Results in Physics 14 (2019) 102465

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Results in Physics
journal homepage: www.elsevier.com/locate/rinp

Synthesis of equi-atomic Ti-Al-Mo-Si-Ni high entropy alloy via spark plasma T

sintering technique: Evolution of microstructure, wear, corrosion and
oxidation behaviour
⁎
L.R. Kanyanea, , N. Malatjia, A.P.I Popoolaa, O.S.I Fayomia,b
a
Department of Chemical, Metallurgical and Materials Engineering, Tshwane University of Technology, P.M.B. X680, Pretoria, South Africa
b
Department of Mechanical Engineering, Covenant University, P.M.B. 1023, Canaan Land, Ota, Nigeria

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

Keywords: Equi-atomic Ti-Al-Mo-Si-Ni high entropy alloys (HEAs) with outstanding wear and oxidation properties is fab-
High Entropy alloys (HEAs) ricated by means of Spark plasma sintering (SPS) technology. The influence of sintering temperature on surface
Spark plasma sintering microstructure, phase evolution, densification, microhardness, corrosion, wear and oxidation properties of de-
Wear veloped Ti-Al-Mo-Si-Ni HEAs was investigated at 800 °C, 900 °C and 1000 °C. The microstructural evolutions of
Oxidation
the synthesized HEAs were evaluated by means of scanning electron microscope coupled with energy dispersive
spectroscopy (SEM/EDS). The SEM images showed no significant major porosity; however for the HEA sintered
at 800 °C, the densification results prove that 2.6% porosity is present in the HEAs. XRD showed the presence of
BCC and FCC solid solution structures with intermetallic precipitates of TiSi2 and Ni2Si2. The Vickers micro-
hardness and wear resistant properties was evaluated using diamond base micro hardness tester (EMCO) and
tribometer (Rtec) respectively, with the sample sintered at 1000 °C showing maximum densification of 98.8%
with microhardness of 612HV and coefficient of friction (CoF) of 0.23µ. The developed HEAs also showed good
oxidation resistant behaviour after a test using thermal gravimetric analyzer (TGA).

Introduction additive manufacturing (LAM) and casting are used to produce this
class of alloys. However, in these work spark plasma sintering (SPS) is
Industrial development requires materials with good oxidation and used as a fabrication technique. SPS is known for its ability to sinter
wear resistant materials [1]. Substitutional alloys also known as high materials which possess good mechanical properties achieved by con-
entropy alloys (HEAs) remains promising alloys for such as chemical trolling the grains size of the developed alloy when related to other
plants, nuclear plants and furnace parts. These alloys are known to offer conventional methods [12,13].
good mechanical properties for advanced engineering application due Chen, Fu [14] Synthesized Co1.5CrFeNi1.5Ti and
to their nature of forming solid solution phases [2–5]. Today, HEAs Al0.2Co1.5CrFeNi1.5Ti high entropy alloys and investigated the tribolo-
remain the promising multi principal element alloys with combination gical properties of the alloy. The developed alloys showed better wear
of outstanding chemical and mechanical properties for advanced en- properties as compared to conventional wear resistant steels. High
gineering application at both room and elevated temperatures [6–8]. temperature oxidation properties of equi atomic NbMoCrTiAl HEA was
For example, Senkov et al. [9] studied the mechanical properties of studied by Gorr et al. [15], the surface of the synthesized HEA was
Ta20Nb20Hf20Zr20Ti20 HEA, the researchers found that the alloy ex- largely covered by porous and non-protective oxide film consisting of a
hibited outstanding combinations of room temperature and high tem- mixture of various oxides after oxidation test.
perature mechanical properties. Furthermore, studies showed that bcc Material selection is an important factor in developing HEAs, Mo, Ni
solid solution phase structures of developed Nb25Mo25Ta25W25 and and Si were considered due to high melting points, these elements are
V20Nb20Mo20Ta20W20 HEAs [10] presented enhanced mechanical be- chosen as prime candidates for the new HEA system. To permit the
havior at various temperature. Other studies includes Hf25Nb25Ti25Zr25 formation of a protective oxide file during thermal gravimetric test, Al
HEA [11] which presented excellent structural stability. and Ti were incorporated to the alloy system, while Ti, Si and Al are
Numerous methods such as spark plasma sintering, sputtering, responsible for reducing the alloy density.

