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OPEN Effects of ­Al3Ni compound

on localized plastic deformation
and creep strain of Al/Si
hypoeutectic material
Shakib Alsowidy  & Belqueis Al‑Asry *
The mechanical resistance of AS10/xNi hypoeutectic alloy with (x = 0.05% and 0.1%) has been
investigated. Vickers hardness (HV) was determined for the samples before and after sintering. All
samples were subjected to a compressive creep test at a constant temperature of 298 K and a constant
load of 45 MPa. Creep parameters, such as creep rate, sensitivity (m), time exponent (n), β, and ɣ have
been calculated and related to the Ni content. Microstructure investigation was conducted using the
scanning electron microscope technique (SEMT). After sintering, the results showed that there was
a significant improvement in the hardness with the addition of nickel. There is an increase in creep
resistance as a result of the distribution of ­Al3Ni chemical compound across grain boundaries, which
stops additional dislocation movement and hence reduces the creep rate.

Previously, in order to withstand severe operating conditions, the structural materials of the automotive industry
are made of cast iron and its alloys. Currently, the components of the structures of the automotive industry are
mostly made of Al and its ­alloys1 (Fig. 1).
Modern structural industries require strong and lightweight metals due to a growing desire to minimize
fuel consumption. These requirements are very important to the economy and environment-friendly3. So, these
conditions must be taken into account. Aluminum and its alloys are currently the most popular light metals. The
greatest Al advantages include its low density about (2.7 g/cm3) and high plastic deformation up to 30 ­percent4.
Aluminum alloys, such as Al/Si, Al/Mg, Al/Cu, etc., have various characteristics such as resistance to cor-
rosion, mechanical strength, good castability, working at RT up to 400 °C, responsive to heat- treatment, and
low ­cost5. All alloys mentioned above have α-Al dendrite phase. The spacing between dendrites is one of the
important factors in determining the alloy properties like the strength of the alloy. As the spacing between main
dendrites and secondary dendrites becomes smaller, the structure becomes ­fine6. The addition of an alloying
element to the Al major produces secondary phases. These phases are intermetallic compound phases that
reduce the secondary dendrite arms spacing (SDAS)7. On the other hand, heat treatment of metal is considered
a favorable technique for enhancing characteristics of aluminum after casting and cold w ­ orking8.
Aluminum Silicon alloys are commonly subjected to a variety of mechanical loads and relatively harsh envi-
ronmental conditions when employed in structural a­ pplications9. These stresses can cause long-term irreversible
plastic deformation before failure even if they are below the yield strength of aluminum a­ lloys10. As a structural
material has a high resistance to ambient environmental stresses as the service life has improved. Microstruc-
ture defects include dislocations and grain boundaries. Small grain size structure means a larger area of grain
boundaries that act as barriers to the dislocation motion. So, the resistance to dislocation motion increases with
increasing grain-boundary a­ rea11. It is reported that the strength of the material is related to the grain size by
the following Hall–Petch e­ quation12,

σ =k D−1/2 (1)
where σ is the yield strength is a constants and D is the average grain size. This means that decreasing grain size
and increasing grain boundary area reflects on the strength of ­mater13. From those mentioned above, localized
plastic deformation and mechanical plastic strain decrease as microstructure defects ­increase14.
However, in addition to the possibility of high dislocation concentration in pure aluminum that may produce
after cold-working, pure Al has significantly poor mechanical properties, such as low hardness (~ 20 HB) and
low yield strength (~ 70 MPa)14. The poor mechanical properties of this material are a result of microstructure

Department of Physics, Faculty of Science, Sana’a University, Sana’a, Yemen. *email: [email protected]

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Figure 1.  The car body is made of lightweight aluminum ­alloy2.

­defects15. To address all of these issues, the density of defects across the dendritic microstructure must be reduced
dramatically. The goal of the current study is to improve the microstructure characteristics of the AS10 alloy
in order to increase its mechanical strength and reliability factor by adding traces of nickel alloying element.

Materials and methods

Powder Aluminum (Al; 99.99%), Silicon (Si; 99.99%) and Nickel (Ni; 99.99%) have been chosen in this work. All
materials were obtained from the BDH company (England) by Materials Science Laboratory at Sana’a University.
The nanopowder aluminium, silicon, and nickel were accurately weighted in balance to make the required com-
position as shown in the Table 1. The balanced elements were mixed in a powder form at room temperature. The
balanced powder mixture was subjected to compression using a hydraulic pressure system with a constant load
of 250 KN for 5 min for all three samples. The compacted circular disks obtained with dimensions of 6 × 32 mm
is shown in Fig. 2. After that, the compressed samples were sintered in a controlled atmosphere furnace at about
773 K to allow the bounding of particles for each other.

