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Met. Mater. Int., Vol. 19, No. 1 (2013), pp.

105~112
doi: 10.1007/s12540-013-1017-2

Technology for Obtaining Samples of Layered Composite Materials


with Metallic Matrix
Dumitru Nedelcu

1,*

and Ioan Carcea

Gheorghe Asachi Technical University of Iasi, Faculty of Machine


Manufacturing and Industrial Management, Department of Machine Manufacturing Technologies,
Blvd. D. Mangeron No. 59A, 700050 Iasi, Romania
2
Gheorghe Asachi Technical University of Iasi, Faculty of Materials Science,
Department of Materials Science, Blvd. D. Mangeron No. 41, 700050 Iasi, Romania
(received date: 27 December 2011 / accepted date: 23 February 2012)
Layered composite materials significantly improved the mechanical process of fracturing, which means
better fracture strength, while preserving surface properties such as hardness, resistance to wear and resistance to high temperatures. The properties are significantly influenced by the interphase mass transfer at
the surface matrix-fiber reinforcement. We developed a mathematical model to determine the molar flux at
the interface in stationary and in a nonstationary regime. The technological parameters are: hydraulic pressure, reinforced material, alloy type, fiber diameter, mass ratio between the reinforcement and the composite masses and mould preheating temperature. A mould patented in Romania was mounted on a hydraulic
press to obtain the samples. We studied the material structure, matrix and fiber element distribution, metallic
matrix element distribution and matrix and fiber element content variation. The results recorded revealed a 75%
to 120% increase of the fracture strength, which means an improvement of the mechanical process of fracturing. We concluded that the reinforcement material, mass ratio and fiber diameter have a significant
influences on the fracture strength.
Key words: composites, diffusion bonding, mechanical properties, scanning electron microscopy (SEM)

1. INTRODUCTION
Metals and alloys are generally produced and shaped in
bulk form but can also be intimately combined with another
material that serves to improve their performance: The
resulting material is a metal matrix composite (MMC). This
class of composites encompasses many different materials
that can be distinguished according to their base metal (e.g.,
aluminum, copper, titanium); according to other factors such
as, reinforcement or phase (e.g., fibers, particles, whiskers); or
according to their manufacturing process (e.g., powder
metallurgy, diffusion bonding, infiltration, stir casting) [1].
The choice of traditional materials used in high precision
technology processes are strongly influenced by the materials own performances and processing procedures.
The major advantage of multi-layered composite materials, as compared to classical materials is the possibility to
change the materials thermal and mechanical properties,
which may vary considerably [2]. The possibility to combine
*Corresponding author: dnedelcu@tcm.tuiasi.ro
KIM and Springer, Published 10 January 2013

several materials of different types and with distinct physical


properties into one monolithic multi-layered material enables
specialists to create materials the functional purposes of
which are extremely different, such as: impact and high temperature resistant materials, wear resistant materials, and
materials that enhance or, on the contrary, prevent heat conduction.
As far as fracture strength is concerned, the most interesting composite materials are those in which fragile layers, which enjoy high elasticity and low ductility (ceramics,
refractory metals, intermetallic compounds), and high ductility layers alternate.
The main purpose of such composites is the significant
increase of the mechanical work of fracturing, which means
better impact resistance, while preserving the surface properties, i.e. hardness, resistance to wear and resistance to high
temperatures [3,4].
In fact, many long-range applications combine porous and
continuous layers; porous layers may be made up of powder, fibers or conglomerates. A layered structure is inherent
for many reinforced composites including continuous fiber
(for instance, if the layers comprise different fibers). Finally,

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Dumitru Nedelcu and Ioan Carcea

composites will be made of identical layers of continuous


unidirectional fibers. These composites are designed in such a
way as to reduce cross anisotropy, whereas the neighboring
layers are only subjected to changes of the reinforcement
material direction (most of the time, these directions are
perpendicular on one another) [5].
More recently, novel multiscale simulation strategies based
on embedded cell models in three dimensions have been
used to predict the toughness and notch sensitivity of fiberreinforced MMCs (133). The representation of the material
in front of the notch tip - where damage is concentratedincludes the actual fiber/matrix topology in the composite,
whereas the rest of the solid is modeled as a linear thermoelastic, transversally isotropic homogeneous solid [1].
Generally speaking, regular structures with periodic planeparallel layers are the most frequently found, as they enjoy
a bidirectional isotropy: in the layer plane and perpendicularly on the layers. There are, however, composites containing
other symmetry elements, such as unidirectional undulated
layers or cylindrical or spherical layers. There are several
types of stratified systems, namely systems the geometric
parameters of which have random values or systems without symmetry elements (irregular composites) [6].
In this last category, it is necessary to distinguish the socalled quasiregular structures, which, although lacking symmetry elements, are very close to regular structures, which means
that their structural parameters vary within narrow limits [7].
Figure 1 shows examples of layered composites with regular structure [2]. Two of the mechanical properties playing
a major role in structural material operation may be considered: modulus of elasticity and mechanical work of fracture. These characteristics govern the behavior of a stressed
structure, more precisely the stresses of the critical elastic

