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ORIGINAL CONTRIBUTION
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Casting is one of the economical processes among many and maintain the thermal stability, but reduces the ductility
affordable procedures to transform raw material into useful because of the establishment of many complex intermetallic
components, and defect-free casting is being challenge in compound phases of Al2Ni and Al3Ni2 [22].
foundry metals. Method of fabrication of AMMCs plays a Ferroniobium (FeNb) is a microalloying element predom-
vital role for enhancement of strength and reduction in cost. inantly used in high-strength low alloy (HSLA) steels. It is
There were lots of practices industrialized for the fabrication an iron-niobium alloy consisting of 60–70% of niobium con-
of AMMCs, and there were stir casting, squeeze casting, ultra- tent, and the rest of the elements is iron and other impurities.
sonic-assisted casting, hot pressing, high-pressure die casting When it adds to HSLA steels, it results the strength enhance-
(HPDC), selective laser melting (SLM), spark plasma sintering ment and weldability and refines the as-cast austenite struc-
(SPS) and powder metallurgy (PM) [10]. Among these, stir ture. The commercial grade ferroniobium (FeNb) is 1370 °C,
casting (liquid state) processing is one of the easy and most which is much greater than the fabrication temperature of
economical methods due to simplicity, flexibility, scalability, 750 °C. Hence, when it is added to the molten metal, it dis-
easily adoption and productivity [11, 12]. solves rather than melting taking place. As a result, it forms
Defect-free casting plays an important role in production of the Fe2Nb heterogeneous phase in matrix alloy [23]. The
industrial components. Insufficient fluidity can lead to various wide applications of the FeNb reinforcements into alloys are
casting defects. For instance, when the molten metal does not automobiles, gas pipelines, tool steels, ship hulls, train tracks
flow freely, it can cause misruns, cold shuts or insufficiently and several high-temperature systems [24].
filled areas, resulting in incomplete or flawed castings [13, 14]. The current study aims to systematically compare
Proper fluidity helps minimize such defects and ensures the microstructures and mechanical properties of as-cast
soundness and integrity of the final cast component. Fluidity Al5Cu2Ni/xFeNb composites (x = 1, 3, 5 wt% of FeNb)
plays a crucial role in casting processes, particularly in metal fabricated by electromagnetic stir casting method via sand
casting. It refers to the ability of molten metal to flow and fill mold and metal mold system. An attempt has been made to
the mold cavity completely before solidification occurs [15]. study the metallography and fractography of the composites
The fluidity of the molten metal is influenced by several fac- to know the structural changes resulting in the enhancement
tors, including its elemental composition, pouring temperature of mechanical properties with an increasing wt% of FeNb as
and the design of the mold [16, 17]. a reinforcement element. As of now, no research has been
Sand and metal molds have been widely used for the fab- carried out FeNb as a particulate reinforcement element into
rication of metals in the casting process. They have superior Al-Cu-based metal matrix composites.
heat dissipation ability. The most common casting compo-
nents are Aluminum and its alloys for aircraft and automotive
applications. Sand casting method is one of the expendable Experimental Methodology
mold methods, and it was found to be the most widely used
casting method because of its economic characteristics. It is The details of materials and their selections, the process-
being used to produce approximately 70% of all metal cast. ing method to fabricate the Al5Cu2Ni/xFeNb composites
The metal mold casting method has been predominantly used and the method of testing as per the ASTM standard are
to manufacture a large variety of components with low surface discussed in this section. However, the characterization of
roughness and high dimensional accuracy and consists of the metallography and enhancement of physical and mechanical
ability to rapidly solidify cast alloys and thus, refine dendrite properties will be discussed in the following sections.
structure [18, 19].
