metallurgy lies
in the ability of this technique to produce complex
shapes with exact dimensions at a very high production
rate and low cost.[1–3] For this reason, it is very desirable
to use reinforced (with Fe3O4, iron oxide) aluminum
matrix composites in structural applications (automo-
tive, aeronautical, etc.) because of their outstanding
stiffness-to-weight and strength-to-weight ratios.[1–9]
Additionally, it is very attractive to add iron oxide
(Fe3O4) reinforcement to improve the magnetic perme-
ability of these composites, thereby obtaining a good
synchronization between the thermal and electrical
conductivities and the magnetic permeability.[1,2,10–15]
In this paper, ‘‘aluminum-iron oxide (natural Fe3O4 in
the form of the mineral magnetite) powder composites’’
were developed as alternative materials using a micro-
wave and a tubular ceramic oven sintering program with
various aspect ratios varying from 0.25 to 0.85 for the
simultaneous preparation of Fe3O4 particles and alumi-
num powders (at the laboratory scale). These compos-
ites are clean and light and are very useful for
application in the aeronautics industry.
EMIN BAYRAKTAR, Full University Professor, FAYZA
AYARI, Research Associate, and DHURATA KATUNDI, Research
Engineer, are with the School of Mechanical and Manufacturing
Engineering, Supmeca/LISMMA - Paris, Paris, France. Contact e-mail:
bayraktar@supmeca.fr MING JEN TAN, Associate Professor, is with
the School of Mechanical & Aerospace Engineering, Nanyang Technolo-
gical University, Singapore, Singapore. AYSE TOSUN-BAYRAKTAR,
Professor, is with the Chemical Processing Department - P. Vauqelin,
21, Av. Boutroux, 75013 Paris, France.
Manuscript submitted January 29, 2013.
measure the micromechanical properties of materials,
and it is advantageous for its ability to determine the
hardness and local elasticity modulus for particular
conditions; it is also able to handle small sample sizes. In
fact, at present, the hardness and Young’s modulus can
be easily defined using the Oliver–Pharr[5] equations
based on microindentation tests of small-sized speci-
mens.
The main objective of this study is to compare
experimental and numerically simulated indentation
load-depth curves using a conical indenter for the
investigated aluminum metal matrix composites. Exten-
sive experimental work was initially performed on the
specimens under various loading conditions. Then, a
numerical simulation was established for the validation
of experimental microindentation tests that were applied
to the considered material to provide a simple under-
standing of certain parameters of the material, which
was produced here under laboratory conditions. The
results concern the influence of the load on the behavior
of the indentation-depth curves. The numerical results
of Berkovich indentation tests applied to a set of
specimens are thoroughly discussed. A significant step
forward has been achieved in the load-depth monitoring
during loading and unloading during the microindenta-
tion cycles. In this paper, the experimental results were
validated with a numerical finite element model (FEM)
of the microindentation behavior of an aluminum
matrix composite material that is used in aeronautic
and automotive applications.
It is also interesting to study the behavior of the
aluminum matrix composites reinforced with Fe3O4
under cryogenic cycling. Normally, magnetite Fe3O4
conducts electricity at ambient temperatures. Its

