CHAPTER 1

INTRODUCTION

1.1 THERMAL SPRAY COATING

Thermal spray coating is a widely adopted technique used to
enhance surface properties by depositing molten or semi-molten materials
onto a substrate. It encompasses various methods, including plasma spray,
flame spray, high-velocity oxy-fuel (HVOF), and electric arc spraying. In
thermal spraying, feedstock in the form of powder or wire is melted using
a heat source such as a flame or plasma arc, and then propelled at high
speed toward the substrate using a carrier gas. On impact, the droplets
flatten, solidify, and build up to form a dense, adherent coating. This
technique is especially useful for applying ceramics, metals, and
composites to protect components from wear, corrosion, oxidation, and
high temperatures.

Figure 1.1 HVOF process

Plasma spraying, a subset of thermal spray, is particularly effective
for depositing high-melting-point materials like Yttria-Stabilized Zirconia
(YSZ), making it ideal for thermal barrier coatings (TBCs) in aerospace
and power generation industries. The advantages of thermal spray include
a wide material selection, minimal heat input to the substrate, and the
ability to coat large or complex geometries. However, surface preparation
is critical for achieving good adhesion, and the porosity of the coatings may

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require post-processing in some applications. Overall, thermal spray
coating is a versatile and cost-effective solution to extend the service life
of components operating in aggressive environments.
1.2 CHEMICAL VAPOR DEPOSITION (CVD)
Chemical Vapor Deposition (CVD) is a surface coating process
wherein volatile precursor gases react or decompose on a heated substrate
surface to form a solid material. The process typically occurs in a high-
temperature chamber, where one or more volatile compounds (such as
silane, titanium tetrachloride, or methane) are introduced and chemically
react on the substrate’s surface, forming a thin, uniform, and dense film.
CVD is highly valued for its ability to produce high-purity, conformal
coatings with excellent adhesion, making it ideal for semiconductor,
optical, and corrosion-resistant applications.

Figure 1.2. CVD set up

The process is also highly tunable, enabling control over film
thickness, composition, and crystalline structure. There are several variants
of CVD, including low-pressure CVD (LPCVD), plasma-enhanced CVD
(PECVD), and metal-organic CVD (MOCVD), each tailored to specific
application needs. While the advantages of CVD include excellent coating
uniformity and quality, the process demands precise control over
parameters such as temperature, gas flow, and pressure. Additionally, CVD

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systems often involve toxic and corrosive gases, requiring stringent safety
measures and proper waste management. Despite its complexity, CVD
remains indispensable in industries requiring ultra-thin films, such as
microelectronics, photovoltaics, and biomedical devices.
1.3 PHYSICAL VAPOR DEPOSITION (PVD)
Physical Vapor Deposition (PVD) is a vacuum-based coating
process in which solid materials are vaporized and deposited onto a
substrate to form a thin film.

Figure 1.3 PVD set up

Common PVD techniques include sputtering and evaporation. In
sputtering, energetic ions from a plasma collide with a target material,
ejecting atoms that condense on the substrate. In evaporation, the material
is heated until it vaporizes, and the vapor travels in a vacuum to deposit as
a film. PVD produces coatings with excellent hardness, wear resistance,
and adhesion, and is widely used in tooling, decorative finishes, and
electronics. The process allows for precise control of film thickness and
composition, and it can coat substrates at relatively low temperatures,
making it suitable for temperature-sensitive materials. One major
advantage of PVD is its environmental friendliness, as it avoids hazardous

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chemicals. However, the requirement for vacuum equipment increases the
system complexity and cost. PVD coatings are typically thinner than those
produced by thermal spray, but they offer superior mechanical and
tribological properties due to their dense and uniform structure. In
advanced applications, PVD is essential for depositing functional layers in
semiconductors, hard coatings on cutting tools, and anti-reflective or
conductive coatings in optics and solar panels.
1.4. ELECTROPLATING
Electroplating is an electrochemical process used to deposit a thin
layer of metal onto the surface of a conductive substrate. This is achieved
by immersing the substrate (cathode) and a metal anode in an electrolytic
bath containing a metal salt solution.

Figure 1.4 Electroplating process

When electric current is applied, metal ions from the solution are
reduced and deposited onto the surface of the substrate, forming a uniform
coating. Electroplating is widely used for decorative, corrosion-resistant,
and functional applications. Commonly electroplated metals include
nickel, chromium, gold, silver, zinc, and copper. This technique allows for
precise control over the thickness and composition of the deposited layer,
making it suitable for enhancing surface appearance, wear resistance,
electrical conductivity, and corrosion resistance. Electroplating is
commonly employed in industries such as automotive, electronics,

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aerospace, and jewelry. However, challenges include the use of toxic
chemicals, generation of hazardous waste, and the need for stringent
control over operating conditions like temperature, pH, and current density.
Proper surface preparation (such as cleaning and degreasing) is also critical
to achieving good adhesion. Despite its environmental concerns,
electroplating remains a versatile and cost-effective coating method for a
wide range of industrial and consumer products.