Characterization
The Vickers hardness test (localized plastic deformation resistance or impact force resistance) was performed
using mechanical equipment designed in the Materials Science Laboratory at the Physics Department in the
Faculty of Science, Sana’a University, Yemen, as shown in Fig. 3.
A compressive creep test was performed on all samples at a constant load of 45 Mpa and a constant tempera-
ture of 298 K by using a compression device (CMT4000,China).
Microstructure investigation was conducted using the scanning electron microscope technique (SEMT)
(JEOL JSM 6510 Lv). Imaging has been done by irradiating samples with a highly accelerated electron beam.
Secondary electrons (SE) and backscattered electrons (BSE) produced from the top and beneath the samples
were detected and processed by scanning backscattered electron detector (SBED) and finally displayed as an
image on the screen.

Alloy Sample Si (%) Ni Al

AS10 A0 10 0 Balance
AS10-0.05Ni A1 10 0.05% Balance
AS10-0.1Ni A2 10 0.1% Balance

Table 1.  Chemical composition of the Al–Si–Ni alloys.

Figure 2.  Compressed sample.

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Figure 3.  Schematic diagram of Vickers hardness tester.

Vickers hardness
In Vickers hardness testing, Pyramidal indenters methods are used and produce geometrically identical
­indentations16. On each specimen, at least three indentations were made and the average of these indentations
served as the representative hardness value. The Vickers hardness number, HV is calculated using the following
­expression17:
L
HV = 1.85 (2)
d2
where L is the indentation load in kg and d is the mean diagonal of the indentation in mm.

Transient creep strain

With regard to the transient interval of the creep curve, the transient creep strain is commonly touted by the
familiar Friedel’s e­ quation18:
εtr = βtn (3)
where Ɛtr and t are the transient creep strain and time. β and n are the transient creep parameters. The exponent
n is determined from the slope of the relation between lnεtr and lnt, while the coefficient β is calculated from the
intercepts at lnt = 0 as clear from the Eq. (4):
ln εtr = lnβ + n lnt (4)

Steady‑state creep stage

The applied stress provides a driving force for the dislocation movement and diffusion of atoms. As the stress is
increased, the rate of deformation also increases. In general, it is found that
ε̇st ασn
where n is termed the stress exponent.
By utilizing the relationship between the coefficient β and the strain rate of steady state creep (ε̇st), we are able
to determine the exponent ɣ, as indicated in the e­ quation19:
β = β0 (ε̇st )γ (5)
By taking the logarithm of both sides of the equation:
lnβ = lnβ0 + γlnε̇st (6)
The equation governing the rate of steady state creep is:
 
Q
ε̇st = Aσn exp − (7)
RT
where, Q is the activation energy; n is the stress exponent; and A is a constant.
Strain rate sensitivity parameter (m) was calculated by the e­ quation20:
m = (∂ ln σ/(∂ ε̇st )) (8)
Parameter (m) is very important in characterizing structure superplastic deformation.

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The activation energy is the energy needed to change the position, and its value is determined by the
­equation21:
Q = −R(Ln(ε̇st )/Ln(1/T)) (9)
where T and R are temperature (Kelvin), and the gas constant, respectively.

Result and discussion

Mechanical properties
Vickers hardness measurements
Table 2 lists the Vickers hardness values of AS10-xNi specimens before and after sintering. The hardness increases
from 67 to 86.9 at 0.05% Ni and also from 80 to 92.9 at 0.1% Ni. From Table 2, the highest hardness value at 0.1%
Ni before sintering is 80 HV, while the highest hardness value at 0.1% Ni after sintering is 92.95 HV.
From the Vickers hardness results, it is found that by increasing Ni-content, the HV significantly increases
before and after sintering as shown in Fig. 4. From Al/Ni-binary phase diagram, it is clear that the maximum
solubility of Ni into Al is 0.04% and most Ni constituent atoms react with Al atoms to produce ­Al3Ni chemical
compound. By increasing Ni-content the amount of ­Al3Ni also increases as observed in images of SEM. The
formation of a hard ­Al3Ni-IMC improves mechanical strength that is a very important characteristic in automo-
tive Al-alloys22,23.
In the literature ­studies24 and like ceramic materials, ­Al3Ni chemical compound has a complex crystal struc-
ture (orthorhombic), and works as a dislocation slip resistance. So, the dislocation slip is destroyed and the
material becomes ­hard24,25. All these factors make Al alloy stronger and more surface indentation resistance.