METALLURGICAL AND MATERIALS TRANSACTIONS B

conductivity decreases slightly with decreasing temper-
ature, as will be detailed in the text later. Below 120 K
(153 °C), Fe3O4 becomes an insulator. Additionally,
cryogenic cycling can cause significant changes in a
composite material, with potholing, delamination, and
microcracking representing some of the more dramatic
phenomena.[18,19] Shrinkage of the matrix during curing
and mismatched coefficients of thermal expansion
among the reinforcement, the matrix, and the ply
groups in a laminate are the main causes of the internal
stresses that cause laminate microcracking at cryogenic
temperatures.[17–25] Structural failure has occurred in
cryogenic liquid-storage systems when they were not
designed to account for microcracking and thermal-
cycling-induced stresses.[24–29] For this reason, a prelimin-
ary study was carried out concerning the cryogenic-cycling
behavior of the studied composites to evaluate the
interface between the matrix and the reinforcement.
II. EXPERIMENTAL STUDY
A. Preparation of Fe3O4 Magnetic Nanoparticles
The preparation of the Fe3O4 magnetic nanoparticles
was adapted from a method that has been presented in
the literature.[1,2,12,15–17] First, ferric chloride (FeCl3,
820 mg) was dissolved in 30 mL of deionized water
under mechanical stirring and nitrogen atmosphere at
298 K (25 °C) in a three-necked flask. A volume of
Fig. 1—(a) Specimens prepared with various aspect ratios and (b)
Typical optical microscopy of the surface obtained from two sintered
specimens (2.5 wt pct Fe3O4).[1,2]
10 mL of ferrous chloride tetra hydrate (FeCl2Æ4H2O,
53 mg/mL) aqueous solution was then added into the
flask under stirring. Ten minutes later, ammonia aque-
ous solution (4.5 g, 25 pct) was slowly injected into the
flask. The reacting solution turned black with the
injection of the ammonia solution. The total amount
of the reacting solution was approximately 45 mL. The
reaction was maintained for 4 hours. When the reaction
was completed, the Fe3O4 nanoparticles were separated
and washed with deionized water several times with the
aid of a magnet until the deionized water was neutral.
The purified Fe3O4 nanoparticles were again dispersed
into 45 mL of deionized water. After this step, the Fe3O4
magnetic nanoparticles were collected and washed with
deionized water several times with the aid of a magnetic
bar. Finally, the Fe3O4 nanoparticles were measured in a
laser granulometer at Le Conservatoire National des
Arts & Métiers (CNAM) in Paris.
The particle-size distributions were variable (45 to
70 nm). In the method that we used, the agglomeration
phenomenon was considerable. However, another syn-
thesis method was also used to prepare Fe3O4 nanopar-
ticles to compare the two methods in terms of feasibility
and the cost of producing a given quantity at the
laboratory scale.[1,2]
For this second method, we adopted a method from
the literature that has been successfully applied for the
synthesis of magnetite (Fe3O4) nanoparticles in aqueous
solutions without any surfactants.[15] The Fe3O4 particle
sizes were measured in the same manner as in the case of
the former synthesis method, in a laser granulometer.
The resultant Fe3O4 nanoparticles exhibited an average
diameter of 30 to 45 nm. The procedure described here
for the synthesis of Fe3O4 nanoparticles in an aqueous
solution, while similar to previous protocols reported in
the literature, contains significant new synthesis modi-
fications, which were predominantly developed at the
chemical process laboratory in Paris (‘‘École Chimie,
Établissement de P. Vauquelin,’’ Paris 13ème). In the
framework of the present research, the first synthesis
method was chosen because it was very simple to carry
out, and the main goal of the study is to design
aluminum-based powdered composite reinforced with
Fe3O4 nanoparticles for novel aeronautics applications.
Formerly, this type of composite has been successfully
applied for novel designs of alternators and other
automotive components.
B. Manufacturing of Green Compact Specimens
from Powder Materials and Sintering Conditions
Two manufacturing methods were used in this study
for the aluminum-based powder composites reinforced
with Fe3O4 nanoparticles. Detailed information con-
cerning the microwave sintering method used for this
composite material has been presented in previous
articles.[1,2] The application of microwave heating
energy to the processing of various materials, such as
ceramics, metals, and composites, offers several advan-
tages (lower energy costs and shorter processing times)
over conventional heating methods for many industrial
processes. However, in view of the production rate of
METALLURGICAL AND MATERIALS TRANSACTIONS B
Fig. 2—(a) SEM micrographs of the microstructures of Al-Fe3O4 composite samples with 20 pct Fe3O4 (b) Map of the microstructural
analysis.[2]

the composite, an effective sintering method was
achieved with a simple tubular ceramic oven in this
study. The specimens were prepared with compact
geometry from aluminum and Fe3O4 powders.
Aluminum with a purity of 99.7 pct and a grain size of
<2 lm (Merck Co, France) was used as the base
material. The purity level of the Fe3O4 was found to be
99.62 pct, and the grain size was found to be 20 to
70 nm (the grain size was measured with a laser
granulometer). The weighed-out samples were mixed
by high-energy mechanical ball milling. Zirconium balls
of 3 to 5 mm in size were used as the grinding media.

