Composites Part B 162 (2019) 397–410

Contents lists available at ScienceDirect

Composites Part B
journal homepage: www.elsevier.com/locate/compositesb

Experimental and numerical study of Al-Nb2Al composites via associated T

procedure of powder metallurgy and thixoforming
H.M. Enginsoya,∗∗, F. Gatamortab, E. Bayraktarb,c,∗, M.H. Robertb, I. Miskioglud
a
Department of Mechanical Engineering, Uşak University, Uşak, Turkey
b
University of Campinas, UNICAMP/FEM-Dept. of Materials, Campinas, SP, Brazil
c
Supmeca -Paris, Mechanical and Manufacturing Engineering School, France
d
Michigan Technological University ME-EM Department, Houghton, MI, USA

A R T I C LE I N FO A B S T R A C T

Keywords:
Recycling of fresh scrap aluminium
Cost effective engineering
Combined powder processing + thixoforming
Intermetallic based composites
Finite element analysis (FEA)
In this study powder metallurgy and thixoforming methods are used together to manufacture aluminum alloy
based composite materials reinforced with Nb2Al particles and glass bubbles (GB). Fresh scrap recycled alu-
minum chips, AA7075 received mainly from Brazilian aeronautic industry, are used as the raw material.
Processing parameters of the manufacturing techniques were optimized and the distribution of the reinforcing
particles as well as their interfaces with the matrix were analyzed. The mechanical properties of the newly
designed composite material were determined by compression and bending tests. Very detailed interface analysis
and microstructure and fracture surface evaluations were performed by Scanning Electron Microscopy (SEM).
The results indicate that the proposed combined powder metallurgy and thixoforming method yields metal
matrix composites with good mechanical properties. A non-linear finite element model (three dimensional) was
used to simulate the bending and compression behaviour of Al-Nb2Al composites. A subroutine, VUHARD, was
written to use with ABAQUS to analyze the effect of thixoforming and sintering on the micro and macrostructure
of the manufactured materials. Different ratios of reinforcing particulates (Nb2Al, Glass Bubbles) used in the
experimental specimens were used in Representative Volume Element (RVE) for the microstructure modeling.
Numerical models for the macrostructure were created using these micro-structures. It has been observed that
there is a good agreement between numerical analysis and experimental results. Proposed process offers an
original method for the production of newly designed composite material from recycled waste aluminum that
can have a major impact on the energy consumption in the aluminum industry, and when enhanced with the
numerical tools for simulation it can lead to the development of better performing materials for the aviation
industry.

1. Introduction
One requirement to increase the efficiency of an aircraft engine is to
increase the operating temperature of its several constituents. The
maximum limit in the temperature-stress integration for nickel based
super alloys commonly used in these engines have almost been reached
and further increase in temperature needs the use of new alloys [1,49].
New generation composites reinforced with intermetallics are pro-
mising to fulfill this requirement. These are structural materials re-
sistant to high temperatures and oxidation and known for their physical
and mechanical properties, which are suitable for aeronautical and
automotive engineering applications [2].
Among the new refractory metals for advanced gas turbine
applications, niobium (Nb) with its medium density and high melting
point good potential to be used as a base in new alloys.
In addition, at high temperatures the mechanical properties of
commercial Nb alloys are very low, and its oxidation resistance needs to
be improved by the addition of significant amounts of Ti and Al. These
alloy compositions lead to the formation of ordered intermediate me-
tallic phases [2–5]. Due to the brittleness of intermetallic compound
materials at room temperature, the application areas of these materials
have been limited. Another study on microstructure of Nb-Aluminates
[6] has shown that the microstructure was indicated entirely as eutectic
alloys and growth directions of these eutectic intermetallics were
“001”.
By adding ductile reinforcements in various forms, the toughness of

∗
Corresponding author. Supmeca -Paris, Mechanical and Manufacturing Engineering School, France.
∗∗
Corresponding author.
E-mail addresses: murat.enginsoy@usak.edu.tr (H.M. Enginsoy), bayraktar@supmeca.fr (E. Bayraktar).