Creep properties
Isothermal creep curves for the tested alloys were studied by applying a stress of 45 Mpa and a deformation
temperature of 298 K. The effects of Ni alloying element additions on the mechanical performance of Al/Si-based
alloy are described as creep behavior (Fig. 5). As shown in this Figure, there are three significant regimes: the
first regime represents the primary creep. In this regime, the strain is relating with time by the formula, Eq. (3).
As testing time increases, the transient strain also increases with a deceleration rate (Figs. 6, 7, 8, 9 and 10). This
behavior may be due to two main reasons, (I) residual dislocation motion in the microstructure, (II) static fric-
tion stress (σ0). The second constant creep rate regime is called the steady-state creep region. In this region, the
dislocation motion is uniform and the creep parameters of the materials are determined during this regime as
exhibited in Eq. (5). After this region, the nucleation of necking regions is ­expected26. In the necking regions, the

Vickers hardness (Hv)

Material Before sintering After sintering
A0 56.01 59
A1 67.37 86.98
A2 80.04 92.95

Table 2.  Vickers hardness number (VHN) for alloys.

95 Before Sentring
After Sentring
90
Vickers Hardness (HV)

85

80

75

70

65

60

55

0.00 0.02 0.04 0.06 0.08 0.10

Content Ni (%)

Figure 4.  VH as a function of Ni-content.

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18
A0 (AS10)
16 A1 (AS10-0.05Ni)
A2 (AS10-0.1Ni)
14

12

Strain (%)
10

0
0 50000 100000 150000 200000 250000 300000 350000
Time (Sec)

Figure 5.  Isothermal creep curve of a constant applied stresses 45 Mpa.

0.0000030
A0
A1
0.0000025
A2

0.0000020
Creep rate (Sec)-1

0.0000015

0.0000010

0.0000005

0.0000000

0 50000 100000 150000 200000 250000 300000 350000

Time (Sec)

Figure 6.  Relation of creep rate versus creep time for AS10-xNi alloys.

-4.5

-5.0

-5.5
Ln ε tr

-6.0

-6.5

-7.0 A0
A1
A2
-7.5
6.0 6.5 7.0 7.5 8.0 8.5 9.0
ln t

Figure 7.  Relation between (Ln Ɛtr) and (ln time) for AS10 at different Ni content and stress 45 Mpa.

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0.40

0.38

0.36

0.34

Sensitivity (m)
0.32

0.30

0.28

0.26

0.24

0.22

0.00 0.02 0.04 0.06 0.08 0.10

Content Ni (%)

Figure 8.  Relation of strain -rate sensitivity with Ni content.

stress concentration becomes more and finally leads to failure as observed in the third regime in Fig. 5. In the
same Figure, the minimum creep rate decreases with increasing Ni-content as observed through the variation
of slope of steady-state regions. The AS10-0.1Ni alloy exhibits the highest creep resistance (low creep rate). This
improvement in creep resistance is attributed to the presence of A ­ l3Ni, as shown in SEM Fig. 11 b,c which spreads
across particles porosities and grain boundaries and does not allow more dislocation movement to occur and then
lower creep r­ ate27. This distribution of A
­ l3Ni helps to resist dislocation motion and finally leads to a lower creep
rate. It is found that with increasing nickel content, the average particle size d ­ ecreases28. As the nickel content
increases, the diffusion of Ni atoms in the Al lattice increases. This diffusion leads to the growth of aluminum
dendrite ­arms29, particularly the secondary dendrite arms (SDA) as shown in Fig. 12.
During solidification, nickel element promotes the formation of smaller and uniform grains. This refinement
of the microstructure lead to improve mechanical properties, including higher strength and better resistance to
creep ­deformation30.
In order to specify the effect of deformation time on the creep-strain acceleration, the data of the relation-ship
between creep strain rate and time have been extracted from Fig. 5 and replotted in Fig. 6.
In order to identify the mechanism of creep deformation, the activation energy of deformation has been cal-
culated and compared with the reference ­map31. The activation energy was calculated from Eq. (9) and tabulated
in the Table 3. From this table and Fig. 6, it can be concluded that when adding Ni element to Al/Si alloy, the
secondary creep rate decreases while the creep lifetime in this stage increases. The activation energy increases
with increasing nickel content and this indicates that the material’s resistance to deformation is improved. This
means that as the Ni-content increased as the lifetime of the material increased. This refers to the enhancement
in creep resistance and life ­time32.
Figure 7 shows the transient creep behavior as a plot of lnƐtr against lnt. From the curves, the slope represents
time exponent (n) while the intercept represents (β) parameter. All these parameters are shown in the Table 4 as
a function of Ni-content. The exponent (n) was found to have values ranging from 0.222 to 0.653. These values
obtained are in well consistent with the values reported by S­ alem18.
The steady-state strain rate ε̇st of the alloys has been calculated from the gradient of the regular parts of the
acquired creep curves in Fig. 5. According to the Eq. (8), the mechanical response of materials is determined via
the sensitivity for deformation loads. This sensitivity parameter has been calculated from the slope of the steady-
state regions of creep curves in Fig. 5 and tabulated as a function of Ni-content as shown in Fig. 8.