1.5. ANODIZING
Anodizing is an electrochemical process that enhances the natural
oxide layer on the surface of metals, primarily aluminum and its alloys.
During anodizing, the metal component is made the anode in an electrolytic
cell and immersed in an acid electrolyte, usually sulfuric, chromic, or
phosphoric acid. When electric current is passed through the cell, oxygen
ions are released from the electrolyte and react with the metal surface,
forming a thicker and more durable oxide layer. This layer is highly
resistant to corrosion, abrasion, and wear, and can also serve as a base for
dyeing or sealing, providing decorative as well as protective finishes.
Anodizing is widely used in architectural, automotive, marine, and
aerospace applications due to its ability to improve surface hardness and
provide long-lasting color finishes without peeling or flaking. The
thickness and properties of the anodized layer can be controlled by
adjusting the process parameters such as current density, time, and
electrolyte composition. One of the significant advantages of anodizing is
that it does not involve the application of foreign materials, making it
environmentally friendly and maintaining the dimensional stability of
components. However, it is generally limited to certain metals like
aluminum, magnesium, and titanium, and does not significantly improve
impact resistance. Despite this, anodizing remains a popular surface

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treatment method for improving both the aesthetics and durability of metal
components.
1.6. LASER CLADDING
Laser cladding is an advanced surface engineering technique used to
deposit a high-performance coating material onto a substrate by melting
the coating material and a thin layer of the substrate using a high-powered
laser beam.

Figure 1.5 Laser Cladding process

The process typically involves feeding a powdered or wire-based
material into the laser-induced melt pool, where it fuses with the substrate
to form a metallurgically bonded coating with minimal dilution. Laser
cladding allows for the application of wear-resistant, corrosion-resistant,
and high-temperature-tolerant materials, such as cobalt-, nickel-, or iron-
based alloys, ceramics, and composites. One of its key advantages is the
ability to precisely control the heat input and cladding depth, resulting in
minimal thermal distortion and high coating quality with excellent bonding
strength. Additionally, the rapid solidification during the process leads to
refined microstructures and enhanced mechanical properties. Laser
cladding is widely used in aerospace, power generation, oil and gas, and

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tooling industries for repair, refurbishment, and performance enhancement
of high-value components. However, the equipment costs are relatively
high, and the process requires a skilled operator and careful control of
parameters such as laser power, scan speed, and powder feed rate. Despite
these challenges, laser cladding stands out for its precision, efficiency, and
ability to deposit custom-tailored coatings with superior functional
performance, making it a preferred choice for critical applications.

1.7 THERMAL BARRIER COATINGS

The application of thermal barrier coatings (TBCs) is a critical
advancement in extending the service life and performance of metallic
substrates operating under extreme environments, especially in aerospace
and power generation sectors. Among the various substrate materials,
Hastelloy X, a nickel-based superalloy known for its exceptional strength,
oxidation resistance, and thermal stability, is widely used in high-
temperature applications such as gas turbine engines, nuclear reactors, and
heat exchangers. However, despite its excellent properties, Hastelloy X
still suffers from thermal degradation, oxidation, and surface wear when
exposed to prolonged high temperatures. To address these issues, advanced
surface engineering techniques have been developed, with double-layered
thermal barrier coating systems gaining considerable attention.
Specifically, a duplex coating comprising an inner bond coat of NiCrAlY
(Nickel-Chromium-Aluminum-Yttrium) and an outer ceramic topcoat of
YSZ (Yttria-Stabilized Zirconia) applied using the plasma spray technique
has shown significant promise. The role of such a double coating is
multifaceted, primarily involving the enhancement of thermal insulation,
oxidation resistance, and overall mechanical integrity of the coated
Hastelloy X substrate under harsh service conditions.

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 Figure 1.6 Schematic representation of coatings
The NiCrAlY bond coat serves as a crucial intermediary between the
metallic substrate and the ceramic topcoat. Its function is not merely
adhesive; it provides a thermally stable and oxidation-resistant interlayer
that accommodates the thermal expansion mismatch between Hastelloy X
and YSZ. NiCrAlY forms a dense, adherent thermally grown oxide (TGO)
layer, primarily composed of alumina (Al₂O₃), upon exposure to high
temperatures. This TGO acts as a diffusion barrier, significantly reducing
the ingress of oxygen to the substrate and thereby delaying oxidation and
hot corrosion. The addition of yttrium in the NiCrAlY alloy improves the
adherence of the alumina scale, reduces spallation, and promotes the
formation of a continuous and slow-growing oxide layer. Furthermore, the
NiCrAlY bond coat effectively alleviates the thermal stresses generated
during heating and cooling cycles due to its ductility and thermal
compatibility with the substrate and topcoat materials.
Over the NiCrAlY bond coat, the YSZ ceramic topcoat serves as the
primary thermal insulator. Yttria-stabilized zirconia, particularly 8 wt%
yttria partially stabilized zirconia (8YSZ), is favored due to its low thermal
conductivity, high melting point, and phase stability at elevated
temperatures. The porous and segmented structure of plasma-sprayed YSZ
coatings contributes to the reduction of heat flux to the underlying
substrate. In addition to providing thermal insulation, the YSZ layer also
acts as a physical barrier to corrosive gases and molten salts that may be