https://doi.org/10.1016/j.compositesb.2018.12.138
Received 5 August 2018; Received in revised form 25 December 2018; Accepted 30 December 2018
Available online 31 December 2018
1359-8368/ © 2018 Published by Elsevier Ltd.
H.M. Enginsoy et al.
intermetallic compound matrix composites is increased. In fact, for the
strengthening of thermodynamically stable and not very brittle inter-
metallic phases, it is necessary to examine the nature of the phases at
equilibrium and transformation temperatures [3–7,49].
About 30 years ago, research on intermetallic compound materials
had intensified in order to substitute these for super alloys. These works
were aimed mainly at manufacturing of automotive parts. Nb-
Aluminates are well known as lightweight materials with high strength
and good creep resistance at high temperatures [8]. Later, some of the
researches have shown that the Nb-Al system intermetallic compounds
can be used very well for replacing super alloys as alternative inter-
metallic compounds produced with different manufacturing processes
(foundry, powder metallurgy-sintering and/or sputtering, etc.) [9–11].
However, all of these intermetallic compound materials were used as
matrix in the manufacturing of the different parts [2,10–17].
Lately, the most convenient combination of efficient tests and
modern numerical tools have been presented for the accelerated design
of Nb-based superalloys [2,13,17]. In this study, it was envisaged to
accelerate the evaluation of the thermodynamic and kinetic databases
providing the comprehensive predictive design of the multi-phase mi-
crostructures. Also in these situations were included multi-component
microstructures as the dynamic systems for the phase stability of the
solid solutions and intermetallics. The experimental results show that
this intermetallic compound has a high potential to combine oxidation
resistance and creep strength at applications at 1300 °C and above [13].
A new idea to manufacture the designed composites has been pro-
posed in this study, i.e., a combined technique was used in which a pre-
compacted mixture of metal matrix and reinforcement material was
processed by powder metallurgy followed by thixoforming [18]. High
strength aluminum alloy fresh scrap AA7075 chips that result from the
machining processes in the aviation industry were used as the matrix
material. As such, recycled fresh scrap materials (AA7075 chips) were
repurposed into new and novel materials. Novelty and originality of
this comprehensive work is in the use of Nb2Al intermetallic compound
as a reinforcement element with glass bubbles in the aluminium matrix.
In addition and we have developed a new idea for using a detailed
Finite Element Analysis to analyze the influence of the thixoforming
and sintering manufacturing methods on the micro and macrostructure
of the composites. For this special case, a subroutine, called “VUHARD”
was written and used in the commercial Abaqus/Explicit software.
We have basically used Nb2Al intermetallic compound as a re-
inforcement element due to its good interface with the matrix [18],
with glass bubbles. Glass bubbles increase the damping capacity of
certain parts made of composite materials. They are also resistant to
high temperatures (∼750 °C) [5].
The mechanical properties of the produced composite materials
were investigated by compression and bending tests. Interface analysis,
microstructure and fracture surface evaluation of four different com-
positions were carried out with Scanning Electron Microscopy (SEM).
The process outlined above offers an original occasion for the pro-
duction of newly designed composite material from recycled wastes
which are especially significant in the aluminum industry as it offers
significant energy savings during production.
2. Materials processing and a novel composite design
Aluminum alloy AA7075 (5.1wt%Zn, 2.2wt%Mg, 1.5wt%Cu) was
used as the metal matrix [48]. This alloy was received as chips recycled
from machining of aeronautical parts. The chips were subjected to
conventional ball milling to reduce their dimensions. These chips are
presented in Fig. 1 with DSC diagram to determine the evolution of
liquid fraction depending on the temperature. Initial chip dimensions
were less than 1–1.5 mm. In this Figure, the mass fraction of liquid was
also shown obtained with “Scheil condition.” The purity level of Nb2Al
was found to be 95%. The particle size of Nb2Al varied from 10 μm to
30 μm as measured with a Laser Granulometer Density of Nb2Al was
398
Composites Part B 162 (2019) 397–410
measured as 6.87g/cm3. The density of the glass bubbles were 0.20g/
cm3and they were hollow spheres with diameters that ranged from
2 μm to 20 μm.
As the basic reinforcement, Nb2Al intermetallics were used in this
work. The reinforcement Nb2Al particles were added directly to the
aluminum matrix at the levels of 30, 40, 50 and 60 wt%. Ball milling
with a ratio of ball to powder 20:1 was used to attain a homogeneous
distribution of Nb2Al in the matrix. The duration of this step was 2
hours. Then the glass bubbles were blended into the mixture and ball
milling was performed for 1 hour with a conventional milling device to
achieve a homogeneous distribution of glass bubbles in the structure.
The Brazilian Nb company supplied fresh scrap Nb2Al compound. This
compound was analyzed by XRD and X-ray diffraction (Fig. 2). All of
the intermetallic compounds were cleaned meticulously and then high
speed milled during 1 hour before they were mixed with aluminium
powder. Before (left column) and after milling (right column) status of
Nb2Al intermetallic powders are shown in Fig. 3. Thus, very hard
particles were milled by using high speed milling device (4000 rpm)
[5].
A binary phase diagram of Nb-Aluminium couple is shown in Fig. 4.
With regard to this phase diagram, composite materials developed in
this study are located in certain intermetallic regions (Nb2Al) [5].
In Fig. 5, Differential Thermal Analysis (DTA) results of Glass
Bubbles (GB) powders are shown. From DTA curves, the temperature-
transformation points of the Glass Bubbles (GB) are observed in detail.
In the same figure images of Glass Bubbles (GB) powders obtained by
Scanning Electron Microscopy (SEM) are also presented. Glass Bubbles
reacts by adding about 5% mass when heated from room temperature to
140 °C. The reason for this may be some chemical reactions in Glass
Bubbles and this situation must be investigated further. Hollow glass
spheres have very low density and these diameters of 2–20 μm are
perfectly rounded (0.20 g/cm3) [48].
Thixoforming experiments to produce graded composites were
performed. After milling, the blended powder was heated to promote
the formation of the appropriate liquid fraction in the metal alloy and to
obtain the semi-solid, thixotropic material. Heating temperature was
chosen according to thermodynamic calculations using a commercial
software; simulations were made using “Scheil condition.”
Thixoforming temperature was defined as 625 °C, corresponding to a
liquid fraction of 50% and the material was held at this temperature for
15 minutes and then thixoforming operation was performed at a pres-
sure of 20 MPa.
In order to compare the composites manufactured by sintering or
thixoforming, part of the blended powder was compacted by cold iso-
static pressing (CIP). A green compact pressure of 400 MPa was used
that resulted in initial green density ranging from 85% to 95% of the
theoretical value [50]. Then the sintering processing was carried out.
Sintering temperature was fixed as 640 °C. Two different composite
groups with no glass bubbles and 5% by volume glass bubbles were
prepared for thixoforming process [5].
All of the products were then tested in quasi static compression and
bending, performed with a servo-hydraulic INSTRON Universal test
device (model Instron 5500R, equipped with a load cell of 250 kN).
Microstructures and fracture surfaces of the tested composites were
observed by using Scanning Electron Microscopy (JOEL-SEM) [48].
3. Finite element simulations
Simulations of micro and macrostructure of the metal matrix com-
posites manufactured in this study were performed with Abaqus/
Explicit®, commercial software. To analyze the effect of the thix-
oforming and sintering manufacturing methods on the micro and
macrostructure of the composites a subroutine, VUHARD, was written
to use with Abaqus. Different ratios of reinforcing particulates (Nb2Al,
Glass Bubbles) used in the manufactured composites were used in
Representative Volume Element (RVE) for the microstructure modeling.
H.M. Enginsoy et al.
Fig. 1. a) Aluminium chips from AA7075 as matrix materials and b) with DSC diagram for this chip and also, c) Mass fraction of liquid obtained with “Scheil
condition”.
Numerical models for the macrostructure were created using these
micro-structures. Furthermore, modeling of reinforcement particles and
their interactions with the aluminum matrix phase was achieved using
the Cohesive Zone Model ascribed to brittle fracture (CZM) [19–23].
The component properties in the modeling are shown in Table 1.
Three point bending and compression test simulations were carried
out with the finite element method and the effect of micro and mac-
rostructure of the simulated samples were investigated in detail.
Numerical and experimental results have shown a good agreement.
3.1. Modelling of micromechanical structure
Microstructural modeling was done in two stages. In the first stage,
the reinforcement particulates were introduced into the matrix phase
and distributed within RVE to obtain a realistic heterogeneous dis-
tribution of the particulates. In the second stage, modeling of the pro-
duction method (thixoforming and sintering) and their effect on the
microstructure was performed.
3.1.1. Constituents modelling
Icosahedron geometry that was used for numerical modeling of a
399
Composites Part B 162 (2019) 397–410
single Nb2Al particulate is shown in Fig. 6(a), and randomly distributed
Nb2Al particulates in the unit volume element is illustrated in Fig. 6(b).
When the microstructure of the manufactured composites was in-
vestigated, it was found that the microstructure resulted from thix-
oforming and sintering was quite different. In the next sections 4.1 and
4.2, the experimental mechanical behavior of the samples obtained by
sintering and thixoforming production methods (compression and 3p
bending) is shown to be different and the production methods cause
different internal structure. For this reason, finite element modeling is
developed in this context. It was also observed that the initial damage
that led to the failure of the specimens occurred at the interface be-
tween the hard particles (Nb2Al compounds) and the soft matrix (Al).
To model the particles, icosahedral element type was chosen. This
element type offers a geometry that approximates the geometry of the
Nb2Al particulate well. In this situation, the effects of these hard par-
ticle compounds on microstructure of the production method are de-
termined to contribute to the mathematical model [11,29]. Geometry of
Nb2Al average particle was taken as 25 μm based on the measurements
described earlier.
A perfect spherical geometry is used for numerical modelling of
glass bubbles (GB). Fig. 7 shows that both a single and the random
H.M. Enginsoy et al.
Fig. 2. XRD diffraction of the basic reinforcement, Nb2Al intermetallics used in this work.
Fig. 3. Before (left column) and after milling (right column) of Nb2Al intermetallic powders.
Fig. 4. Nb-Al couple Binary phase diagram to show the situation of Nb2Al in-
termetallic compound.
distribution of the spheres in the RVE. The average diameter used for
the GB was 11 μm. This geometry which was formed after sintering and
thixoforming processes that difference in various chemical reactions
[18]. Thus, perfect spherical shape is used in sake of the simplicity for
400
Composites Part B 162 (2019) 397–410
the finite element modeling [34].
Fig. 8(a)–(d) show general presentation of 3D structural model.
Fig. 8(a) and (b) indicate the random distribution of the GB and Nb2Al
particulates in the RVE, respectively. Fig. 8(c) presents again the
transitional situation of GB and Nb2Al together, and also the final
composite (GB+Nb2Al in the aluminum matrix) is shown in Fig. 8(d).
Fig. 9 shows flow chart of the finite element algorithm for multi-
scale structural material modelling. Also, realistic modeling strategy of
a heterogeneous compound is shown with all details at the micro scale.
Representative Volume Element (RVE) is used for this reason in het-
erogeneous structure simulating [30–34].
To obtain the realistic heterogeneous microstructure modeling is
used Representative Volume Element (RVE) [23,35–37]. This technique
identified as a numerical model taken part the complex construction in
the composite microstructure. Complex geometric and boundary con-
ditions of reinforced particles are created. Then structural formation
equations and heterogeneous distributions are defined by RVE.
The volume fractions of Nb2Al and Glass Bubbles (GB) phases in the
RVE are given below by Eqs. (1) and (2), respectively
V0
v0 =
V (1)
V1
v1 = = 1 − Vo
V (2)
H.M. Enginsoy et al. Composites Part B 162 (2019) 397–410