Fig. 1. Types of stratified composites with regular structure: (a) planeparallel layers A, B; dt is the distance of transition from one layer to
another in the direction perpendicular to the layers, (b) parallel corrugated layers, dt and lt are regular distances in the two directions (X and
Y), (c) coaxial layers with constant thickness in a cylinder, and (d)
ball, separate layers of spherical thickness.

strain level and the capacity to bear overloading. The full


description of the elastic properties of a layered composite
with elastic isotropic phases requires information on the
angular dependence of at least two characteristics, namely,
in most cases, the E modulus and Poissons ratio n. Youngs
modulus of a perpendicularly layered composite may be
determined as a mean only for non-elastic layers that are in
contact with one another. The transverse strain of each layer is
determined using Poissons ratio. If the layers are interconnected, their transverse strains should be equal, which would
lead to additional elastic stress or compressive stresses along
the layers. When Youngs modulus and Poissons ratio are
known for a specific layered composite, the acoustic oscillation conveyance rate may be determined for the two main
axes. The joining of the layers of a composite material is
designed to increase the fracture strength or mechanical
work of fracturing of the composite as a whole, while preserving its main functional properties.

2. EXPERIMENTAL PROCEDURES
From the very moment they are incorporated in the liquid
metallic matrix, the reinforcement fibers are in permanent
contact with the alloy. The manner in which the interaction,
mass transfer and static equilibrium stages succeed each
other depends on the temperature, and pressure, and on
possible changes in the chemical composition. During the
manufacturing process, when the liquid alloy is characterized by continuous movement, the diffusion and the mass
transfer at and from the interface liquid alloy - fiber take place
under a stationary regime. After the fiber pre-forms are
infiltrated, as well as after solidification there may appear
conditions for stationary regime diffusion at the interface.
When solidification occurs, the kinetics of the biphasic system processes is conditioned by the non-stationary regime
diffusion of the elements at and from the interphase limit.
Depending on the nature and state of the components, the
factor limiting the complex processes taking place during
the manufacture and solidification of composite materials
may be either the diffusion and mass transfer in heterogeneous systems or the chemical interaction at the interface
level.
The processes taking place on the surface of reinforcement fibers that are completely incorporated in the metallic
melt may be limited either by the resistance to the mass
transfer of a thin static film that covers the fiber or by the
rate of the heterogeneous chemical reactions.
For a radius R fiber whose surface interacts with the liquid alloy in which it is immersed the following possibilities
arise: the chemical reaction rate can be much higher than
the diffusion rate; the diffusion rate can be higher than that
of the chemical reactions and the diffusion rate and the
chemical reaction rate can both be reduced and can act as

Technology for Obtaining Samples of Layered Composite Materials with Metallic Matrix

107

and r=R1, we obtain the concentration gradient on the fiber


surface, and by replacing these in Relation (4) we obtain
the molar flux on the surface.
(JA,r)S = (R2CDA-P)/(mR1(R2-R1)) ln((1-mXA2)/(1-mXA1))
(6)
Generally speaking, the concentration of element A in the
melt is rather low and the logarithmic term can be developed in
Taylor series. If the superior power terms are neglected, we
obtain:
(JA,r)S=(R2CDA-P)/(mR1(R2-R1)) (XA1-XA2)
Fig. 2. Diffusion to and from the particle surface.

limiting factors in the process.