Al–Cu alloys (2xxx series) consist of a lightweight to Selection of the Material
high-strength ratio, appreciable mechanical properties and
are eco-friendly in machining. It has applications in struc- The commercial base alloy which is used for this investiga-
tural, aerospace, marine and automotive industries due to its tion is Al-5Cu, the elemental composition of the base alloy
combination of high-specific strength, specific modulus and (A206) chosen for the present study as depicted in Table 1.
reasonable ductility [20, 21]. Nickel (Ni) up to 2 wt% addition For fabrication of defined Al–Cu-based composites,
into Al–Cu alloy could refine the microstructure, enhance the Aluminum (Al), Copper (Cu) and Nickel (Ni) are taken as
mechanical properties, resist the hot tearing of Al–Cu alloys an ingot form with a purity of 99.97% and Ferroniobium
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J. Inst. Eng. India Ser. D
(FeNb) is considered as particulate reinforcement with a size characterization. The detailed fabrication procedure and speci-
of 60 mesh [24]. The composites for this study are fabri- fications of the composite material along with reinforcement
cated with different weigh fractions of ferroniobium (FeNb) particulate discussed elsewhere [24].
powder reinforced into Al5Cu2Ni matrix alloy, as shown in
Table 2. The step-by-step procedure of the current investiga- Microstructures
tion is illustrated in the following line chart as demonstrated
in Fig. 1. The specimens were sectioned into 10 × 5 × 10 mm3 from the
fabricated composites. It was polished with emery sheets from
Fabrication Procedure 220 grit size to 2000 grit size for getting a fine surface. Then,
after being polished with velvet cloth with 3 microns diamond
For the fabrication of Al5Cu2Ni/xFeNb composites with par- past to obtain a mirror surface, [25] it was etched with Keller’s
ticulate reinforcement of ferroniobium (FeNb), an electromag- reagent, which has been broadly using an etchant for Al-based
netic stir casting method has been adapted. A 99.97% pure composites [24]. Therefore, the metallography was captured
aluminum ingot was melted at 750 °C, along with the addition and examined by OM and SEM with EDS. The line-intercept
of 5% copper (Cu) and 2% nickel (Ni). However, to increase method has been adapted for measuring the grain size of the
the wettability of the matrix alloy, magnesium with 0.1 weight composites as per ASTM E112-10 standard [5].
percent was added to the melt [5]. The molten metal’s impu-
rity gases were released using the hexachloroethane degassing Density and Porosity Measurement
tablets [20]. Therefore, molten metal was brought to a semi-
solid state at a temperature of 650 °C; then, pre-heated FeNb The rule of mixture (ROM) and the water displacement tech-
reinforcement particulates were incorporated into the semi- nique (the Archimedes principle) can be used to compute the
solid liquid. Subsequently, Electromagnetic stirring (EMS) theoretical density (DTH) and experimental density (DEX) of
was applied to stir the molten metal with a stirring speed of the composites [5]. The governing Eq. 1 and 2 can be used to
500 revolutions per minute, as shown in Fig. 2 [24]. A K-Type calculate:
thermocouple with an accuracy of ± 5 °C has been used to
1
measure the temperature of molten metal as shown in Fig. 2a. DTH = wf1 wf2 wf3 wf4 (1)
The furnace temperature was raised to 750 °C. Subsequently, d1
+ d2
+ d3
+ d4
the molten metal was allowed to sand mold and metal mold
and kept some time to get solidify. However, the gating system According to Eq. 1, where wf1, wf2, wf3 and wf4 are the
was machined, and final composites were taken for further weight fractions (wt%) of Aluminum (Al), Copper (Cu),
Nickel (Ni) and Ferroniobium (FeNb), respectively, as shown
in Table 2, and d1, d2, d3 and d4 are the relative densities
Table 2 Experimental design (Table 3).