METALLURGICAL AND MATERIALS TRANSACTIONS B

Fig. 3—Damaged surfaces developed during thermal shock testing: (a) Microcracks that were caused by the thermal shock after 20 cycles and
(b) Plastic deformation around the microcracks at the surface.
The ball-to-powder weight ratio was 5:1. As a process
control agent, stearic acid (C18H36O2) and zinc stearate
were used to prevent excessive cold welding during the
mechanical milling. The powders were mixed by stirring
before being transferred into the ball-mill jar. Mechan-
ical alloying was performed in a FRITSCH Mono Mill
PULVERISETTE (Germany), which is a planetary ball
mill with a revolution speed of 600 rpm. The ball-milling
time was 120 minutes, with an interim period of
30 minutes every half hour to prevent overheating.
After ball milling, the grain size of the mixture was
measured. There was little difference in the grain size
before and after milling (the grain size of the aluminum
was approximately 1 lm[1,2]). The blended powders were
then compacted by cold uniaxial pressing with a green
compact pressure of 250 MPa with the intent of
producing an initial green density ranging from 85 to
95 pct. The aspect ratio of the geometry was 0.85. The
porosity of the specimens after sintering was found to be
between 5 and 10 pct.
The compacted specimens were sintered [893 K
(620 °C) for 3.5 hours] in a ceramic tubular oven under
argon atmosphere to prevent oxidation during the
sintering. A typical microstructure is shown in Figure 1;
this image corresponds to a composite containing
2.5 wt pct Fe3O4 nanoparticles.[1,2] The specimens were
tested under various aspect ratios.
C. Cryogenic-Cycling Behavior of the Composites
A preliminary study of the cryogenic-cycling behavior
of the produced aluminum matrix composites reinforced
with nanoparticles (Fe3O4) was conducted in the frame-
work of the present paper. The interaction between the
matrix and the reinforcing particles was also investi-
gated during cryogenic cycling. For this study, three cut
and polished symmetric laminates were allowed to
equilibrate at 295 K (22 °C) and were then placed into
a liquid nitrogen bath [77 K (196 °C)] for 10 minutes.
Each sample was examined prior to cycling to insure
that there were no initial cracks or defects on the
surface. After exposure to liquid nitrogen, the samples
were placed in a desiccator and allowed to return to
room temperature. Each sample was exposed to a
minimum of four or five cryogenic cycles; afterward,
microcracking was revealed under optical microscopy at
a high magnification at the interface between the
reinforcement and the matrix.
D. Application of Microindentation Tests
Microindentation tests were conducted on the alumi-
num metal matrix composites to explore their mechan-
ical and tribological properties. In this test, the pressure
distribution is focused under the indenter. The subsequent
METALLURGICAL AND MATERIALS TRANSACTIONS B
detection of microscratches is challenging, and the
utilization of the same tip for both scratching and
microimaging may be the best method for microscratch-
hardness testing. It is necessary, nevertheless, that the
experiments be carried out under the best possible
conditions, so the samples must be cleaned and polished
to avoid any corrosion.
This paper presents a detailed comparison of exper-
imental and numerical approaches to microindentation
tests on aluminum matrix composites reinforced with
Fe3O4 nanoparticles. The present study aims to deter-
mine the local yield conditions for a particular material
using a microindentation testing technique; here, the
load-depth penetration curve yields information con-
cerning the indentation hardness and the elastic mod-
ulus. For reproducibility, the experimental results are
compared to a simple FEM, and a good correlation is
found.
Two maximum applied forces were used: 500 and
1000 mN. The creep time was taken to be 2 seconds.
For each specimen, a matrix region was identified on the
specimen for the application of 9 measurements was
taken, and the mean value for each graph was obtained.
A CSM standard indentation test device was used:
MHTX S/N: 50-0121. The loading and unloading speed
was taken to be 1000 mN/min for the maximum applied
load of 500 and 2000 mN/min for the maximum applied
load of 1000 mN.
Additionally, microindentation tests were also carried
out on specimens containing different Fe3O4 weight
Table I. Crack Densities as Surface Percentages, Depending
on the Number of Cryogenic Cycles
No of Cryogenic Surface Percentage
Cycling (Crack Density at Surface) (pct)
5 0.1
10 0.12
12 0.55
15 1.08
20 2.23
22 2.5
26 3.7
Fig. 4—(a) Schematic representation of the force-depth curve for the microindentation procedure and (b) measurement device.
METALLURGICAL AND MATERIALS TRANSACTIONS B
ratios (5, 10, and 20 wt pct) to compare the effect of the
reinforcement quantity on the stiffness values. These
tests were carried out at below the maximum applied
force of 1000 mN, and the creep time was taken to be
2 seconds. For each specimen, a matrix region was
identified on the specimen for the application of
9 measurements, and the mean value for each graph
was obtained.
III. RESULTS AND DISCUSSION
A. General Remarks on the Experiments
The manufacturing of novel Al-based metal matrix
composites reinforced with Fe3O4 nanoparticles is useful
for engineering applications. It is interesting to evaluate
these materials in terms of their mechanical and physical
properties, particularly the optimization of the electrical
and magnetic permeability. Fe3O4 is considered suitable
because of its lower cost and high free energy of
reaction. The low-cost fabrication of this material can
be achieved without difficulty by controlling the pro-
cessing parameters, as has been explained in previous
reports by the present research team.[1,2] In our previous
work, some of the processing parameters and physical
properties (magnetic capacity, etc.) have been deter-
mined; however, we require more comprehensive study
to understand the role of the magnetite Fe3O4 as the