When element A diffuses through a liquid static film with
R2-R1 thickness (Fig. 2) toward the interphase surface, the
equation of the JA,r radial molar flux can be deduced from
the equation of continuity in spherical coordinates of incompressible liquids in which ur (radial speed) is equivalent to
radial flux JA,r.
d(r2JA,r)/dr = 0 for R1 < r R2

(1)

The interface relation is:


aA + B = bP + R

where A and B are the reactants, A from the liquid and B


from the particle; P and R are the reaction output, P is liquid and R is solid.
Since the liquid reaction output diffuses in the opposite
direction, we may write:
aJA,r = bJP,r

(3)

The molar flux is:


JA, r = (CDA-PDXA)/(1-mXA)dr

XA = XA1 for r = R1
XA = XA2 for r = R2
we obtain:
(5)

This relation establishes the distribution of element A in


the static liquid film that surrounds the fiber.
By deriving Eq. (5) with respect to the conditions XA=XA1

(8)

where kd is the mass transfer coefficient; tc represents the


contact time of the element with the surface; CA,o is specimen As surface concentration and CA,v is specimen As
concentration in volume.
The mass transport through the spaces between the fibers
may be equated with the one occurring in the capillaries.
As a result, the diffusion the coefficient can be calculated
with Equation (9).
Dc = (/)L

(4)

where DA-P is the diffusion coefficient or diffusivity, C is


the molar density of the liquid, m=1-a/b and XA represents
the molar fraction of element A.
If for CDA-P = constant and m0 JA,r is replaced from Equation (4) into Equation (1) and is integrated in the limits:

(1/R1-1/R2)ln((1-mXA)/(1-mXA1))
= (1/R1-1/r)ln((1-mXA2)/(1-mXA1))

In order to evaluate the interactions taking place at the


interface and the superficial phenomena changes it is particularly important to know the size of the molar flux of the
superficial elements that are active on the reinforcement
fibers surface.
During the pouring manufacturing process of metallic
matrix composite materials there occur mass transfer processes in the non-stationary regime and also, and only accidentally, in a zonal regime at the equilibrium point. Thus,
during the infiltration of the fiber pre-forms, as well as during the pouring and solidification processes mass transfer
occurs in the non-stationary regime, which makes it possible to apply Higbies model:
JA,r = (2DA-P/tc)1/2(CA,o-CA,v) = kd(CA,o-CA,v)

(2)

(7)

(9)

where is the surface stress, represents viscosity, L is the


average atomic displacement and is the unit permeability.
In order to obtain a sample of the layered composite
materials, the mould presented in Fig. 3 was designed and
built. This mould was patented according to the Romanian
OSIM system [7] and was mounted on a minimum 40tf
hydraulic press.
Thanks to this mould, the composite material created may
be easily sampled. The mould includes the following components: a) fixed mould assembly (1) including a base plate
(5) fastened by screws (10), on which another plate (6) is
mounted, which supports a compression mould (7) with a
lower cover designed for material sampling; b) punch assembly
(2) made up of a punch plate (11) and a punch (13) and fastening plate (12) with screws (14); c) a handle (8) used to
lift the compression mould (7) equipped with lifting rods

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Dumitru Nedelcu and Ioan Carcea

Here are the advantages of this technique: extra energy,


faster solidification and less equipment wear; better filling
of the pouring mould due to alloy static flow; pore reduction; and manufacture of reinforced parts using a single
operation. The proposed technology can be developed in
industry without great investments because it can use mills
that already exist in production workshops. The remarkable
properties of layered composite materials justify the design
and construction costs incurred in building pressing moulds
for liquid matrix alloys.

3. RESEARCH AND RESULTS

Fig. 3. Equipment to obtain samples of layered composite materials:


1-fixed die assembly, 2-punch assembly, 3-removable ring, 4-temperature sensor, 5-base plate, 6-upper plate, 7-compression mould, 8-handle, 9-lifting rods, 10-screws, 11-punch plate, 12-fastening plate, 13punch, 14-screws.

(9) and a spacer ring under the compression mould (7), used to
lift the composite material sample; d) a sampling ring (3)
and e) a temperature sensor (4).
The layered composite manufacturing process requires the
observance of the following stages: manufacture of alloy with
the required chemical composition; pouring mould preheating
at 200 to 300 C; lubrication of the active mould surface
using colloidal graphite; transfer of the semi-fluid suspension in the metallic matrix cavity; fastening of the matrix
onto the hydraulic press table; application of pressure until
full part solidification occurs; composite material removal
from the matrix; matrix cleaning.
All the parts touching the liquid metal are covered with a
graphite film, in order to diminish the friction between the
parts and to limit corrosion.
In addition to its improving the mechanical properties by
decreasing the inner flaws (pores), liquid forging allows
improving of size tolerances and part surfaces, making them
ready to use.
Liquid forging is currently very frequently used in industry for the manufacture of many ferrous or non-ferrous alloys.
The method has been successfully used both on semi-solid
alloys with high melting points and on low melting point
alloys. It has also been increasingly used in CMM.
When conducted under pressure, liquid forging changes
the alloy solidification conditions.