Material Wt%
for the fabrication of Al-based of
composites
M
FeNb DEX. = (2)
V
Al5Cu2Ni/1FeNb 1
According to Eq. 2, a high-precision electronic weighing
Al5Cu2Ni/3FeNb 3
balance with a 0.1 mg accuracy was used to measure the
Al5Cu2Ni/5FeNb 5 test specimen’s weight. In order to determine the density,
Fig. 1 Line chart represents the step-by-step procedure of the current study
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Fig. 2 Schematic of EMS casting set-up: a K-type thermocouple; b Electrical furnace; c EMS mechanism; d Metal mold with AMMC; e CO2
sand mold, f Fabricated AMMC
Table 3 Obtained results Description Material Ultimate tensile Microhardness (Hv) Grain size
from Mechanical testing and strength (MPa) (µm)
Grain size measurement with
percentage of error deviation Sand mold system Al5Cu2Ni/1FeNb 95.29 ± 5 62.00 ± 3 66 ± 3
Al5Cu2Ni/3FeNb 123.35 ± 3 67.13 ± 2 51 ± 3.5
Al5Cu2Ni/5FeNb 134.85 ± 5 72.83 ± 4 47 ± 4
Metal mold system Al5Cu2Ni/1FeNb 184.85 ± 5 130.28 ± 4 59 ± 2
Al5Cu2Ni/3FeNb 192.70 ± 6 132.26 ± 6 46 ± 2.5
Al5Cu2Ni/5FeNb 206.81 ± 8 150.52 ± 8 44 ± 3
the specimen’s mass (M) was divided by the volume (V) of pyramid shape and dwelling time of 15 s. An average of five
water displaced. indentations was taken for study. The tensile specimens were
In accordance with Eq. 3, the porosity of composites machined with EDM according to the standard of ASTM E8,
could be determined by differentiating the theoretical density as shown in Fig. 2 [26]. However, the tensile test was per-
(DTH) from the experimental density (DEX) and dividing it formed on a digitally controlled hydraulic 100 KN dynamic
with the theoretical density (DTH) and comparing the results: testing machine with a crosshead speed of 0.5 mm/min with
an aligned gauge length of 25 mm linear and bi-axial exten-
DTH − DEX
Porosity = × 100% (3) someter [25]. Therefore, three specimens were tested, and an
DTH average of three values was considered for the study (Fig. 3).
Mechanical Properties
Results and Discussion
The fabricated composites were sectioned into 10 × 5 × 10
mm3 and prepared as per the specification of a test proce- Fabrication of Al5Cu2Ni/xFeNb composites (x = 1, 3, 5 wt%
dure for measuring the Vickers microhardness as per the of FeNb) was done successfully via a two-step electromag-
ASTM E 384–17 standard test procedure [24]. A test load netic stir casting method by a sand mold and metal mold
of 100 g was applied with an indenter of 136° diamond system. From the obtained results, the characterization of
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metallography, density, porosity and mechanical properties It seems that the grain size of the composites gradually
has been discussed in the following sections. decreased with increasing wt% of FeNb in both the cases,
as shown in Fig. 5.
Microstructures Characterization From Fig. 6, SEM with EDS graphs reveals that the pri-
mary α-Al dendritic structure with Cu-eutectic regions are
The improvement of mechanical properties of Al-Cu cast different for sand and metal mold cast samples because of
alloys depends not only on chemical composition but, more the difference in the rate of solidification [8]. Since metal
important on microstructural features such as the morphol- mold, as-cast composites presented a higher amount of solid
ogy of α-Al primary dendrites and intermetallic particles, solubility of Cu and Ni than that of sand mold as-cast com-
which are act as grain refining sites in the microstructure posites. Hence, finer and higher amounts of intermetallic can
[31]. The optical micrographs of the composites fabri- be expected to precipitate in metal mold as-cast samples. It
cated by both sand and metal molds are shown in Fig. 4. was observed that from Fig. 6c, the intermetallic compound
The microstructures consist of primary α-Al dendrites sur- phases of A l2Cu, Al3Ni2 and the heterogeneous phase of
rounded by the eutectic Cu and the different intermetallic Fe2Nb. In the EDS graphs of the composites, Fe and Nb
phases of A l2Cu as an irregular phase along with A l3Ni2 peaks were noted, which evident the presence of FeNb par-
and Fe2Nb phases; these phases might be acting as a nucle- ticles in the composites.
ation site [27]. The formation of microstructures depends
upon the rate of cooling as well as the process of filling and Characterization of Physical Properties
solidification time [28]. From Fig. 4a and d, it was observed
that a coarser microstructure is formed in cast specimens Figure 7 shows that there is not much variation between
which are made by the sand-casting process due to longer theoretical density and experimental densities of metal mold
solidification time. However, fine equiaxed α-Al dendrites cast composites. Hence, less porosity was found in the metal
were observed in the metal mold cast specimens due to the mold cast composites maximum of 3.29% at 5 wt% of FeNb.