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present in combustion environments. The low thermal conductivity of YSZ
(approximately 1–2 W/m·K) ensures that even when the surface is exposed
to temperatures exceeding 1000°C, the underlying Hastelloy X remains
within its safe operational limits, thus preventing thermal fatigue and
microstructural degradation.
The plasma spray method, particularly atmospheric plasma spraying
(APS), is an established technique for depositing both the NiCrAlY bond
coat and the YSZ topcoat. The high temperature of the plasma jet allows
for efficient melting of the feedstock powders, ensuring strong mechanical
interlocking with the substrate and between coating layers. Plasma
spraying offers the advantage of producing coatings with controlled
porosity, thickness, and microstructure, which are critical parameters
influencing the thermal insulation and durability of the TBC system. In the
case of Hastelloy X, the surface is typically roughened or grit-blasted
before coating to enhance mechanical adhesion. The NiCrAlY bond coat
is deposited first, typically to a thickness of 100–150 µm, followed by the
YSZ topcoat, which can range from 200–500 µm depending on the thermal
protection requirements. The success of the duplex coating depends on
precise control of processing parameters such as plasma energy, spray
distance, feed rate, and substrate preheating, which influence the
microstructure and bonding quality.
One of the critical roles of the double coating system is resistance to
oxidation and hot corrosion, especially in aggressive environments such as
those found in aircraft engines and power plants. While Hastelloy X has
good inherent oxidation resistance, prolonged exposure to high-
temperature gases, especially in the presence of vanadium, sodium, and
sulfur contaminants, can lead to rapid surface degradation. The NiCrAlY
bond coat, through the formation of a slow-growing alumina scale,
significantly mitigates this risk. The ceramic YSZ topcoat further protects

9
the bond coat and the substrate by acting as a barrier against oxygen and
corrosive species. This layered defense mechanism delays the onset of
TGO growth and maintains the structural integrity of the coated component
over extended service durations.
The thermal shock resistance and cyclic durability of the double
coating system are equally important. Thermal cycling can lead to the
development of cracks and delamination at the interface of dissimilar
materials due to differences in their coefficients of thermal expansion
(CTE). The NiCrAlY bond coat plays a pivotal role in relieving such
thermal stresses, thanks to its intermediate CTE and ductility. Additionally,
the segmentation cracks and porosity in the YSZ layer accommodate the
strain and reduce the propagation of stress-induced damage. This
combination results in a coating system that can withstand repeated heating
and cooling cycles without failure, which is crucial for applications
involving fluctuating temperatures and mechanical loads.
From a microstructural standpoint, the NiCrAlY bond coat exhibits
a dense, metallic morphology with a fine distribution of γ and β phases that
contribute to its mechanical stability and oxidation behavior. The addition
of yttrium aids in refining the microstructure and promoting uniform oxide
scale formation. The YSZ topcoat, in contrast, has a columnar or lamellar
structure with microcracks and porosity that enhance strain tolerance and
thermal shock resistance. Cross-sectional micrographs of the coated
Hastelloy X typically reveal a well-adhered, multilayered structure with a
distinct TGO layer formed at the bond coat/topcoat interface after thermal
exposure. The presence of a uniform and adherent TGO layer is indicative
of good coating performance and is often correlated with extended coating
life.
In terms of mechanical performance, the double coating enhances
the hardness, wear resistance, and surface toughness of Hastelloy X.

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Plasma-sprayed NiCrAlY and YSZ coatings are known to increase the
surface hardness due to the ceramic nature of the YSZ and the work-
hardened metallic bond coat. This makes the coated components more
resistant to erosive and abrasive wear, especially in high-speed flow
environments where uncoated Hastelloy X may suffer significant material
loss. Additionally, the coatings reduce the surface roughness and friction
coefficient, which can be beneficial in reducing wear from sliding contacts.
Another significant benefit is the extension of component lifespan
and operational temperature window. With the double coating in place,
Hastelloy X components can be operated at higher surface temperatures
without compromising internal structural integrity. This allows for
improved thermal efficiency in turbines and engines, contributing to fuel
savings and reduced emissions. Moreover, the duplex coating system
enables maintenance intervals to be extended and reduces downtime
associated with part failure, leading to lower overall operational costs.
The evaluation and characterization of the duplex coatings involve
techniques such as scanning electron microscopy (SEM), X-ray diffraction
(XRD), energy-dispersive spectroscopy (EDS), and thermal cycling tests.
These assessments help in understanding the coating microstructure, phase
composition, elemental distribution, and failure mechanisms. For instance,
XRD confirms the presence of tetragonal zirconia phases stabilized by
yttria in the topcoat, while SEM and EDS reveal the uniform distribution
of Cr, Ni, Al, and Y in the bond coat and the integrity of the TGO layer.
Long-term thermal cycling tests simulate real-world service conditions and
provide insights into coating spallation, crack propagation, and interfacial
delamination tendencies.
The double coating of NiCrAlY and YSZ over Hastelloy X via the
plasma spray method plays a vital role in enhancing the thermal,
mechanical, and oxidation performance of the substrate. The NiCrAlY

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bond coat provides an essential oxidation-resistant, stress-relieving layer
that enhances adhesion and protects against high-temperature degradation.
The YSZ topcoat, with its low thermal conductivity and strain-tolerant
structure, offers excellent thermal insulation and corrosion resistance.
Together, they form a synergistic barrier system that significantly extends
the operational life of Hastelloy X components in severe environments.
The plasma spray technique enables precise deposition of these coatings,
ensuring a defect-free and reliable barrier that meets the demands of
modern high-temperature applications. This approach continues to be an
essential strategy in the development of advanced materials for aerospace,
energy, and industrial systems, pushing the boundaries of material
performance and durability in extreme service conditions.