reinforcement and to optimize the manufacturing pro-
cedures. All the detailed results related to the analysis of
the microstructure and the distribution of the particles
in the matrix are shown in Figure 2.
Here, the reinforcing particles are found in the form
of quasi-spherical and/or thin rectangular shapes and
are distributed more or less uniformly in all samples.
Some local clustering still can be found in many of the
samples, especially in samples with higher loadings
(>2 pct).
In fact, a perfectly homogeneous distribution of the
Fe3O4 nanoparticles in the matrix could not be achieved
in most of the specimens examined here because of the
facile agglomeration of the Fe3O4 nanoparticles. As we
have explained in Section II–B, microporosity was
always present in the matrix (between 5 and 10 pct)
because of the uniaxial cold compacting. Microporosity C. Analysis of Microindentation Tests and FEM
appeared even at high compact pressures. We chose the Modeling for the Micromechanical Behavior
uniaxial cold compacting method for the sake of of the Test Specimens
simplicity and low-cost manufacturing. However, this Microindentation testing has become a popular tech-
method was not efficient enough to produce a homoge- nique because of its simplicity and the fact that it
neous particle distribution in the composite microstruc- provides valuable information about the morphology
ture because of the nanoscale magnetite Fe3O4. The and mechanical properties of composite materials.
homogeneity of the microstructure could be improved Microindentation appears to be a promising tool for
using a wet process instead of the dry-mill process that the micromechanical and microstructural investigation
was employed in this study. of composites.[15,16] Microindentation differs from the
classical measurement of hardness, wherein the impres-
B. Cryogenic-Cycling Behavior of Microcrack Evolution sions are generated and then imaged with a microscope.
The load and the associated penetration depth are
At room temperature, magnetite Fe3O4 conducts
recorded simultaneously during both loading and
electricity, though not nearly as well as copper. Its
unloading, producing a force-depth diagram, as shown
conductivity decreases slightly with decreasing tempera-
schematically in Figure 4.
ture until it reaches a Verwey transition temperature of
The Oliver and Pharr Method (Power Law Method)[5]
120 K (153 °C). Below this temperature, magnetite
recognizes the fact that the first portion of the unloading
Fe3O4 essentially becomes an insulator. Such metal-to-
curve may not be linear and can be described by a simple
insulator transition behavior is not in agreement with the
power-law relationship:
single-conduction-band theory, which places magnetite at
a focal point of research. One suggested explanation is
F ¼ kðh  hp Þm ; ½1
that in former theories, electron–electron interactions
were too quickly dismissed. As expected, a continuous where k is a constant, and m is an exponent that de-
increase of saturation magnetization with the increase of pends on the indenter geometry. A power-law function
the magnetite weight fraction in the composites should be is used to describe the upper part of the unloading data:
observed. The coercivity should follow the characteristic  
filler-loading-independent response of soft magnetic mi- h  hp m
F ¼ Fmax ; ½2
croparticles. Another important practical consideration hm  hp
is how well the behavior of the electrical conductivity and
the interface area between the matrix and the reinforce- where the constants m and hp are determined by a
ment are known. What will happen in the structure if this least-squares fitting procedure. The contact stiffness
composite undergoes cryogenic cycling? S = (1/C) is given by the derivative at peak load:
To understand the cryogenic behavior of the struc-   " m1 #
ture, preliminary tests were carried out on the prepared dF hm hp  1
S¼ ¼mFmax  m ¼mFmax hm hp
specimens. In the first stage, the evolution of transverse dh max hm hp
cracking was evaluated as a function of the number of
cryogenic cycles. In general, it was difficult to detect any ½3
crack before 10 cycles had been conducted, and the first and the tangent depth, hr, is therefore given by:
appearance of the crack density was detected from the
10th cryogenic cycle of the tested specimens. Certain Fmax
hr ¼ hm  : ½4
specimens exhibited heavily local plastic deformation in S
which a high crack density formed during cryogenic
cycling. This behavior was attributed to highly concen- The contact depth, hc, is then given as:
trated regions of reinforcing particles that were found to
be significantly agglomerated in the matrix because of hc ¼ hm  eðhm  hr Þ; ½5
the non-homogeneity of the mixture during the com-
pacting stage (Figure 3). In Table I, the crack densities, where e now depends on the power-law exponent m.
depending on the number of cryogenic cycles, are given The tangent is found by differentiating the unloading
as surface percentages. Each result is the mean value of curve and evaluating at maximum load (Fmax). The
three or four specimens that were used for each intercept of this tangent with the displacement axis
cryogenic cycle obtained from software called ‘‘Archi- yields hr.
med.’’ The concentration of the particles and their As indicated above, all the parameters, such as the
distribution in the matrix influence this phenomenon. indentation hardness (HIT), the indentation modulus
Overall, these preliminary results demonstrate that the (EIT) and the Vickers hardness (HV), were determined
processing characteristics of the specimens studied here by the Oliver and Pharr method as follows:
were not harmfully influenced by the presence of the Ap ¼ fðhÞ; ½6
nanoparticles. If the distribution of the nanoparticles
can be made homogeneous in the matrix, the thermal- where Ap is the projected contact area.
expansion characteristics can be improved, and the
Fmax
resistance to thermal-cycling-induced stresses can also HIT ¼ and ½7
be increased. Ap ðhc Þ