less solidification time, as shown in Fig. 4c and f. The fine Similarly, a significant variation was found between the
α-Al dendrites structure has been improved with increasing theoretical density and experimental density of sand mold
the wt% of FeNb nano reinforcement particles which act as cast composites. Thus, the porosity of the sand mold cast
heterogeneous nucleation sites to enhance the fine dendritic composites is significantly higher, which is a maximum of
structure in both the cases, as shown in Fig. 4. 12.99% at 5 wt% of FeNb as shown in Fig. 7b. Bannaravuri
The microstructure revealed that a low degree of poros- et al. [5] argued that porosity up to 4% is reliable and accept-
ity (micro-pores) was observed in composites fabricated by able for fabrication of composites. Hence, the metal mold
metal mold as compared with sand mold. The gating system cast composites are reliable, acceptable, and it can deliver
has not facilitated in a metal mold. Thus, the pressure is good mechanical properties as compared with sand mold
employed in metal mold because the molten metal is directly cast composites.
injected. Hence, the molten metal rapidly solidified, called The interfacial bonding of reinforcement particles pro-
supercooling and formed the highly refined grain structure motes the residual pores in the fabricated composites, and
[21], as shown in Fig. 4e, f. However, the sand mold system the clustering of reinforcement particles may be causing the
provides a low cooling rate, and it leads to coarse and irregu- porosity. On the other hand, during the solidification pro-
lar networks [28] as shown in Fig. 4a–c. cess, environmental gases are entrapped into molten metal
The grain size of the as-cast composites via metal mold [5]. The porosity of the composite increased with increased
has been refined and smaller as compared with sand mold, as wt% of FeNb particles because of pore nucleation at the
shown in Fig. 4 and Fig. 5. The grain size of the composites FeNb particle surfaces resulting in the depletion of the flu-
fabricated via sand mold and metal molds is 66, 51, 47 µm idity of liquid metal [24]. Valibeygloo et al. [11] noticed
and 59, 46, 44 µm, respectively, at 1%, 3% and 5% of FeNb. similar results that the porosity of the composites increased
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for metal mold system, the composites could enhance the to brittleness raised with the addition of ceramic particles.
mechanical properties as compared to matrix alloy which is And on the other hand, the increment in tensile strength
3.38%, 7.77% and 15.66% at 1, 3 and 5wt% of FeNb. The with the addition of reinforcement also leads to a decrement
monotonic increment noticed at 5wt% of FeNb in both the of elongation. Li et al. [7] concluded that among the four
mold system. strengthening mechanisms, the main contributor to strength
The UTS of the composite gradually improved with enhancement is thermal expansion mismatch strength-
increasing wt% of FeNb particulate reinforcement in sand ening (Δ𝜎CTE ), and reported up to 5wt% of M g2Si in Al-
and metal mold casting methods. However, the UTS of the 5Cu/xMg2Si composites; thus, the UTS gradually increased
metal mold cast composites had a monotonic increase with and elongation decreased.