CHAPTER 2
LITERATURE REVIEW

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 Virupakshappa Lakkannavar et al (2021) utilized an air jet erosion
tester to investigate the erosion behavior of NiCrAlY/Cr3C2/h-BN
composite coatings that are plasma-sprayed at three different temperatures
and 40 m/s on T22 boiler steel alloy. 30 and 90◦ are the impingement
angles. To identify the erosion mechanism, SEM and X-ray diffraction
techniques are used to analyze the surface morphology and phase generated
on the eroded surface. Findings of erosion test indicate that the erosion
resistance was notably enhanced by addition of Cr3C2 and h-BN because
of its lubricating characteristics and capacity to reduce frictional forces
during erosion. The combined influence of Cr3C2 and h-BN enhanced the
coating hardness and erosion wear resistance, thereby improving its overall
resistance to erosion. The weight loss method was employed to calculate
the erosion rate, and the NiCrAlY/Cr3C2/h-BN coating showed up to
30.55% and 34.48% lower erosion rate as compared to uncoated T22
substrate at 600 ◦C for 30◦ and 90◦ impact angles, respectively. This
characteristic is affected by the hard reinforcement Cr3C2’s high-
temperature stability, the h-BN’s self-lubricating ability, the formation of
a protective oxide layer that forms at 600 ◦C, and the eroded coating’s
ductile behavior of material removal. The study also reveals that the
NiCrAlY/Cr3C2/h-BN coating system on T22 boiler steel alloy has
excellent erosion resistance, making it suitable for use in high-temperature
and erosive environments in boiler systems and similar industries.
Yongsheng et al (2023) studied the corrosion behavior of hot-dip
galvanized steel in simulated industrial atmospheric environment. The
results were compared with the immersion test to obtain the characteristics
of atmospheric corrosion. Firstly, the micro-morphology of the zinc layer
and corrosion product layer on the surface of hot-dip galvanized steel was
observed by SEM and EDS. Then, the phases of hot-dip galvanized steel
in different corrosion cycles were analyzed by XRD diffraction patterns

13
and FTIR infrared spectroscopy. Finally, electrochemical tests were
conducted to compare the electrochemical parameters of hot-dip
galvanized steel under different corrosion cycles in order to study the
differences in corrosion rates at different corrosion stages. The results
indicate that the main product of salt spray corrosion is ZnO, and it contains
a small amount of Zn5(CO3)2(OH)6 and Zn4(OH)6SO4. The above
corrosion process can be divided into three stages, and the corrosion
mechanism is consistent with the experimental phenomenon. Specifically,
as corrosion develops, the corrosion product layer becomes denser,
improving the corrosion resistance of hot-dip galvanized specimens.
However, the corrosion products on the surface are looser in the immersion
test. When the corrosion time increases, corrosive media is prone to invade
the galvanized layer, resulting in pitting corrosion.
Dan Xin et al (2022) investigated the cyclic hot corrosion behavior
of GH4738 alloy coated with a mixed salt (75 wt% Na2SO4+25 wt%
NaCl) at 750 ◦C and 800 ◦C. X-ray diffractometer (XRD), scanning
electron microscope (SEM), energy dispersive spectrometer (EDS), and
transmission electron microscope (TEM) are used to analyze the phase
compositions and film structures of the corrosion products, as well as to
explore the corrosion mechanism. The results show that a thicker oxide
layer is formed at higher temperatures, indicating poorer hot corrosion
resistance at elevated temperatures. The corrosion products form at both
temperatures to show a distinct layered structure, the outer layer is mainly
composed of Cr2O3 and a small amount of TiO2, while the inner layer
consists of Al2O3, CrS, and TiS. In addition, it is found that the corrosion
mechanism of O, S, and Cl elements in the corrosion process is synergistic
and accompanied by alkaline melting.
Zaiqing et al (2022) studied the corrosion behavior of laser-based
powder bed fused (LPBF) 316 L under various heat-treatment conditions

14
(as-printed, solution annealed and hot isostatic pressed) in lead-bismuth
eutectic (LBE) at 550 ◦C is studied. The wrought 316 L and counterpart
fabricated by powder metallurgy-hot isostatic pressing (PM-HIP) were
investigated as references. LPBF 316 L achieves reduced susceptibility to
the LBE environment and acquires a shallower corrosion/dissolution depth
in comparison to wrought and PM-HIP 316 L. As-printed and hot isostatic
pressed LPBF specimens show restricted discernible phase transformation
while the other conditions exhibit significant phase transformation. The
enhanced corrosion resistance of LPBF 316 L in LBE is attributed to a
dislocation cellular microstructure, a high proportion of low-angle grain
boundaries, and elevated chromium and silicon contents. Dislocation cell
boundaries and twin boundaries have higher resistance to LBE ingress than
the high-angle grain boundaries. Compared to the matrix, the preferential
corrosion by LBE of LPBF materials at columnar boundaries is related to
the carbides and (Si, Mn) enriched oxides formed during LPBF process.
LPBF-HIP material exhibits a three-dimensional alternating structure of
recrystallized and unrecrystallized areas, effectively impeding LBE ingress
and thus can be a promising candidate as the structural material in the LBE
system.
Majid Laleh et al (2020) explored a new mechanistic insights into
the corrosion processes within a pre-painted hot-dip Zn-55Al-2Mg-1.5Si
coated steel exposed to a coastal environment. This study is the first to
conclusively show that corrosion initiation is not only affected by the
electrochemical activities of constituent phases but also by their
morphology. Corrosion initiates when sub-micron Zn particles within the
Zn-Al binary eutectic dissolve. Thereafter, corrosion propagates by the
dissolution of large Zn particles and by Mg dealloying from MgZn2 and
Mg2Si intermetallic phases. The late stages record the corrosion of primary
Al-rich dendrites, leading to a volumetric expansion in corrosion product.