METALLURGICAL AND MATERIALS TRANSACTIONS B

 1  m2s prepared for investigating the micromechanical behav-
EIT ¼ 1m2i
and also ½8 ior of these composites. Some of the experimental
1
Er  Ei analysis of microindentation under two different load
conditions is shown in Figure 5 as an example of this
pffiffiffi study. First of all, we obtained the loading and
pS
Er ¼ pffiffiffiffiffiffiffiffiffiffiffiffiffiffi ; ½9 unloading curves (Figure 5(a)) by determining the
2b Ap ðhc Þ evolution of the load and depth as a function of time
(Figure 5(b)). For each set of test conditions, we carried
where Ei is the elastic modulus of the indenter out 12 tests on a matrix region that was determined by
(1141 GPa), mi is the Poisson’s ratio of the indenter the software of the testing program. Afterward, we
(0.07), Er is the reduced modulus of the indentation calculated the mean values.
contact, ms is the Poisson’s ratio of the sample (0.35) Several parameters obtained from the microindenta-
Fmax tion test of a specimen (called Al-I here) are given in
HV ¼ : ½10 Table II. Here, only two different maximum applied
9:81Ap ðhc Þ
loads were used.
Also of interest is the evaluation of the stiffness values
In the framework of this preliminary study, we carried of the specimens containing different Fe3O4 weight
out microindentation tests on certain specimens that we ratios (5, 10, and 20 wt pct) to compare the effect of the
reinforcement quantity on the stiffness values. These
tests were carried out at below the maximum applied
force of 1000 mN, and the creep time was taken to be
2 seconds. For each specimen, a matrix region was
identified on the specimen for the application of nine
measurements, and the mean value for each graph was
obtained.
The stiffness value can give an idea of the measure of
resistance offered by an elastic body to deformation. It
represents the ratio of the force applied on the body to
the displacement produced by the force.
It seems that these composites are very sensitive to
changes in their microstructure under deformation. In
reality, this claim is not completely valid for the stiffness,
as is observed in Figure 6. The stiffness value is very
sensitive to the indenter; for example, in this test, we
used a Vickers indenter, and the material exhibited