The planning of the experiments was achieved by means


of the Taguchi methodology [9].
The model proposed by Viger and Sisson is also easy to
study; this is the matrix model of the system comprising I
factors: F1, F2 ... Fi each factor having ni levels. Each experiment was conducted three times. The proposed matrix model
takes into consideration six technological parameters with
two levels (Table 1). We will try to determine the coefficients
of a type (10) model:
Zt = M+Pa+Mat+A+D+Rm+Tp+PaMat+PaA+PaD+PaRm
+PaTp+MatA
(10)
where M is the general average grade; Pa represents the
hydraulic pressure, [MPa]; Mat represents the reinforced
material; A is the type of alloy used; D is the fiber diameter; Rm is the mass ratio between the reinforcement and
composite masses; and Tp is the metallic matrix preheating
temperature [C].
After the orthogonality and number of degrees of freedom conditions were analyzed, there were 16 experimental
tests to be made.
We proceeded with the analysis of the model graph (Fig.
4(a)) which was compared with the standard graph (Fig.

Fig. 4. Taguchi graphs: (a) for model: Pa represents the hydraulic pressure, Mat represents the reinforced material, A is the type of alloy
used, D is the fiber diameter, Rm is the mass ratio between the reinforcement and composite masses, Tp is the metallic matrix preheating
temperature, and (b) standard.

Table 1. Variation levels of input parameters


Input parameter Levels
First level
Second level

Pa [MPa]
75
100

Mat
Stainless steel mesh with 1.4 mm eye
Fiberglass mesh with 1.4 mm eye

A
AlSi5Cu3Mg
AlSi7Cu2Mg

D [mm]
0,5
0,3

Rm
10
20

Tp [C]
25
125

Technology for Obtaining Samples of Layered Composite Materials with Metallic Matrix
Table 2. Assigned columns of independent factors
Factors
Tests number
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16

Pa

Mat

Rm

Tp

1
1
2
2
1
1
2
2
2
2
1
1
2
2
1
1

1
1
2
2
1
1
2
2
1
1
2
2
1
1
2
2

1
2
1
2
2
1
2
1
1
2
1
2
2
1
2
1

1
2
1
2
2
1
2
1
2
1
2
1
1
2
1
2

1
2
2
1
1
2
2
1
1
2
2
1
1
2
1
1

1
2
1
2
1
2
1
2
1
2
1
2
1
1
2
2

Fig. 5. Average effects of input parameters on tensile strength.

109

4(b)); we thus obtained the assignment of the columns of


independent factors (Table 2).
Figure 5 shows the mean effects of the input parameters
on the fracture stress. According to the graphs in Fig. 5, the
fracture stress is higher if the reinforcement material is a
steel mesh, due to the better adherence of the reinforcement
matrix and to the lower fragility of the stainless steel fibers
as compared to glass fibers. The higher the reinforcement
ratio, the higher the fracture stress, at least in the presence
of lower ratios. Increasing the tensile strength with the fiber
diameter is available at low values. Increasing the diameter
leads to a decrease of the tensile strength because of reinforcement effect reduction. The quality of the matrix alloy
also has a certain influence on the fracture stress, which is
noticeable at least until the yield point is reached. The pressure applied by the piston influences the mechanical characteristics both by its effect on the matrix alloy and by its
adherence to the reinforcement material, as well as by removing certain pouring flaws. The reinforcement preheating

110

Dumitru Nedelcu and Ioan Carcea

temperature has a moderate effect on the mechanical characteristics as a result of the effect the former has on the adherence between the matrix and the reinforcement material.
The fracture strength of a composite material with a metallic
matrix is strongly influenced by the following factors: matrix
fracture strength, reinforcement fracture strength, reinforcement volume (its shape and distribution) and the amount of
intermetallic interface compound. A perfect interface of a
composite material involves the presence of a matrix-reinforcement reaction product, one that does not diminish the
stress bearing section of the reinforcement material.
The tensile test was performed according to the EN
10002-1 European standard, on an INSTRON 3382 (USA)
universal testing machine running Bluehill Series IXTM
software. Here are the sizes of the cylindrical specimen used:
4 mm calibrated diameter, 20 mm inter-mark length, 70 mm
total length and 1 mm/min cross-piece speed. Here are the
equipment characteristics: 100 kN load rating; 0.005 mm/min.
minimum speed; 500 mm/min. maximum speed; 0.0598 m