increased wt% of FeNb as compared with sand mold cast
composites as shown in Fig. 8. Strengthening Mechanism Analysis
The composite was expressed 12% higher in tensile
strength fabricated by metal mold in comparison with a sand To investigate the strengthening mechanism behind the
mold, as shown in Fig. 8. The % of elongation of the com- strength enhancement of mechanical properties of the com-
posites was reduced with the addition of reinforcement due posites, in principle, there were four main strengthening
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J. Inst. Eng. India Ser. D
mechanisms that cause the strength enhancement—load- In agreement with load-bearing strengthening, the FeNb
bearing, grain refinement, Orowan and coefficient of ther- particles act as resistance toward the movement of disloca-
mal expansion mismatch; it is expressed in Eq. 4 [6, 24]: tions during loading concerning the composites [24]. The
resistance of dislocation motion creates a cycle around the
Δ𝜎 = Δ𝜎load + Δ𝜎Hall−petch + ((Δ𝜎orowan )2 + (Δ𝜎CTE )2 )1∕2 fine Fe2Nb phase and disparity of thermal expansion coef-
(4) ficient, which leads to more resistance toward the motion
The Orowan strengthening takes place in association of successive density dislocations leading to load-bearing
with the distribution of FeNb particulates and their dis- capacity as well as an escalation in the potency of com-
locations. Moreover, the size of the F e2Nb phase in the posites [29]. Due to the difference in thermal expansion
composites is much larger than 1 µm. As a result, this coefficients between matrix and reinforcement particu-
mechanism seems to have no effect [7]. lates, the density dislocation and load-bearing capacity of
According to grain refinement strengthening, from the the hard particles in the matrix are increased, as a result
obtained results of a grain size measurement, grain size enhancing the strength of composites. It can be measured
gradually decreased with increasing wt% of FeNb. Hence, by Eq. 6 [24]:
the grain size of composites has refined and strengthened
1
mechanical properties as per Hall–Petch Eq. 5 [6]: Δ𝜎load = V 𝜎 (6)
2 P ym
√
Δ𝜎Hall−petch = K∕ d (5) where VP is the volume fraction of the particulates, and 𝜎ym
is the yield strength of the matrix alloy.
where ‘K’ is the Hall–Petch coefficient, and ‘d’ is the grain
diameter. The grain size of the metal mold as-cast com-
posites is much more refined as compared with sand mold
as-cast composites. It might be the reason for the strength
enhancement of metal mold cast composites.
The FeNb particles in the composites contribute to
load-bear strengthening by impeding the movement of
dislocations during loading, as stated in reference [24].
This impeded dislocation motion creates a cycle around
e2Nb phase and a difference in thermal expan-
the fine F
sion coefficients, leading to increased resistance toward
the motion of successive density dislocations, which in
turn increases the load-bearing capacity and potency of
the composites, as noted in reference [29]. The difference
in thermal expansion coefficients between the matrix and
reinforcement particles increases the density dislocation
and load-bearing capacity of the hard particles within the
matrix, thereby enhancing the strength of the composites.
This enhancement can be quantified using Eq. 6 from ref-
Fig. 9 Microhardness of Al5Cu2Ni/xFeNb composites with FeNb
erence [24]. reinforcement
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In line with a coefficient of thermal expansion mismatch reinforcement particulates and the matrix alloy.ΔT repre-
strengthening, during the solidification process—lots of geo- sents the difference between pouring temperature and test
metrical dislocations are generated because of the distinc- temperature, while VP and dP correspond to the volume per-
tion inside coefficients of thermal expansion regarding the centage and average particle size of the FeNb, respectively
Fe2Nb phase and other intermetallic compound phases of [24].
Al2Cu and Al3Ni2 [24]. Thus, the strength of the compos- During solidification, the coefficient of thermal expan-
ites increased with increasing wt% of FeNb particles as per sion difference between the matrix alloy and the reinforced
Eq. 7 [7]: FeNb particulates generates thermal stresses, resulting in
√ thermal expansion mismatch strengthening. These thermal
12Δ𝛼ΔTvp stresses in the interface between the particles and the matrix
Δ𝜎CTE = 𝛽Gm b (7)
bdp (1 − vp ) make plastic deformation more difficult, leading to improved
mechanical properties [6]. However, there may be significant
In this context, the shear modulus of the matrix alloy is variations in the solidification process and rate of heat trans-
denoted as Gm , while b represents the Burgers vector of the fer between sand and metal molds. As a result, metal mold
Al matrix, which is approximately 0.286 nm. Additionally, β cast composites could exhibit better mechanical properties
is a constant value of 1.25 and Δ𝛼 represents the difference than sand mold cast composites [19].
in coefficient of thermal expansion (CTE) between FeNb
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Microhardness Analysis fracture. Similarly, Fig. 9d–f shows that the metal mold
casted composites found smaller sized dimples and micro-
There is a remarkable variation in microhardness of the cracks found; thus, the brittle fracture takes place (Fig. 10).