⁎
Corresponding author.
E-mail address: lrkanyane@gmail.com (L.R. Kanyane).

https://doi.org/10.1016/j.rinp.2019.102465
Received 30 March 2019; Received in revised form 19 June 2019; Accepted 19 June 2019
Available online 22 June 2019
2211-3797/ © 2019 Published by Elsevier B.V. This is an open access article under the CC BY-NC-ND license
(http://creativecommons.org/licenses/BY-NC-ND/4.0/).
L.R. Kanyane, et al. Results in Physics 14 (2019) 102465

Table 1
Summarized pattern of fabricated TiAlMoSiNi.
Alloy Temperature (°C) Pressure (kPa) Holding Time (min) Theoretical Density (g/cm3) Actual Density (g/cm3)

Ti-Al-Mo-Si-Ni 800 50 8 5.3 5.1626

900 5.1976
1000 5.2406

For that reason, in this study, attempts were made to fabricate equi
atomic Ti-Al-Mo-Si-Ni HEAs under different sintering temperature. The
effect of sintering temperature on microstructures, formation of phases,
microhardness, oxidation and tribological properties of the developed
HEAs are investigated.

Experimental method

Ti, Al, Mo, Si and Ni powders were mixed in equi atomic ratio of
20% each using tubular mixer for a period of 8 h. The mixed powders
were poured into a 40 mm diameter graphite die. SPS system (FCT
Systeme GmbH Rauenstein) was used to consolidate the powders at
different sintering temperature of 800, 900 and 1000 °C. During sin-
tering, heating rate of 100 °C/min with a holding time of 8 min was
Fig. 1. Densification of Ti-Al-Mo-Si-Ni sintered high entropy alloy (a) 800 °C, used for each sintering temperature. Constant Applied pressure of
(b) 900 °C and (c) 1000 °C. 50 MPa was used.
Sintered HEAs were sand blasted and the densities were measured
using Archimedes method.
Proper metallographic procedure was followed, the synthesized
HEAs samples were cut transversely (5x5mm) and mounted in an

Fig. 2. SEM micrographs of Ti-Al-Mo-Si-Ni sintered high entropy alloy (a) 800 °C, (b) 900 °C and (c) 1000 °C.

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L.R. Kanyane, et al. Results in Physics 14 (2019) 102465

Fig. 3. EDS of TiAlMoSiNi (Equi-atomic) sintered high entropy alloy.

Fig. 4. XRD patterns of sintered Ti-Al-Mo-Si-Ni high entropy alloys.

epoxy- based resin, polished using metallography procedures and 1.5 V to stop potential of −1.5 V and at a scan rate of 0.001 mV/s. The
etched with kroll agent solution for investigating the microstructural dynamic parameters of the fabricated alloys were determined using the
evolution of the developed alloys. The microstructures of Ti-Al-Mo-Si- liner fit method on the curves using the NOVA software.
Ni were characterized by means of SEM. The phases present in the Emco TEST microhardness tester was used to measure the used the
synthesized HEAs were identified using an XRD and present phases microhardness properties of the developed alloy. The indenting load of
were revealed using X-Pert High Score Plus software. The electro- 100 kgf and a dwell time of 10 s. The tribological behaviour of the
chemical behavior of the specimens was studied in 0.5 mol/L of H2SO4. synthesized alloy was studied using Rtech tribometer with a load of
The experiment was achieved using Autolab potentiostat equipped with 150 N form the contact ball for 300 s and a sliding distance of 3 mm.
nova software. Polarization curves were recorded at a start potential of Thermal gravimeteric Analyzer (TGA) was utilized to evaluate the

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L.R. Kanyane, et al. Results in Physics 14 (2019) 102465

Table 2 effect of sintering temperature on the oxidation behaviour of the fab-

The chemical mixing enthalpy (ΔHijmix; kJ/mol) of binary equi-atomic alloys ricated high entropy alloys. The fabricated alloys were studied at
calculated by Miedema’s approach. temperatures of between 45 °C and 900 °C. The heating rate of 10 °C/
Elements Ti Al Mo Si Ni min was employed while feeding 20 mL/min of air.