Fig. 5. Differential thermal analysis of Glass Bubbles (GB) powders used to produce composites; and images of the material obtained by SEM.

Table 1 ts = (1 − D¯ ) t¯s, (4)

Properties of constituent materials [24–28].
tt = (1 − D¯ ) t¯t
Properties Symbol Unit AA7075 Nb2Al Glass Bubbles
δmf
Density ρ g/cm3 2.81 6.87 0.20 T dδ
Modulus of elasticity E GPa 71.7 188.7 – D¯ = ∫ GCeff− G0 ,
Shear modulus G GPa 26.9 72.3 –
0
δm (5)
Ratio of Poisson υ – 0.33 0.305 –
Ultimate tensile stress σus MPa 572 – – where, t̄n - t̄s - t̄t : maximum nominal traction parameters, D̄ : accumu-
Yield tensile stress σys MPa 503 – – lated in the interface damage, GC : fracture energy, G 0 : elastic energy,
Elongation A – 11% – – Teff : effective traction at damage initiation, δm0 -δmf initial thickness
Compressive Strength σs MPa – – 37.9 boundary conditions.
Thermal conductivity λ W/m.K 130 – 0.047
C3D4 (general linear element type) has been used as 3D solid ele-
ments for the microstructure. Mesh size was taken as 0.5 μm and total
where v0, v1, v are volumes for Nb2Al, Glass Bubbles (GB) and RVE, element numbers were at the level of 250,000.
respectively. The average stresses and strains that occur in the RVE
were modeled using Eq. (3) [38]. 3.1.2. Particle/matrix interface relations
Cohesive Zone Model (CZM) is used to determine a relation to de-
1 1
σ (r ) =
¯ V
∫ σ¯ (r ) dV ¯ε (r ) =
V
∫ ¯ε (r ) dV scribe the fracture at the interface between the reinforcement particles
V V (3) and the aluminum matrix. This relation is given by Eq. 6