4–2 Scanning electron microscope

In order to investigate the microstructure and the effects of Ni addition on the characteristics of AS10 alloy, mor-
phology and topography have been conducted on unmodified and modified specimens by secondary electrons
(SE) and backscattered electrons (BSE) images produced by scanning electron microscopy as shown in Fig. 9.
It’s well known, that the microstructure of Al/Si/Ni contains many different phases and has a finer structure than
that containing only one or two p ­ hase33. This phenomenon has been expected and detected in this work when
modifying Al/Si binary composition by adding traces of Ni-atoms into AS10 binary. These changes in microstruc-
ture size are very clear when comparing between Fig. 9a–c. In Fig. 9, it can be seen that there are three regions
contained in the overall structure. The first region is the elementary Al powder large particles with a black-gray
color. The second region is the master alloy which consists of primary silicon surrounded by the third region of
the eutectic Al-Si structure with white grey.
Because the force increases gradually during compaction, the nanocomposite structure begins to produce a
sandwich structure Fig. 9. This occurs due to the collision of particles during compaction. During sintering, this
structure easiest the welding of the particles together and turns to produce rough surfaces with coarse grains
(large size) as can see in Fig. 10. The successive welding of the particles continues as a result of the sintering

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Figure 9.  SEM images of the (a) hypo-eutectic AS10, (b) Ni added (500 ppm) and, (c) Ni added (1000 ppm).

treatment. This leads to making a dense structure and so more hardness. It can be seen that the primary silicon is
independent in the Al-Si alloy. In many regions but not all, it can be seen cracked silicon particles. This observa-
tion may due to the indentation region that has been occurred during testing. In the unmodified and modified
alloys, there are many porosities uniformly distributed in the overall structure.

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Figure 10.  Different grain shapes due to compaction and sintering.

If one compares binary and ternary alloys from Fig. 11a–c, respectively, he will detect that in binary composi-
tion the particles are in the form of elongated plates with large sizes whereas they are small elongated plates and
semi-sphere particles in the ternary composition. This reduction in the size of the modified alloy is attributed to
the parts of million of Ni atoms that are added to the alloys. From the Al/Ni binary equilibrium phase-diagram,
Al and Ni atoms engaged in a chemical reaction and formed ­Al3Ni IM’C-phase. It can be observed that ­Al3Ni
is included in the structure as small black particles are distributed randomly in the microstructure as shown
in Fig. 11c. The key factor behind HV’s improvement is this new phase. Like ceramic materials, any chemical
compound works, as a dislocation slip resistance, so the dislocation slip is destroyed and the material becomes
­harder34,35. These factors resist the indentation of the Al surface. Figure 12b showcases an image that has been
processed using ImageJ software, clearly highlighting the distinct dendritic structure of the Aluminum ­particles36.

Conclusion
The present research investigates the mechanical properties and microstructure of Al-10%Si added to it 0.05%
and 0.1% Ni. The ternary alloy has a higher hardness than the binary one due to the formation of the chemical
compound ­Al3Ni. The variation in slopes of steady-state areas shows that the minimum creep rate reduces with
increasing Ni concentration. The highest creep resistance is found in the AS10-0.1Ni alloy (low creep rate).
­Al3Ni, which distributes across grain boundaries, prevents further dislocation movement, which in turn lowers
the creep rate, and is responsible for this improvement in creep resistance. The activation energy rises as nickel
concentration rises, which suggests that the material has better deformation resistance. This indicates that the
material’s lifetime rose as the Ni-content rose. If one compares the binary and ternary alloys, from SEM photos
it will see that the silicon powder particles in the ternary composition are smaller, and semi-spheres. The addi-
tion of Ni atoms to the alloys may be to blame for this reduction in the size of the modified alloy’s structure.

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Figure 11.  Binary and ternary alloys form.

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Figure 12.  The distinctive dendritic structure of the Aluminium particles.

Materials m ε̇st Q(KJ ­mol−1)

A0 0.37861 4.3E−5 25
A1 0.23927 1.23E−7 39
A2 0.23168 7.31E−8 40

Table 3.  Comparison of the steady – state creep characteristics of the tested alloys.

Materials n β ɣ
A0 0.22266 0.00136 0.656461785
A1 0.1545 9.51289E−4 0.437330623
A2 0.65394 1.12447E−5 0.693559402

Table 4.  Comparison between transient creep parameters for the tested alloys.

Data availability
The authors confirm that the data supporting the findings of this study are available within the article.

Received: 22 September 2023; Accepted: 27 December 2023

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Author contributions
B.prepared the samples, analyzed them, and wrote the manuscript. S.reviewed the analysis and manuscript.

Competing interests
The authors declare no competing interests.

Additional information
Correspondence and requests for materials should be addressed to B.A.-A.
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