Ti 0 −30 −4 −66 −35

Al 0 −5 −19 −22
Results and discussion
Mo 0 −35 −7
Si 0 −35 The experimental pattern of the fabricated HEAs obtained for
Ni 0 TiAlMoSiNi are showed in Table 1 below. Applied pressure and holding
time of the developed HEA were kept constant during the SPS process.
The relative densities of the synthesized HEAs at varied sintering
Table 3
temperature parameters are presented in Fig. 1. The developed HEAs
The calculated values of parameters (ΔHmix, ΔSmix, Tm, δ and Ω) for the in-
showed high densification of greater than 97% are reached for all sin-
vestigated alloys.
tered HEA samples at all sintering temperature. Furthermore, it is evi-
Alloy ΔHmix (KJ/ ΔSmix (J K−1 mol−1) Tm (K) δ Ω dent that the densities of the sintered HEAs increase with increasing
mol)
temperature. Maximum relative density of 98.88% is attained at
Ti-Al-Mo-Si- −41.3 13.38 1837 1.519% 0.595 1000 °C, followed by 900 °C with 98.06% and lastly 800 °C with
Ni 97.408% densification.

Microstructural analysis

Fig. 2 present the SEM micrographs of the fabricated Ti-Al-Mo-Si-Ni

HEAs. The effect of sintering temperature (at 800 °C, 900 °C and
1000 °C) on the morphological evolution was evaluated on the syn-
thesized HEAs. For each sintering temperature effect, the micrographs
show no significant surface pores. The fabricated HEAs shows gray (Ti
rich phase), white (Mo rich phase) and small black precipitated spots
(Si rich phase) contrast phases present. The microstructure also shows
no evident of crack or initiation of stress at all sintering temperatures.
However the densification results proves that there is porosities avail-
able in all the developed alloys ranging from 2.6% for HEA sintered at
800 °C and 1.12% porosity for HEA sintered at 1000 °C. The HEA sin-
tered at 1000 °C (Fig. 2c) portray smaller grain size with thicker grain
boundaries which promotes the increase in the TiSi2 phase rim. This
Fig. 5. Effect of sintering temperature on Microhardness properties. increase in grain size can alter the microhardness and tribological
properties of the material. Comparatively, Fig. 2a consists of lager
grains size with thinner grain boundaries as compared to Fig. 2b and c
(sintered at 800 °C and 900 °C respectively). This morphological feature
also indicates that these alloys have similar phase composition and
solidification behaviour as indicated on the SEM micrographs.
From Fig. 3(a) spectrum 22, it is clear that the dark gray section
represented is a Ti-rich (BCC) phase. EDS also detected Si rich BCC at
the black sports as represented by Spectrum-21 (Fig. 4d). Spectrum 20
presented the TiSi-rich phase. The developed HEAs are expected to
show good strength due to the presence of the BCC structure present.

Phase formation

Table 2 present the chemical mixing enthalpy (ΔHijmix; kJ/mol) of

binary equi-atomic alloys calculated by Miedema’s approach while
Table 3 presents the calculated values of mixing enthalpy and entropy
of Ti-Al-Mo-Si-Ni HEAs. Zhang et al. [16] anticipated that for the for-
mation of BCC/FCC solid solution phases, the prediction parameters
Fig. 6. Potentiodynamic polarization curves for TiAlMoSiNi HEAs in 0.5 mol/L should be Ω ≥ 1.1 and δ (%) ≤ 6.6%. From the empirical calculations
H2SO4 solution at room temperature. presented in table 3, the parameters of Ω and δ (%) for the synthesized
HEA were found to be 0.595 and 1.519% respectively. It is vibrant that
Ω parameter matches the suggested predictions by Zhang while δ (%)

Table 4
Alloy properties derived from potentiodynamic polarization curves by liner fit.
TiAlMoSiNi samples Ecorr, Obs (V) jcorr (A/cm2) Corrosion rate (mm/year) Polarization resistance (Ω)