Fig. 6. Characteristic curves: (a) base alloy, and (b) composite material obtained.

displacement measurement resolution; 0.5% load cell precision; 0.5% displacement transducer precision.
Here are the testing parameters: cross-piece progression
speed vd = 1,0 mm/min; strain temperature = 23 0.5 C (air
conditioned laboratory).
Figure 6(a) shows results for the tensile test conducted on

Fig. 7. The SEM and EDX images in the case of fiberglass reinforcement: (a) image of fibers embedded in aluminum metal matrix (SEM), (b)
elements of the matrix and fiber distribution (EDX), (c), and (d) varying content and fiber matrix elements along the line of the first image.

Technology for Obtaining Samples of Layered Composite Materials with Metallic Matrix

111

Fig. 8. The distribution of elements in the matrix of Al: (a) distribution of elements in Al matrix alloy and stainless steel fibers (EDX), (b) distribution of aluminum inside the matrix, and (c) distribution of silicon inside the matrix.

the base alloy, whereas Fig. 6(b) shows results of the number 9 tensile test.
The image in Fig. 7(a) (SEM-Scanning electron microscope) shows a break area where the glass fibers appear
distributed in different planes from the pressing direction.
Figure 7(b) (EDX-Energy-dispersive X-ray spectroscopy)
shows the distribution of chemical elements on both the
rupture area and the outer surface of the workpiece. The images
in Figs. 7(c) and (d) shows the distribution of elements
along a reference line (Fig. 7(c)) that passes both inside the
rupture area and inside workpiece surface. It can be observed
that on the exterior the workpiece is covered with a layer of
Al alloy and inside the rupture area the O2 content variation
is similar to that of Si. From the image shown in Fig. 7(d) it
can be seen that the Al distribution is not uniform due to
the uncontrolled nature of the fiber direction in the perpendicular plane due to the means of pressing. Another result
is the focus on the distribution of elements in the Al matrix
alloy and the stainless steel fibers (EDX) (Fig. 8(a), this
includes) the distribution of aluminum inside the matrix
(Fig. 8(b)) and the distribution of silicon inside the matrix
(Fig. 8(c)).

4. CONCLUSIONS
Layered composite materials may be used in numerous
fields and industries, depending on their mechanical properties. The layered composite material we created enjoys
virtually double the fracture strength of the basic material
that was used, which means a significant improvement of
the mechanical work of fracturing. Estimation of some properties of multilayer composites can be done by applying
mathematical models of mass transfer at the interface of the
matrix-fiber reinforcement. Distribution of elements in the
fiber-matrix interface, highlighted by EDX analysis, confirms the mathematical model of molar flux established.

The parameters that were considered, i.e. hydraulic pressure,


reinforcement material used (glass fiber and stainless steel
mesh), type of alloy used, reinforcement fiber diameter, as
well as pressure application time and compression piston
diameter describe perfectly well the technological process
of layered composite material manufacture. The fracture
stress is higher when the reinforcement material is a steel
mesh, due to the higher matrix adherence to the reinforcement material, and to the lower fragility of stainless steel
fibers as compared that of glass fibers. The higher the reinforcement proportion, the higher the fracture stress, at least
in the presence of lower ratios between the reinforcement
and composite mases. Increasing the tensile strength with
the fiber diameter is available at low values. Increasing the
diameter leads to a decrease of the tensile strength because
of reinforcement effect reduction. The quality of the matrix
alloy considerably influences the fracture stress, at least until
reaching the yield point, while the pressure applied by the
piston influences the mechanical characteristics both by the
effect on the matrix alloy and by the pistons adherence to
the reinforcement material, as well as by removing certain
pouring flaws. The preheating temperature has a moderate
effect on the mechanical characteristics, as a result of the
effect the former has on the adherence between the matrix
and the reinforcement material. Our results revealed a 75%
to 120% fracture strength increase, which triggers an increase
of the mechanical work of fracturing. The proposed technology can be developed in industry without great investment
because it can use mills that already exist in production
workshops. The remarkable properties of layered composite
materials justify the design and construction costs incurred
in the building of pressing moulds for liquid matrix alloys.
The paper provides new information concerning the processing and investigation of layered composite materials with
aluminum alloy matrix, reinforced with metal mesh and
characterized by special properties.

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Dumitru Nedelcu and Ioan Carcea

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