In the simulations of the compression and three point bending tests, 1 f

Г= tδ
it was considered that the damage initiated in the microstructure at the 2 (6)
interface between the hard particulate and the matrix in the micro- where, t: cohesive interfacial strength, δ f :interfacial separation, Г :
structure then progressed towards the macro-level. Equations (4) and fracture energy.
(5) below describe this damage evolution. In these equations law of The stress-strain behavior of the microstructure resulting from sin-
exponential softening is used with damage evolution based on energy tering is given by Eq. (7) [39–41].
and stress components in the traction-separation relationships in Co-
∂
hesive Zone Model (CZM) [34]. εij = [Φ(d, D, T , σe, σm − σs )]
∂σij (7)
(1 − D¯ ) t¯n, t¯n ≥ 0,
tn = ⎧ where d : grain size d , D : relative density, T :sintering temperature, σe :
⎨ ¯
⎩ tn, if not ,
Von Mises effective stress, σm : mean stress, σs : sintering potential.

Fig. 6. 3D structural modelling: (a) Nb2Al, (b) random distributions in matrix phase.

401
H.M. Enginsoy et al.
Fig. 7. 3D structural modelling of glass bubbles and random distributions in matrix phase.
Fig. 8. 3D structural models for Glass Bubbles and Nb2Al particulates randomly distributed in the unit volume: (a) GB (5%), (b) Nb2Al (30%), (c) GB and Nb2Al
distribution together, (d) Final composite model structure.
In Eq. (7) σs is the sintering potential function given by Eq. (8).
∂F
σs ≡ = σs (γs, γgb, D , d )
∂Vpore
where F : total free energy of the solid, Vpore : total volume of the pores,
γs, γgb : free surface energy and grain boundary, d : grain size d , D : re-
lative density.
The stress-strain behavior of the microstructure resulting from
thixoforming is given in Eq. (9).
σ = e (a − bT ) (ε + ε0)n (ε˙ + ε˙ 0)m (1 − βfL )
where a, b, n, m , β : parameters for constitutive equation of material
under the Thixoforming conditions.. fL : Liquid fraction of semi-solid
phase.
The parameters in Eq. (9) used in this study were based on 6061
aluminum parameters, updated for AA7075 using some mathematical
iterations and convergence techniques [38,42–46].
Composites Part B 162 (2019) 397–410
3.2. Modeling of macro-mechanical structure and testing conditions
At this stage of the study, the micromechanical models developed
(8) for thixoforming and sintering were used to generate the macro level
samples for bending and compression tests. The model shown in Fig. 10
describes the relationship with RVE in micro modeling and bending and
compression samples.
Compression sample was modeled as a cylinder with 30 mm in
height and 20 mm in diameter. The sample was compressed at a rate of
1 mm/min. The bottom surface of the sample was completely (ALLDOF)
(9) fixed.
The bending specimen was 35 mm long, 3 mm deep and 13 mm
wide. The span used in the three point bending test was 25 mm. The
load was applied by a 13 mm long cylinder with 2.5 mm diameter. The
load was applied at a rate of 1 mm/min. The two supports were also
modelled as 13 mm long cylinders with 2.5 mm diameter. The supports
were taken as completely fixed. The mesh element type was taken as
402
H.M. Enginsoy et al. Composites Part B 162 (2019) 397–410

Fig. 9. Flow algorithm for modeling of multiscale composite material.

Fig. 10. Macro/microstructure relations of metal matrix composites under test conditions; a) three point bending test and b) compression test.

403
H.M. Enginsoy et al. Composites Part B 162 (2019) 397–410

Fig. 11. Microstructure and interface analyses of the specimens produced by thixoforming of composites with 30, 40, and 60 wt% of Nb2Al intermetallic re-
inforcements.

R3D4 (four node-3D bilinear discrete rigid quadrilateral) elements in
both tests for mechanical loading and support fixtures [34,47].
4. Result and discussion
4.1. Microstructure and operational parameters in thixoforming
Before the thixoforming process, thixoforming temperature at which
significant liquid formation is achieved in the composite should be
determined. In this study, thixoforming was successfully carried out
both at 625 °C and 630 °C. No significant difference was detected in the
structure of the composites produced at these two temperatures. The
retention time at the thixoforming temperature can clearly provide the
thermodynamic equilibrium condition in the material and the required
liquid fraction in the semi-solid. In addition, the structure of the
spheroidization has been realized. Thixoforming pressure also influ-
ences the microstructure. Since semi-solid metal exhibits thixotropic
flow behavior, low pressure is essential in the thixoforming process.
Furthermore, the amount of pressure required in the thixoforming
process to push Nb2Al intermetallic particles through the aluminum
chip layers must be higher due to the oxide layers present at the surface
of the aluminum chips. By increasing thixoforming generation pressure,
degradation of the oxide layers is facilitated. This then allows the chips
to be decomposed. Thus, a better reinforcing dispersion is obtained
[51].
Fig. 11 shows microstructure and the interface between the Nb2Al
particles with matrix for the reinforcement ratios of 30, 40, 60 wt%. At
the first stage, quasi eutectic similar structures are observed. Relation of

404
H.M. Enginsoy et al. Composites Part B 162 (2019) 397–410

Fig. 12. Detail of the interface structure in the composite with 60% of Nb2Al particles.

Fig. 13. Special regions taken from different combinations to verify the interfacial matrix/intermetallic reaction phases via vibrational chemical bonds under the
influence of mutual thermal diffusion.