1000 °C −0.31615 1.01E-03 0.007788 2692.94

900 °C −0.31365 6.78E-04 0.009147 2454.67
800 °C −0.43191 1.86E-07 0.010909 2034.1

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L.R. Kanyane, et al. Results in Physics 14 (2019) 102465

Fig. 7. SEM image of TiAlMoSiNi HEA after wear test sintered at a) 800 °C and b) 1000 °C.

parameter breaks the solid solution formation rules for the multi-
component HEAs as proposed. Hence, the XRD results present the In-
termetallic of Titanium silicide and Nickel silicide shown in Fig. 4. This
phenomenon indicates that the formations of intermetallic or complex
phases are to be found in the HEA system as confirmed by the XRD
results (Fig. 4). The XRD gives a clear confirmation that equi atomic Ti-
Al-Mo-Si-Ni HEAs consists of combination of BCC (Ti, Mo and Si-rich
phases) along with intermetallic compounds of TiSi2 and Ni2Si2. BCC in
the alloy is expected to give better mechanical properties. The devel-
oped intermetallic compound was due to high entropy of mixing of the
binary components (Ti, Si) and (Ni, Si) −66 and −35 kJ/mol respec-
tively.

Microhardness

Fig. 5 present microhardness properties of the fabricated HEAs of

equi atomic TiAlMoSiNi. From the results, it is observed that the mi-
Fig. 8. CoF of developed HEAs sintered at various sintering temperature and crohardness properties of the developed TiAlMoSiNi HEAs increases
composition effect. with increasing sintering temperature. The obtained results are inline
with, Makena and Shongwe [17], Otto and Dlouhý [18] and Shongwe
and Diouf [19] who attested that high temperature sintering results in
improved mechanical properties. Maximum microhardness of 612HV0.1
was evident at sintering temperature of 1000 °C. Cantor et al. [20],
stated that the reasonable strength of HEAs can be justified by severe
lattice distortion, particularly the body centered cubic (BCC) struc-
tured. The fabricated HEAs proved to have W-rich and Si-rich phases
BCC phases which are responsible for high microhardness values.
Gowon [24], highlighted that the increase in microhardness properties
of the developed HEAs values is due to particle rearrangement,
homogeneous phase distribution and reduction of grain size which
bring about an increase densification of the alloy and directly influence
increase in the hardness properties of the synthesized HEA.

Electrochemical analysis

Fig. 6 shows the corrosion performance of TiAlSiMoNi equi-atomic

HEA fabricated at 800, 900 and 1000 °C. The Tafel results extrapolated
Fig. 9. Effect of sintering temperature on thermal stability of synthesized by means of dynamic linear fit are represented in Table 4 below. The
TiAlSiMoNi HEAs. polarization results for all fabrication temperatures generally show
good corrosion resistance in the corrosive medium. From the corrosion
data presented by Table 4, the highest polarization reach (Rp) is
2692.94 Ω which is for the alloy fabricated at 1000 °C. Huge deviation

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L.R. Kanyane, et al. Results in Physics 14 (2019) 102465

Fig. 10. SEM image of TiAlSiMoNi HEA after TGA test (a) 800 °C and (b) 1000 °C.