15
 Seyed Reza Siasi Rad et al (2023) investigated the impact of MgO
nanoparticles (0, 0.1, 0.5, and 1 wt%) on the corrosion behavior of hot-
dipped galvalume (Zn-55Al-1.6Si) coating. The corrosion behavior of
coatings was assessed using a salt spray, electrochemical impedance
spectroscopy (EIS), and potentiodynamic polarization tests in air-saturated
3.5 wt% NaCl solution. The surface of the coatings was examined using
field emission scanning electron microscopy (FESEM) and atomic force
microscopy (AFM). The results revealed that MgO nanoparticles were
mainly located in zinc-rich interdendritic areas and filled the micro-holes
within the coating. By creating a protective shield and separating the
coating from the corrosive agents, these nanoparticles enhanced the
corrosion resistance of coatings. Notably, the galvalume coating with the
highest MgO nanoparticle content (1 wt%) exhibited the best corrosion
resistance.
Congjie Kang et al (2022) investigated the hot corrosion behavior
of three types of specimens of TA29 Ti alloy after solution aging treatment
(SAT), low plastic burnishing (LPB) and LPB combined with self-oxygen
diffusion (LPB-OD) at 600 ◦C. The results show that the surface grains of
LPB specimens were refined and produced a large number of dislocations,
stacking faults, grain boundaries and subgrain boundaries. This is
conducive to the diffusion of Al element in the matrix to the surface of the
matrix during the hot corrosion process to form a continuous and dense
Al2O3 protective layer to improve the hot corrosion resistance of the
specimen. The LPB-OD specimen undergoes self-oxygen diffusion
processing to obtain an O rich surface layer and promote the enrichment of
Al element with strong affinity for oxygen towards the surface of the
specimen, resulting in the formation of a special double-layer Al rich oxide
layer during the hot corrosion. This special protective layer further
improves the hot corrosion resistance of LPB-OD specimen. This paper

16
discusses the mechanism of the hot corrosion process of TA29 Ti alloy and
reveals the mechanism of the formation of a special double-layer Al rich
oxide layer under the combined influence of metal element cyclic
chlorination oxidation and surface Al element enrichment caused by self-
oxygen diffusion processing, which provides a new way of thinking to
improve the hot corrosion performance of Ti alloy.
Fereidoon Marefat et al (2022) investigated the arc erosion
resistance behavior of WC/CuCr30 composites prepared by vacuum hot
press sintering and hot extrusion. The microstructure characterization of
WC/CuCr30 composites shows that the Cr particles in the WC/CuCr30
composite have been elongated and the long axis direction is close to
parallel to the extrusion direction after the hot extrusion deformation.
Compared with the longitudinal section, the thermal conductivity of
CuCr30 and WC/CuCr30 composites in the cross section is increases by
3.75% and 3.63%, respectively. The electrical contact testing results under
different voltages shows that the addition of WC particles can extend the
service life of the CuCr30 composite, and the operation times of
WC/CuCr30 composite (4850 times) increases by 34.72% compared to
CuCr30 composite (3600 times) at 30 V DC. The welding force decreases
more obviously with the increase of the voltage, and the average welding
force of WC/CuCr30 composite decreases by 8.57% and 20.9% at 24 V
DC and 30 V DC compared with CuCr30, respectively. The arc erosion
mechanism analysis shows that addition of WC particles is beneficial for
the decrease of arc duration. And WC particles can effectively inhibit the
arc erosion process and delay the formation of bumps and pits.
R. Sasikumar et al (2022) prepared a Al2O3–Cu/35Mo composites
by rapid hot-press sintering-internal oxidation method, by adding trace
amounts of graphene oxide (GO). The results show that the relative
densities of the composites are above 99%, the γ-Al2O3 generated by