Nb2Al intermetallic particles with matrix and diffusion mechanism
mixed with the formation of quasi eutectic structure shows mainly a
diffusional chemical bonding reaction that occurred by means the
thermo-chemical vibrations. This evolution can be observed more easily
in Fig. 12 at the higher magnification of interface.
Relation of Nb2Al intermetallic particles with matrix can be ex-
plained more clearly with diffusion mechanism. By using “EDS”
analyses, all the details of this diffusion mechanism are presented in
Fig. 13 for the different percentages of Nb2Al intermetallics. First of all,
thixoforming temperature (Ts = 620–625 °C) can result in regularly the
correct bonding at the interface of matrix/intermetallic reinforcements.
Due to heat treatment that occurs during thixoforming, the interface
can be implemented very suitable cohesion.
During this operation, very stable vibrational chemical bonds can be

405
H.M. Enginsoy et al.
Fig. 14. Comparison of the evolution of the stress strain curves in three points bending tests for samples manufactured by sintering (a) and thixoforming (b).
Fig. 15. Stress distributions resulting from three point bending test reinforcement/matrix interfaces.
formed between the intermetallic particles (heavy atoms: e.g. Nb and or
Nb2Al) and the matrix (light atoms: Al). For this reason, Nb2Al particle
reinforcements show quasi homogeneous interface. It means that under
the effect of mutual thermal diffusion, it can ensure easily vibrational
chemical bonds. Due to the interface matrix/intermetallic reaction
phases, it can result from a stable interface [5,48].
4.2. Mechanical properties and failure analysis
As for mechanical behavior of the specimens obtained by thix-
oforming and sintering processes, one may compare the bending test
results of the sintered and thixoformed specimens as presented in
Fig. 14. It is evident that the bending response of the sintered specimens
when compared to the bending response of the specimens manu-
factured by thixoforming is different. Fig. 14 compares the evolution of
the stress strain curves in three points bending tests for samples man-
ufactured by sintering and thixoforming. A comprehensive study was
presented here by comparing of the experimental and FEM results that
they are very conformable. As can be seen well from these figures,
sintered specimens behaved in a very brittle manner as and the max-
imum strain before final failure was about 0.6%; evolution of the stress
strain curves are mainly in staircase identified by decohesion at the
406
Composites Part B 162 (2019) 397–410
interface. Fracture along the interface began at the early stages of the
test for these specimens indicating that cohesion of the reinforcement
particles with the matrix is very weak. Specimens manufactured by
thixoforming behaved in a more ductile manner and the maximum
strain reached about 10% before final failure. The effect of Nb2Al in-
termetallic reinforcements on the response of the specimens can be
observed for both methods of manufacturing; as the Nb2Al content in-
creases, the specimens become more brittle. However, the quality of the
specimens obtained by thixoforming is always better than the speci-
mens obtained with sintering.
To support these results, more detailed information is presented
from FEM results in Fig. 15. Here, stress distribution at the interface,
intermetallic compounds/matrix depending on the distance was cal-
culated in case of three point bending test. Evolution of the stress at
interface was indicated for both of the two processes; sintering and
thixoforming. In Fig. 14, both of these curves justified the experimental
and FEM results given. Fig. 15 shows the effect of sintering and thix-
oforming processes on the stress distributions between the Al matrix
and Nb2Al particles in the internal structure of the Nb2Al-30 sample
with three point bending test (at the end of the test and sample pro-
duced by thixoforming). In the graph in Fig. 15, the sample produced by
thixoforming has been shown to have higher stress values than the
H.M. Enginsoy et al.
Fig. 16. Comparison of the three points bending test results for thixoformed composites at different deformation levels.
sample produced by sintering at the matrix-particle interface. There are
two important reasons for this situation. First reason; since the sintered
samples have less ductile structure, they can carry stress to a certain
level. Since three point bending test does not carry high stresses in the
sample, damage is started. After the formation of the damage, the
sample did not carry high stress.
Therefore, less stress distribution has occurred in sintered samples.
Second reason; samples produced by thixoforming have a ductile
structure and can carry higher stresses. As the sample can carry more
stresses in the three point bending test, the damage began later.
Therefore, a higher stress distribution has occurred in the samples
produced by thixoforming.
Much more detail about stress distributions and deformation be-
havior of the composites are presented in Fig. 16 in case of three point
bending tests. In this figure, entire results were given by FEM for the
three different compositions depending on the percentage of Nb2Al
intermetallics. Each composite was classified at the three deformation
stages that are variable from 1 up to 3%.
As can be observed from these pictures, Nb2Al intermetallic com-
pound has a significant effect on the damage behaviour of the compo-
sites in case of three points bending test. Ductility decreases in the
composites containing high percentage of the Nb2Al intermetallic
compounds. It means that stress distribution is not homogeneous and is
concentrated in a very narrow area. Finally, the specimens become
inflexible even more and more rigid in case of higher amount of Nb2Al
intermetallics so fracture happened as brittle manner.
Other interesting results of thixoformed specimens were obtained
when the glass bubbles were added in the structure (Fig. 17). Specimens
without glass bubbles and with 5 vol% glass bubbles were tested in
compression and the results are presented in Fig. 17, where results for
each Nb2Al content (30, 40, 50 and 60 wt %) is given separately. It
seems that glass bubbles improve ductility for all cases except for the
composites containing the highest Nb2Al intermetallics.
It can also be observed in Figs. 14 and 17 that the numerical si-
mulations performed with the method explained in detail in the former
section third can predict the stress-strain response of the compression
and bending samples exceptionally well and FEM created in this work
407
Composites Part B 162 (2019) 397–410
helps to explain and interpret the damage mechanism combined with
the microstructure and relationship between intermetallic reinforce-
ments and matrix mainly at interface due to chemical diffusion bonding
with thermal treatment mechanism. This is the originality of this pre-
sent work carried out in this work.
In case of the fracture surfaces of the aluminum matrix composites
reinforced with Nb2Al intermetallic particles obtained from three point-
bending tests are evaluated and presented in Fig. 18. All of the fracture
surface-damages obtained by SEM are quasi similar for the four com-
posites considered in this study. In this figure, high magnification
fracture surfaces are shown at the right column. It can be observed that
fracture of hard particulates embedded in the soft matrix is the source
for damage initiation. Brittle fracture is mainly observed at the inter-
face with Nb2Al intermetallics. Any interfacial debonding is found at
the fracture surfaces, which indicates that the composites do not con-
tain voids or other defects. However, particle fracture seems to be the
main internal damage mechanism, especially at the higher content of
Nb2Al intermetallics. In Fig. 18 the effect of these reinforcements on the
more brittle response of the composite is noticeable. But the resistance
to fracture of the Nb2Al intermetallics can be optimized at the medium
level of the reinforcement such as 30 wt%. The results given in this
work are not definitive but they are indicative. More experimental
analyses are needed for much more reliable results.
For sake of simplicity, another evaluation of the thixoformed spe-
cimens can be made by studying fracture toughness values of these
composites reinforced with Nb2Al particles [3,5,7,14,15]. For this
reason, fracture toughness values of these composites were examined
by Vickers indentation on the transverse sections of the polished me-
tallographic specimens. The measurements were taken with indentation
loads of 500g on the four composites with 30, 40 and 60 wt % Nb2Al.
The following equation was used for each level of these composites in
order to give a general idea on the fracture toughness values:
KIC = 0:0095(Hv*P/4l)1/2 (10)
where Hv is the Vickers hardness value and l is the length of the crack at
the end of the Vickers diamond and P is the applied load on the spe-
cimen. The fracture toughness value for transverse sections could be
H.M. Enginsoy et al. Composites Part B 162 (2019) 397–410