of current density was observed between sample sintered at 800 °C are also responsible for improved tribological performance due to their
(1.86E−07 A/cm2) and 1000 °C (1.01E−03 A/cm2). Even thou the hardness in nature [24]. Overall tribological properties of the devel-
potential of the sample sintered at 800 °C is lower, the sample possess oped HEAs are outstanding as compared to commercial alloys such
low current density. This could be a result of high diffusion of particles stainless steel [25] and Ti alloy [26] which develops oxides during wear
at almost all sintering temperature which prevent acidic attack and test as a result of friction. The presence of BCC phase and intermetallic
current penetration on the alloy surface [17,21]. High sintering tem- phases present in the alloy system also helps in balanced mechanical
perature also resulted in current density of 1.01E−03 A/cm2. The ob- strength and ductility [27,28].
served outstanding corrosion resistant properties of the developed alloy
can also be attributed to the present elements [14,22] in the HEA Thermal gravimetric test results of developed HEAs
system such as Al, Ti, Mo and Ni which are known for anti-corrosion Sample weight and temperature change plot. The developed TiAlSiMoNi
properties. high entropy alloy at varied sintering temperature is presented in Fig. 9.
From the sample weight loss against the temperature in air from 45 °C
Wear analysis to 900 °C, it is evident that the sample which is sintered at 1000 °C
shows that it is more resistant to oxidation as compared with the others
Fig. 7 present SEM wear scars of synthesized TiAlMoSiNi HEA sin- with a minimal mass gain of 2.04 mg. There was a huge deviation of
tered at (a) 800 °C and (b) 1000 °C and the effect of sintering tem- mass gain for sample sintered at 800 °C at 550 °C. This early rapid mass
perature on wear properties of the developed HEA is assessed. Gen- gain proved that the alloy developed oxide scales which resulted in
erally, developed HEAs with high microhardness properties showed poor high temperatures oxidation resistant at temperatures of more
better wear resistance. It could be observed that at lower sintering than 550 as compared to alloys sintered at 900 and 1000 °C. While on
temperature the developed HEA shows more deterioration as compared the other hand sample sintered at 900 °C was showed to be stable up to
to the HEA sintered at 1000 °C. Both micrographs show excessive ma- 610 °C throughout the exposure in air at 40 °C until 900 °C. The sample
terial loss. This is attributed to the fact that the fabricated HEAs were shows high degree of deflection between 610 °C and 950 °C with
highly resistance to plastic deformation which resulted in material loss average mass change of 3.06 mg. High temperature sintering proved
on the alloy surface [23]. Fig. 7a also shows furrows and grooves on the to have much influence on the oxidation properties of the developed
surface and also showed accumulation of detached debris as well as HEAs.
cracks which can be lined with high weight loss as compared to Fig. 7b.
On the other hand, Fig. 7b shows material carry overs with no plastic SEM of the oxidized HEAs. Fig. 10 present the surface microstructural
deformation from the contact ball and also adhered wear debris are evolution of oxidized TiAlSiMoNi high entropy alloy fabricated at
present on the SEM image. varying sintering temperature. From the micrographs it can be
Fig. 8 present the average coefficient of friction (CoF) responds of observed that the formation of oxide on the surface of the developed
the sintered HEAs. This demonstrates the response of the synthesized HEAs is evident after exposing the sample to 950 °C while at the heating
alloys to the working load of 150 N for a period of 5 min. Developed rate of 20 °C/min while feeding air at 20 mL/min. The developed oxides
HEAs with higher hardness properties resulted in increased resistance on the surface of the synthesized HEAs were identified by means of
to wear loss. From the results, there is a general trend between sintering XRD. The addition of Ti, Al, Si, Mo and Ni all resulted to form their
temperature of the developed HEAs and the CoF could be deduced. oxide. These oxides formed prevent oxygen to diffuse on the alloy and
From all the synthesized HEAs, as the sintering temperature increases, hence reduced the oxidation rate of the alloy at elevated temperature.
the CoF decreases. Maximum CoF was found to be 0.273 µ for 4 A Lavoie et al. [29] stated that even though Ni2Si2 possess good high
(sintered at 800 °C) while minimum CoF was at 1000 °C with average temperature properties, the agglomeration of Ni2Si2 becomes the main
value of 0.219 µ. These may be attributed to the hardness test results. degradation mechanism at high temperatures. When compared to TiSi2
Which also showed that the higher the sintering temperature, the phase, Ni2Si2 has substantially lower stress at ambient temperature due
higher the microhardness. Also, high diffusion of particles is expected at to low relaxation temperature. TiSi2 phase present in the HEA is known
the sintering temperature of 1000 °C which enhances the tribological for its superior properties such as high melting point, low density and
properties of the alloy. The incorporated materials such as Ni and Mo good oxidation resistance [30]. The developed scales of the SEM images

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L.R. Kanyane, et al. Results in Physics 14 (2019) 102465

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