17
internal oxidation is diffusely distributed on the copper matrix. The
incorporation of GO produced a small number of hard MoC particles at the
interface, which facilitated the interfacial bonding of the composites. In the
30 V DC, 10–30 A electrical contact test, the anode mass of the composites
increases, while the cathode mass decreases. And GO reduces the total
mass loss of the electric contact by 63.6%, 38.9%, 51.3% and 20.9%,
respectively. A comparison of the electrical contact properties of the two
materials showed that the addition of GO dispersed the concentrated
erosion of the arc. At 10 A and 30 A, the arc energy is reduced by 75.5%
and 12.5%, respectively. With the gradual increase in electric current, GO
makes the Al2O3–Cu/35Mo composites more stable during the electric
contact process, improves the anti-welding ability of the contact and
reduces contact resistance.
C. Dharmendra et al (2020) analyzed the microstructure of spherical
γ' phases and annealing twins obtained by solid solution and aging
treatment in laser powder bed melting forming nickel based superalloy, and
the hot corrosion behavior and hot corrosion mechanism of the alloy
sample in 75wt% Na2SO4 + 25wt% NaCl mixed salt at 750 °C were
studied. The results show that compared with the as-deposited sample, the
sample with γ' phase and annealing twin structure (1190SA) improves the
hot corrosion resistance of the alloy. At the same time, the smaller the γ'
phase and the higher the annealing twin content, the better the hot corrosion
resistance. This is mainly because the γ' phase and annealing twin structure
provide a fast channel for the outward diffusion of Al and Cr elements,
hinder the inward diffusion of S elements, and promote the rapid formation
of three-layer continuity. A dense oxide layer (Cr2O3-TiO-Al2O3), shallow
sulfide layer and matrix zone without corrosion defects such as micropores
constitute a corrosion layer. The dense oxide layer hinders the further
diffusion of corrosive medium elements into the matrix, which

18
significantly affects the hot corrosion resistance of the alloy samples. In
addition, it is also found that the hot corrosion mechanism of S, O and Cl
elements in the hot corrosion process is a synergistic process involving
acid-base melting and internal sulfurization

CHAPTER 3
EXPERIMENTAL WORK

3.1 HASTELLOY X
Hastelloy X is a nickel-based superalloy renowned for its excellent
resistance to high temperatures, oxidation, and corrosion, making it
particularly suitable for extreme environments such as aerospace engines,
gas turbines, and chemical processing industries. Developed primarily for

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high-performance applications, this alloy has become one of the most
dependable materials in environments where both mechanical strength and
corrosion resistance are critical. The nominal chemical composition of
Hastelloy X includes approximately 47% nickel (Ni), 22% chromium (Cr),
18.5% iron (Fe), 9% molybdenum (Mo), with trace amounts of cobalt
(1.5%), manganese (1%), silicon (1%), carbon (0.05–0.15%), and other
elements like aluminum, titanium, and copper in very small quantities. The
synergy between these alloying elements imparts the alloy with a balance
of strength, thermal stability, and corrosion resistance that is difficult to
achieve with conventional stainless steels or simpler nickel alloys.
Nickel, the base element, provides the essential corrosion resistance
and high-temperature strength, while chromium enhances the alloy's
resistance to oxidation and scaling at elevated temperatures. Molybdenum
contributes significantly to the material's resistance to localized forms of
corrosion, such as pitting and crevice corrosion, especially in reducing
environments. Iron acts as a stabilizer in the matrix, improving the overall
mechanical behavior, while cobalt aids in strengthening and contributes to
phase stability at high temperatures. The controlled addition of carbon
enhances creep resistance by promoting the formation of carbides, which
can help maintain structural integrity during prolonged exposure to stress
and heat. Silicon and manganese are primarily included to improve the
alloy's workability and deoxidation during melting and fabrication.
The mechanical properties of Hastelloy X are exceptional at both
room and elevated temperatures. It possesses a high tensile strength,
typically around 770 MPa (112 ksi), and a yield strength of about 360 MPa
(52 ksi) at room temperature. More importantly, these mechanical
properties are well-retained up to temperatures nearing 1200°C (2190°F),
a key requirement for aerospace and industrial heat-treating applications.
The alloy has good fatigue resistance and stress-rupture properties,

20
enabling it to withstand cyclic loading and long-term exposure to high-
temperature stresses. Its creep resistance, particularly at temperatures
between 800–1100°C, is one of its defining strengths. Additionally,
Hastelloy X exhibits good ductility and toughness, even after extended
service in high-temperature environments, which makes it easier to
fabricate and weld compared to some other high-strength alloys.
Corrosion resistance is another hallmark of Hastelloy X, especially
in oxidizing and moderately reducing atmospheres. The presence of
chromium and molybdenum makes it particularly effective in resisting
high-temperature oxidation, carburization, and sulfidation. Unlike many
other alloys that form unstable oxides or carbides at high temperatures,
Hastelloy X maintains a stable oxide layer that protects its surface from
further degradation. It also resists corrosion in high-purity water and
various acid environments, though it is not as resistant to strongly reducing
acids like hydrochloric acid as other members of the Hastelloy family, such
as Hastelloy C-276. Nevertheless, its corrosion resistance remains
sufficient for a broad range of industrial applications, particularly those
involving hot gases and chemically aggressive atmospheres.
Fabrication and welding characteristics of Hastelloy X are generally
good, making it a practical choice for engineering components. It can be
forged, hot worked, and cold worked using conventional methods. The
alloy is amenable to machining, although its work-hardening
characteristics necessitate the use of appropriate tooling and cutting
techniques to ensure dimensional accuracy and surface integrity. Welding
can be performed using standard processes such as gas tungsten arc
welding (GTAW), gas metal arc welding (GMAW), and shielded metal arc
welding (SMAW), with minimal risk of cracking or embrittlement. Post-
weld heat treatment is often not necessary, though it may be used in some
critical aerospace applications to restore optimal microstructure and stress