Fig. 17. Comparison of the effect of glass bubbles on the compression behavior of different compositions obtained by thixoforming; experimental and FEM results are
compatible.

variable from 3.15 to 3.60 MPa m1/2 depending on the percentage of
Nb2Al intermetallic particles; In general fracture toughness of the
composites with the medium percentage of the intermetallic particles
(around the 30–40% of Nb2Al) was higher. This evaluation can give
only an indicative idea about the fracture toughness of these composites
but it is useful to see the level of the toughness values in practical point
of view to find practical solutions in case of industrial applications.
5. Conclusions
A new design of Al-Nb2Al composites was developed via associated
procedure of powder metallurgy and thixoforming. AA7075 aluminum
matrix composites were used from recycled chips and reinforced with
Nb2Al at 30 to 60 wt% intermetallic particles. Mechanical properties of
these new types of composites were evaluated. Based on experimental
results, an original FEM modelling has been developed all the details
were given in section 3.
First of all, the properties measured are directly a function of to the
thermal stability of the composites during materials processing (pro-
cessing and subsequent thermal treatments of sintering and thix-
oforming). The better ductile behaviors among the intermetallic re-
inforced composites were found for the 30–40 wt% of Nb2Al with 5%
vol. Glass Bubbles (GB). Samples with this content, because they are
more ductile, can carry higher stress amounts in compression tests
(under 10% strain). In any case, these intermetallic particles are the
most thermally stable. Glass bubbles (5 vol % in the matrix) in the
structure increased ductility. In the samples with 60 wt% Nb2Al and 5%
vol, it was determined that the addition of Glass Bubbles did not con-
tribute to the increase in ductility. In addition, all these cases were
compared both experimentally and numerically.
No interfacial debonding is found at the fracture surfaces; it means
that the composites do not contain defects. However, fracture of the
hard particulate embedded in the soft matrix was observed as the main
reason for internal damage initiation in the composite. It means that
particle fracture is seen as the main internal damage mechanism,
especially at the higher level of Nb2Al intermetallics, Brittle fracture is
mainly observed at the interface with Nb2Al intermetallics. Therefore,
ultimate fracture is after produced through crack propagation by way of
the soft matrix between the clusters. Concisely, it is proposed that
macroscopic fracture is started in the Nb2Al intermetallics particle
clusters that are present in these composites. The matrix inside of the
clusters is exposed to high levels of triaxial stress because of elastic
mismatch of the constituent properties and the restrictions applied on
the matrix by the surrounding particles [15]. More uniform distribution
of Nb2Al particles should result in improved fracture strength. All of the
experimental and FEM results and all of the damage analyses have
shown excellent compatibility thanks to new modelling carried out in
this work. Basically, this type of work is new and its originality is based
on the subroutine “VUHARD” developed to be used with Abaqus in
order to analyze the effect of thixoforming and sintering on the micro
and macrostructure of the manufactured materials.
Interfacial cohesion at the matrix/reinforcement interface is

408
H.M. Enginsoy et al. Composites Part B 162 (2019) 397–410

Fig. 18. Fracture surfaces of aluminium matrix composites reinforced with Nb2Al intermetallic particles (without glass bubbles) obtained from 3P - bending tests
(high magnification pictures are shown on the right column) and EDS.