3,5

3
Stiffness (mN/nm)

2,5

1,5

0,5

0
AF-2 AF-4 AF-9 AF-11 AF-12
Fig. 5—Experimental analysis of microindentation for the Al-Fe3O4
composite samples: (a) loading and unloading curves and (b) evolu- Fig. 6—Evolution of the stiffness values of the specimens containing
tion of the load and depth as a function of time during microinden- different Fe3O4 weight ratios: (AF-2/AF-11/AF-12: 10 pct, AF-4:
tation testing. 20 pct and AF-9: 5 pct).

Table II. Microindentation Parameters Measured for the Specimen Al-I

Maximum Applied Force (mN) Indentation Hardness HIT (MPa) Indentation Modulus EIT (GPa) Microhardness HV
500 286 6.92 27
1000 284 3.13 26.8

METALLURGICAL AND MATERIALS TRANSACTIONS B

Fig. 7—Geometry of the FEA model (left) and boundary conditions of the model (right).

Fig. 10—Zoom of the stress field showing the stress-gradient homo-

Fig. 8—Mesh distributions of parts. geneity.

Fig. 9—Stresses in the compressed zone. Fig. 11—FE and experimental results obtained for Fmax = 500 mN.

METALLURGICAL AND MATERIALS TRANSACTIONS B

different deformation in the matrix and in the area of
reinforcement (agglomeration effect, etc.); its ability to
recover was reduced considerably, perhaps suggesting
the presence of permanent damage. This seems to be a
strong effect of cold working. Deformation at room
temperature leads to the formation of new dislocations,
which in turn makes further deformation more difficult;
dislocations pile up at the grain boundaries, and there is
an increase in strength.
It is difficult to compare the various composites
because there was little difference between specimens
containing different reinforcement ratios. For example,
for a certain series of measurements taken in a region of
agglomerated reinforcement particles, some values can
be variable, and sometimes these measurements were
different from specimen to specimen even if the speci-
mens contained the same reinforcement ratios. Far more
repetitive tests should be conducted to achieve a much
more thorough comparison.
Using these experimental data, we built a model of a
typical cubic specimen formed of aluminum metal
matrix composite and indented by a rough, rigid,
conical punch. This problem illustrates a typical appli-
cation of a metal matrix composite when used in the
microindentation of rigid deformable materials.
The axis-symmetric build model is shown in Figure 7.
The metal matrix composite specimen has 34 9
34 9 34 mm edges. The punch has a conical geometry
Fig. 12—FE and experimental results obtained for Fmax = 1000 mN.
Table III. FE Results for the First Loading Case (Fmax = 500 mN)
Contact Radius (mm) Fmax (N) Hardness (MPa 9 104)
0.052632913 0.513793 0.055141992
Table IV. Numerical Results with a Maximum Load of 1000 mN
Contact Radius (mm) Fmax (N) Hardness (MPa 9 104)
0.065916527 1.0682 0.072126427
METALLURGICAL AND MATERIALS TRANSACTIONS B
with a maximum diameter of 160 lm. A contact pair is
defined between the punch, which is modeled by a rough
conical rigid surface, and a slave surface composed of
the top face of the axis-symmetric elements in the
contact region. The friction coefficient between the
punch and the metal matrix is 0.2. A point mass of 100 g
representing the weight of the punch is attached to the
rigid-body reference node. The model is analyzed with
Abaqus/Standard, and all parts are meshed with tetra-
hedral linear solid elements, as shown in Figure 8.
The metal matrix composite is defined with the
*Material option using the experimental test data. The
test data are defined in terms of the nominal stress and
nominal strain values. The rough surface of the punch is
modeled by specifying a friction coefficient of 0.2 for
the contact-surface interaction with the *FRICTION
option under the *SURFACE INTERACTION definition.
The numerical model is used to study the behavior of
this composite material. Therefore, we consider the
following configuration of the model. The punch is
applied statically with a maximum load downward to
indent the metal matrix composite, and the relation
between the reaction force and the displacement is
measured for both the purely elastic and elastic plastic
cases.
In Abaqus/Standard, the punch is applied downward
by a prescribed displacement boundary condition in the
first step, indenting the metal matrix composite by an
imposed load. The NLGEOM parameter is specified in
the *STEP option because the response involves large
deformation. In the second step, the punch is displaced
back to its original position. The analyses for both steps
are performed using the *STATIC procedure. During a
*STATIC step, the material behaves according to the
elastic plastic definition using the properties specified
with *Material, *Elastic, and *Plastic for this matrix