21
relief. Hastelloy X does tend to develop grain growth when exposed to very
high temperatures for long durations, but this can be controlled through
proper heat treatment schedules and alloy processing techniques.
Hastelloy X finds extensive application in industries that demand
materials capable of enduring high stress, high temperature, and corrosive
atmospheres. In the aerospace sector, it is widely used for components such
as combustion chambers, afterburners, transition ducts, and tailpipes in jet
engines due to its outstanding thermal and mechanical stability. The alloy’s
resistance to oxidation and creep makes it suitable for use in hot zones of
engines, where few other materials can perform reliably over extended
periods. It is also employed in land-based gas turbines, both in power
generation and mechanical drive systems, for parts like turbine shrouds,
combustor liners, and sealing rings. In the chemical and petrochemical
industries, Hastelloy X is utilized in reactor vessels, furnace parts, and heat
exchangers that are exposed to aggressive environments including flue
gases, high-purity steam, and various chlorinated solvents. The alloy's
performance in vacuum furnaces, where both high temperature and clean
atmospheres are required, has made it a standard material for furnace
internals such as heating elements, retorts, and shielding.
In nuclear reactor systems, Hastelloy X is occasionally used due to
its radiation resistance and ability to withstand high-pressure, high-
temperature water and steam. It is also employed in some marine and
offshore applications, where resistance to saltwater corrosion and high
pressure is required, though in these cases, cost and over-specification
sometimes limit its use. Moreover, Hastelloy X has gained interest in the
development of environmental systems such as waste incinerators, fuel
reformers, and heat recovery systems, where it resists the combined effects
of thermal cycling, oxidizing agents, and corrosive residues.

22
 Despite its numerous advantages, the alloy does have some
limitations. The high cost of raw materials, particularly nickel and
molybdenum, makes Hastelloy X an expensive material, often restricting
its use to applications where no other alternative can provide the same level
of performance. Additionally, while its corrosion resistance is generally
good, it is not suitable for highly reducing acids or for exposure to
environments where intergranular corrosion may occur after prolonged
exposure to certain temperature ranges unless properly processed and
stabilized.
Hastelloy X is a high-performance nickel-based superalloy with a
well-balanced composition that imparts excellent strength, oxidation
resistance, and corrosion resistance at elevated temperatures. Its properties
make it ideal for demanding applications in aerospace, chemical
processing, and high-temperature industrial systems. With proven
weldability, thermal stability, and mechanical integrity, Hastelloy X
continues to be a material of choice in environments where reliability and
longevity are critical. As new technologies push the limits of temperature
and corrosion exposure, alloys like Hastelloy X will remain at the forefront
of materials engineering, supporting innovation in power generation,
propulsion, and advanced manufacturing systems.
3.2 NiCrAlY BOND COAT
NiCrAlY is a widely used metallic bond coat material in thermal
barrier coating (TBC) systems designed to enhance the performance and
lifespan of components operating in high-temperature and corrosive
environments, such as those found in aerospace, gas turbines, and
industrial furnaces. The name NiCrAlY stands for the main constituents of
the alloy—Nickel (Ni), Chromium (Cr), Aluminum (Al), and Yttrium (Y).
This alloy typically consists of 60–70 wt.% Ni, 15–25 wt.% Cr, 5–10 wt.%
Al, and a small addition (0.1–0.8 wt.%) of yttrium. The careful balance of

23
these elements imparts the alloy with superior oxidation and corrosion
resistance, good mechanical integrity, and compatibility with ceramic
topcoats such as Yttria-Stabilized Zirconia (YSZ) used in TBC systems.
Nickel serves as the matrix element, providing high-temperature
strength and structural stability. Chromium enhances the resistance to high-
temperature oxidation and sulfidation by forming a protective chromium
oxide (Cr₂O₃) layer. Aluminum contributes significantly to the formation
of a stable and slow-growing alumina (Al₂O₃) scale, which acts as a
diffusion barrier, preventing rapid degradation of both the bond coat and
the substrate. The addition of yttrium plays a crucial role in improving the
adhesion and longevity of the oxide scale through what is known as the
“reactive element effect.” Yttrium enhances the adherence of the alumina
scale to the underlying metal by reducing scale spallation and increasing
oxide adherence during thermal cycling.
NiCrAlY coatings serve as an intermediate bond coat between a
metallic substrate—such as Hastelloy—and the ceramic topcoat in a
multilayer thermal barrier system. The bond coat accommodates the
thermal expansion mismatch between the metal substrate and the ceramic
layer, thereby minimizing the stresses induced by temperature fluctuations.
Additionally, the formation of a continuous and adherent alumina layer on
the surface of the NiCrAlY during high-temperature exposure acts as a
protective diffusion barrier and provides an ideal surface for anchoring the
ceramic topcoat. These attributes make NiCrAlY a standard choice in
thermal spray applications for turbine blades, combustor parts, and exhaust
components exposed to extreme conditions.
Overall, the NiCrAlY bond coat is critical for enhancing the
performance and durability of high-temperature structural components. Its
ability to provide both chemical and mechanical compatibility in layered
coating systems makes it indispensable in modern surface engineering

24
solutions. When applied over high-performance superalloys like Hastelloy
using techniques such as atmospheric plasma spraying (APS), the resulting
system exhibits outstanding thermal, mechanical, and oxidative stability,
ensuring long-term service even under the most aggressive operating
environments.