409
H.M. Enginsoy et al.
substantially influenced by blending and mixture - milling time, com-
pacting pressure and most remarkably sintering temperature. Basically,
thixoforming temperature (Ts = 620–625 °C) can result in regularly the
correct bonding at the interface of matrix/intermetallic reinforcements.
Very suitable cohesion at the interface can just be performed by thix-
oforming processing. Sintering processing for these composites resulted
in relatively lower mechanical properties when compared with the
thixoforming processing [5].
As for the microstructure, very stable vibrational chemical bonds
can be formed between the intermetallic particles (heavy atoms: e.g. Nb
and or Nb2Al) and the matrix (light atoms: Al). Nb2Al particle re-
inforcements show quasi homogeneous interface. It means that under
the effect of mutual thermal diffusion, it can ensure easily vibrational
chemical bonds. Due to the interface matrix/intermetallic reaction
phases, it can result from a stable interface. At least, a suitable cohesion
at the interface can just be carried out at high thixoforming
(∼620–630 °C) and sintering temperatures (∼640–680 °C) [5].
Acknowledgements
The authors acknowledge the financial support provided by
CNPq–CAPES/-SP-BRAZIL in the frame of common project carried out
by Supmeca-Paris, UNICAMP-Campinas/SP-Brazil and Michigan Tech-
USA.
References
[1] Bobrová E, Besterci M. Intermetallic alloys based on Ni-Al produced by powder
metallurgy. Powder Metall Prog 2004;4(1):57–68.
[2] Kim JK, Chung D-S. Fabrication of metal/intermetallic compound laminate com-
posites by thin foil hot press process. In: Ahn BT, Jeon H, Hur BY, Kim K, Park JW,
editors. Advances in nanomaterials and processing, Pts 1 and 22007. p. 1099-1102.
[3] Kurşun A, Bayraktar E, Robert MH. Low cost manufacturing of aluminium-alumina
composites. Adv Mater Process Technol 2016:1–14.
[4] Lloyd DJ. Particle reinforced aluminum and magnesium matrix composites. Int
Mater Rev 1994;39(1):1–23.
[5] Bayraktar E, Robert M-H, Miskioglu I. Design of Al-Nb2Al composites through
powder metallurgy. In: Ralph C, Silberstein M, Thakre RP, Singh R, editors.
Mechanics of composite and multi-functional materials, volume 7: proceedings of
the 2015 annual conference on experimental and applied mechanics. Cham:
Springer International Publishing; 2016. p. 131–9.
[6] Chung D-S, Enoki M, Kishi T. Microstructural analysis and mechanical properties of
in situ Nb/Nb-aluminide layered materials. Sci Technol Adv Mater
2002;3(2):129–35.
[7] Niihara K, Morena R, Hasselman DPH. Evaluation of KIC of brittle solids by the
indentation method with low crack-to-indent ratios. J Mater Sci Lett
1982;1(1):13–6.
[8] Anton DL, Shah DM, Liu CT. High temperature ordered intermetallic alloys III.
Materials research society symposium proceedings. Pittsburgh, PA, USA: Materials
Research Society. p. 361.
[9] McGarry TD, Pindera M-J, Wawner FE. Evaluation of reaction barrier compensating
coatings on SCS-6 fibers in Ti-24Al-11Nb(at%) composites. Compos Eng
1995;5(7):951–74.
[10] Triveño Rios C, Ferrandini P, Caram R. Fracture toughness of the eutectic alloy
Al3Nb-Nb2Al. Mater Lett 2003;57(24–25):3949–53.
[11] Peng LM. Synthesis and mechanical properties of niobium aluminide-based com-
posites. Mater Sci Eng, A 2008;480(1–2):232–6.
[12] Rios CT, Ferrandini PL, Milenkovic S, Caram R. Growth and microstructure evo-
lution of the Nb2Al–Al3Nb eutectic in situ composite. Mater Char
2005;54(3):187–93.
[13] Ghosh G, Olson GB. Integrated design of Nb-based superalloys: Ab initio calcula-
tions, computational thermodynamics and kinetics, and experimental results. Acta
Mater 2007;55(10):3281–303.
[14] Niihara K. A fracture mechanics analysis of indentation-induced Palmqvist crack in
ceramics. J Mater Sci Lett 1983;2(5):221–3.
[15] Lloyd DJ. Aspects of fracture in particulate reinforced metal matrix composites.
Acta Metall Mater 1991;39(1):59–71.
[16] Rios CT, Milenkovic S, Ferrandini PL, Caram R. Directional solidification, micro-
structure and properties of the – eutectic. J Cryst Growth 2005;275(1–2):e153–8.
[17] Rios CT, Contieri RJ, Souza SA, Cremasco A, Hayama AOF, Caram R. Fracture
toughness of a directionally solidified Al–Nb–Ni ternary eutectic. Mater Des
2012;33:563–8.
[18] Kurşun A, Bayraktar E, Robert M-H, Miskioglu I. Design of Al-Nb2Al composites
through combined method of powder metallurgy and thixoforming. International
annual conference on advanced materials and processing technologies. Carlos III
University, Leganes, Madrid, Spain2015. p. 1-9.
[19] Su Y, Ouyang Q, Zhang W, Li Z, Guo Q, Fan G, et al. Composite structure modeling
and mechanical behavior of particle reinforced metal matrix composites. Mater Sci
Eng, A 2014;597:359–69.
410
Composites Part B 162 (2019) 397–410
[20] Yuan Z, Li F, Xue F, He M, Hussain MZ. Analysis of the stress states and interface
damage in a particle reinforced composite based on a micromodel using cohesive
elements. Mater Sci Eng, A 2014;589:288–302.
[21] Meng Q, Wang Z. Prediction of interfacial strength and failure mechanisms in
particle-reinforced metal-matrix composites based on a micromechanical model.
Eng Fract Mech 2015;142:170–83.
[22] García IG, Mantič V, Graciani E. A model for the prediction of debond onset in
spherical-particle-reinforced composites under tension. Application of a coupled
stress and energy criterion. Compos Sci Technol 2015;106:60–7.