composites fabricated by sand and metal mold, as shown in
Fig. 9. The microhardness of the sand mold and metal mold
cast composites is 62, 67.13, 72.83HV and 130.28, 132.26, Conclusions
150.52HV, respectively, at 1, 3, 5wt% of FeNb. Therefore,
the microhardness of the composites increased with the The Al5Cu2Ni/xFeNb composites were successfully fabri-
increasing wt% of FeNb-reinforced particulates in each of cated by the electromagnetic stir casting method by using
the two casting methods. However, the microhardness of sand and metal molds. The following conclusions were
the metal mold cast composites monotonically increased. drawn for this study:
With increasing wt% of FeNb reinforcement particulates into
Al5Cu2Ni/xFeNb, composites could decrease the grain size. 1. The microstructures analysis was revealed that fine grain
The influence of FeNb particulates increases resistance to structure in the metal mold cast composites and also
plastic deformation. As a result, it enhanced hardness and grain refinement noticed with the addition of FeNb par-
subsequently decreased the elongation of the composites in ticulate reinforcement.
both casting methods [29]. 2. The experimental density of the sand and metal mold
By increasing the weight percentage of FeNb reinforce- composites was compared with the theoretical density. It
ment particles, the load-bearing capacity and hardness of was noticed that a higher difference was observed in the
composites can be significantly improved as it increases composites developed by sand mold. Thus, the porosity
their dislocation density [3]. However, during the solidifi- of the sand mold is higher as compared with the metal
cation process, there may be differences in the coefficient of mold. Hence, the metal mold cast composites delivered
thermal expansion (CTE) between the matrix alloy and the less porosity, and it is reasonable and acceptable for fab-
reinforcement particles, which can result in the formation rication.
of a large number of dislocations around the F e2Nb phase. 3. Mechanical properties such as microhardness and ten-
These dislocations create heterogeneous nucleation sites for sile strength were evaluated, and it was found that the
precipitates [11, 24]. properties had improved. The higher tensile strength and
microhardness were noticed in the Al5Cu2Ni/5FeNb
Tensile Fracture Mechanism composite fabricated by metal mold.
4. FESEM fractography of the Al5Cu2Ni/xFeNb compos-
The tensile fracture mechanism of the broken specimen’s ites revealed that metal mold micrographs show less
surfaces was examined by FESEM. Fractography of the elongated dimples. Hence, the material is hard, and it
Al5Cu2Ni/xFeNb composites fabricated by sand mold and could have enhanced the hardness.
metal mold is shown in Fig. 9a–f. There are a number of
influencing factors for fracture in composites, such as the
presence of interface inhomogeneity, local stress field and Acknowledgements The authors would like to thank the Indian Insti-
tute of Technology Guwahati, India, for carrying out the experimental
structural alterations in the matrix [8]. The major influencing work and also thank the National Institute of Technology Manipur
factor for the cause of fractures is voids within the matrix, for granting the academic leave. The full-time research scholar Mr.
causing it to tear [30]. Increasing wt% of FeNb particulates Kumara Swamy Pulisheru acknowledges the Ministry of Tribal Affairs
reduced dimple size because of fine α-Al dendrites forma- Government of India for sponsoring the fellowship for pursuing the
Ph.D.
tion. At 5 wt% of FeNb addition, there is a significant pres-
ence of a coarse eutectic Fe2Nb phase on the fracture sur- Funding No specific grant was received for this research work from
face [7]. The micro-cracks were formed at the boundary of any public, commercial or institute funding agency in any way.
the coarse Chinese character eutectic F e2Nb heterogeneous
phase. Declarations
The FESEM fractography revealed a significant frac-
ture surface after tensile tests. Thereafter have seen Conflict of interest The authors have confirmed that they do not
have any known financial interests or personal relationships that could
the deep dimples spread over the fractured surface of have influenced the reported work in this paper. They have all agreed
the Al5Cu2Ni/xFeNb composites. The fractography of to this submission, and there is no conflict of interest.
Al5Cu2Ni/xFeNb composites casted by sand mold found
large-sized dimples as shown in Fig. 9a–c, indicating ductile
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J. Inst. Eng. India Ser. D
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