composite model. In this case, the punch is pushed down
over a period of one second and then moved back up
again in one second. We define the characteristics of the
equivalent homogeneous material and use these data for
the calculation in the finite element analysis as given
here for two different test conditions.
The deformation and contour plots for oriented
stresses and strains are shown for the elastic plastic
metal matrix composite as obtained from the Abaqus/
Standard analysis in Figures 9 and 10. Although the
metal matrix composite is subjected to large strains, only
Young Module (GPa) Yield Stress (GPa)
30.02796249 0.018380664
Young Modulus (GPa) Yield Stress (GPa)
37.12519685 0.024042142
moderate distortions occur because of the small Pois-
son’s ratio.
It is obvious that the stresses no longer satisfy the
Hertz contact law, as the yield strength has been
exceeded, and plastic deformations are therefore pres-
ent. These figures depict the compressive-load reaction-
force history obtained with Abaqus/Standard for both
steps. As the material is elastic plastic, the stresses relax
during loading and, consequently, lead to a softer
response than in the purely elastic case. A comparison
between the experimental and the FE force–displace-
ment response is shown in Figures 11 and 12. The two
curves exhibit a similar shape, and they are very similar
in the unloading domain. However, a small discrepancy
between the two responses can be observed in the
loading domain. It appears that the numerical data are
higher than the experimental data in the loading
domain. This discrepancy can be attributed to the slip
between the punch and the specimen in the initial
moments of the experimental loading. Additionally, the
hypotheses used in the numerical model are not very
close to the real experimental conditions.
To improve the loading–unloading graph, we have
inserted the equivalent material characteristics ob-
tained under various conditions. The maximum force
of loading was 500 mN in the first case; it was then
taken to be 1000 mN in the second one. The
numerical FE model yields somewhat greater values
than the experimental loading force. These differences
may be attributable to the experimental conditions,
such as the smoothness of the contact surface. If we
gradually decrease the motion, we can obtain an idea
of the loading force that initiates plastic deformations.
In the FE model, a cone tip is used as a rigid indenter
punch. The metal matrix composite material is defined
with the following numerical characteristics associated
with the results presented for both cases in Tables III
and IV.
IV. CONCLUSIONS AND REMARKS
This research project investigated the low-cost man-
ufacturing of novel Al-based metal matrix composite
materials reinforced with Fe3O4 nanoparticles for use in
aeronautical engineering. This low-cost manufacturing
process can be performed without difficulty at the
laboratory scale by simply controlling the processing
parameters. The procedure described here contains
significant new synthesis modifications, which were
predominantly developed at the chemical process labo-
ratory in Paris. However, a considerable agglomeration
phenomenon was observed during the processing of the
specimens, as we have explained in the previous sections.
This production method was not efficient enough to
produce a homogeneous particle distribution in the
microstructure of the composites. The homogeneity of
the microstructure could be improved using a wet
process instead of the dry-mill process that was
employed here.
The cryogenic-cycling behavior of the composites
was evaluated. The evolution of the transverse
microcracking was evaluated as a function of the
number of cryogenic cycles. The crack densities depend-
ing on the number of cryogenic cycles were given as
surface percentages by the software ‘‘Archimed.’’ It was
found that the concentration of the reinforcing particles
and their distribution in the matrix can influence the
microcracking phenomenon. Overall, these preliminary
results demonstrated that the processing characteristics
of the specimens studied here were not harmfully
influenced by the presence of the nanoparticles. If the
distribution of the nanoparticles can be made homoge-
neous in the matrix, the thermal-expansion characteris-
tics can be improved, and the resistance to thermal-
cycling-induced stresses can also be increased.
Microindentation is presently becoming an essential
tool for the optimization of the micromechanical prop-
erties of composite materials. When rigidity and tough-
ness are important, modeling microindentation tests
with the finite element approach provides valuable
complementary information to the experimental micro-
indentation data.
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