[23] Xu Q, Qu S. Irreversible deformation of metal matrix composites: a study via the
mechanism-based cohesive zone model. Mech Mater 2015;89:72–84.
[24] Neuberger M, Grigsby DL, Veazie WH. Niobium alloys and compounds. Springer
Science+Business Media,LLC; 1972.
[25] Rohatgi A, Harach DJ, Vecchio KS, Harvey KP. Resistance-curve and fracture be-
havior of Ti–Al3Ti metallic–intermetallic laminate (MIL) composites. Acta Mater
2003;51(10):2933–57.
[26] Jenab A, Karimi Taheri A. Experimental investigation of the hot deformation be-
havior of AA7075: development and comparison of flow localization parameter and
dynamic material model processing maps. Int J Mech Sci 2014;78:97–105.
[27] Rotella G, Dillon OW, Umbrello D, Settineri L, Jawahir IS. Finite element modeling
of microstructural changes in turning of AA7075-T651 Alloy. J Manuf Process
2013;15(1):87–95.
[28] Canakci A, Varol T. Microstructure and properties of AA7075/Al–SiC composites
fabricated using powder metallurgy and hot pressing. Powder Technol
2014;268:72–9.
[29] Rock C, Okazaki K. Detailed phase analysis of a 77 at.%Nb-Al system prepared by
low-energy ball milling. Nanostruct Mater 1995;5(6):643–56.
[30] Sun CT, Vaidya RS. Prediction of composite properties from a representative vo-
lume element. Compos Sci Technol 1996(56):171–9.
[31] Kanit T, Forest S, Galliet I, Mounoury V, Jeulin D. Determination of the size of the
representative volume element for random composites: statistical and numerical
approach. Int J Solid Struct 2003;40(13–14):3647–79.
[32] Węglewski W, Basista M, Manescu A, Chmielewski M, Pietrzak K, Schubert T. Effect
of grain size on thermal residual stresses and damage in sintered chromium–alu-
mina composites: measurement and modeling. Compos B Eng 2014;67:119–24.
[33] Madke RR, Chakraborty S, Chowdhury R. Multiscale approach for the nonlinear
behavior of cementitious composite. Comput Mater Sci 2014;93:29–35.
[34] Kurşun A, Bayraktar E, Enginsoy HM. Experimental and numerical study of alumina
reinforced aluminum matrix composites: processing, microstructural aspects and
properties. Compos B Eng 2016;90:302–14.
[35] Breslin MC, Ringnalda J, Xu L, Fuller M. Processing, microstructure, and properties
of co-continuous Al-Al2O3 composites. Mater Sci Eng 1995;195:113–9.
[36] Zebarjad SM, Sajjadi SA. Microstructure evaluation of Al–Al2O3 composite pro-
duced by mechanical alloying method. Mater Des 2006;27(8):684–8.
[37] Zebarjad SM, Sajjadi SA. Dependency of physical and mechanical properties of
mechanical alloyed Al–Al2O3 composite on milling time. Mater Des
2007;28(7):2113–20.
[38] Favier V, Bigot R, Cézard P. A physical and micromechanical model for semi-solid
behaviour. Thixoforming: Wiley-VCH Verlag GmbH & Co. KGaA; 2009. p. 221–38.
[39] Niu W, Pan J. Computer modelling of sintering: theory and examples. In: Fang ZZ,
editor. Sintering of advanced materials. Woodhead Publishing; 2010. p. 86–109.
[40] Castro R, Kv Benthem. Sintering mechanisms of convention nanodensification and
field assisted processes. In: Castro R, Kv Benthem, editors. Sintering mechanisms of
convention nanodensification and field assisted processes. Springer-Verlag Berlin
Heidelberg; 2013. p. 100–2.
[41] Li W, Porter MM, Olevsky EA, German RM, McKittrick J. Sintering of bi-porous
titanium dioxide scaffolds: experimentation, modeling and simulation. Mater Sci
Eng, A 2015;636:148–56.
[42] Koeune R, Ponthot JP. An improved constitutive model for the numerical simula-
tion of semi-solid thixoforming. J Comput Appl Math 2010;234(7):2287–96.
[43] Koeune R, Ponthot JP. A one phase thermomechanical model for the numerical
simulation of semi-solid material behavior. Application to thixoforming. Int J Plast
2014;58:120–53.
[44] Papadimitriou I, Utton C, Tsakiropoulos P. Ab initio investigation of the Nb–Al
system. Comput Mater Sci 2015;107:116–21.
[45] Wang J, Phillion AB, Lu G. Development of a visco-plastic constitutive modeling for
thixoforming of AA6061 in semi-solid state. J Alloy Comp 2014;609:290–5.
[46] Bolouri A, Shahmiri M, Kang CG. Study on the effects of the compression ratio and
mushy zone heating on the thixotropic microstructure of AA 7075 aluminum alloy
via SIMA process. J Alloy Comp 2011;509(2):402–8.
[47] Kurşun A, Şenel M, Enginsoy Halil M. Experimental and numerical analysis of low
velocity impact on a preloaded composite plate. Adv Eng Software 2015;90:41–52.
[48] Ferreira LFP, Bayraktar E, Robert MH, Miskioglu I. Particles reinforced scrap alu-
minum based composites by combined processing sintering + thixoforging. In:
Ralph W, Singh R, Tandon G, Thakre P, Zavattieri P, Zhu Y, editors. Mechanics of
composite and multi-functional materials, volume 7: conference proceedings of the
society for experimental mechanics series. Cham: Springer International Publishing;
2017. p. 145–52.
[49] Allouard M, Bienvenu Y, Nazé L, Brancho-Troconis CB. Development of oxidation
resistant high temperature NbTiAl alloys and intermetallics. J Phys IV
1993;03:419–28.
[50] Ferreira LFP, Bayraktar E, Miskioglu I, Robert MH. New magnetic aluminum matrix
composites (Al-Zn-Si) reinforced with nano magnetic Fe3O4 for aeronautical ap-
plications. Adv Mater Process Technol 2018;4(3):358–69.
[51] Ferreira LFP, Robert MH, Bayraktar E. Effect of operational parameters in the semi-
solid processing of Al/SiC composites from machining chips. ECCM16 - 16th
European conference on composite materials, seville, Spain. 22-26 June 2014.
p. 1–8.