Figure 3.1 Powder morphology of NiCrAlY

The scanning electron microscopy (SEM) characterization of
NiCrAlY powder prior to plasma spray coating reveals crucial insights into
its morphology, particle size distribution, and suitability for thermal spray
processes. The SEM image illustrates that the NiCrAlY particles exhibit
predominantly spherical morphology, which is characteristic of gas-
atomized powders. This spherical shape is essential as it ensures good
flowability and uniform feeding during the plasma spraying process. The
particle sizes appear to be relatively uniform, with diameters ranging from
approximately 20 µm to over 100 µm, as indicated by the scale bar of 150
µm. The uniform size distribution and smooth surface texture of the
particles promote consistent melting and deposition during the coating
process, thereby enhancing coating uniformity and adhesion. Occasional
satellites and slightly irregular particles are observed, which may result

25
from incomplete atomization or particle agglomeration during the powder
production process.
However, their presence is minimal and unlikely to significantly
hinder spray performance. The NiCrAlY composition, comprising nickel
(Ni), chromium (Cr), aluminum (Al), and yttrium (Y), is well known for
its excellent high-temperature oxidation and corrosion resistance. These
properties, combined with the powder’s favorable morphology, make it
highly suitable for use as a bond coat or top coat in thermal barrier systems
for aerospace and turbine components. Furthermore, the dense and crack-
free surfaces of the particles suggest that the powder has undergone proper
manufacturing and handling, minimizing the likelihood of porosity or
structural defects in the final coating. Overall, the SEM analysis confirms
that the NiCrAlY powder possesses the necessary physical and
morphological characteristics required for efficient plasma spraying. These
characteristics are critical to achieving a high-quality, adherent, and
durable coating capable of performing under demanding thermal and
oxidative environments.

3.3 NiCrAlY BOND COATING VIA PLASMA SPRAY METHOD

The fabrication of NiCrAlY bond coatings over Hastelloy substrates
via the plasma spray method is a complex but well-established thermal
spray process designed to enhance the high-temperature oxidation
resistance and provide a reliable foundation for further ceramic coating
layers. The procedure involves several critical stages, including substrate
preparation, powder selection, plasma spray parameter optimization,
coating deposition, and post-spray treatment, each of which significantly
affects the performance of the final coated system. The overall goal of the
procedure is to produce a dense, well-adhered, and oxide-free NiCrAlY

26
layer that provides excellent bonding and thermal cycling resistance
between the Hastelloy base and any overlying ceramic coatings.
3.3.1 Substrate Preparation
The first step in the plasma spray process involves meticulous
preparation of the Hastelloy substrate to ensure proper adhesion of the
NiCrAlY bond coat. This involves degreasing the surface using solvents
like acetone or ethanol to remove any oils, dirt, or surface contaminants.
After degreasing, mechanical roughening is performed, typically via grit
blasting using alumina particles (usually between 24–60 mesh) at a
pressure of around 4–6 bar. Grit blasting not only removes surface oxides
and scales but also creates a rough, anchor-like surface topography that
enhances mechanical interlocking between the coating and the substrate.
The roughness (Ra) is typically maintained between 3–6 µm for optimal
bonding.
3.3.2. NiCrAlY Powder Selection
The success of the coating also heavily depends on the choice of
spray powder. Commercially available gas-atomized NiCrAlY powders
are preferred due to their spherical morphology and narrow particle size
distribution, which promote better flowability and deposition efficiency
during spraying. Typical powder particle sizes range from 15–45 µm, and
the composition is tightly controlled to fall within the desired NiCrAlY
range (e.g., Ni-22Cr-10Al-1Y wt.%). Powders must be dry, free from
agglomerates, and stored in moisture-proof containers to prevent oxidation
before spraying.
3.3.3 Plasma Spray System Setup
Atmospheric plasma spraying (APS) is the most commonly
employed method for applying NiCrAlY coatings. The plasma spray
system consists of a DC arc plasma torch, powder feeder, gas control
system, and robotic arm for torch movement.

27
 Figure 3.2 Plasma spray setup
Argon is typically used as the primary plasma gas, with hydrogen or helium
as a secondary gas to adjust the enthalpy of the plasma jet. Standard
spraying parameters include plasma power levels ranging between 30–50
kW, gas flow rates (e.g., Ar: 40 L/min, H₂: 10 L/min), and spray distances
of 80–120 mm. These values are optimized based on the spray equipment
and desired coating characteristics.
3.3.4. Coating Deposition
During spraying, the NiCrAlY powder is fed into the high-velocity,
high-temperature plasma jet where the particles are heated to a semi-
molten or molten state and propelled towards the substrate. The robot-
controlled torch traverses across the substrate surface in a raster pattern to
build up the coating layer by layer. Multiple passes are typically required
to achieve the desired coating thickness, which usually ranges from 100
µm to 300 µm. Parameters such as torch speed, powder feed rate (10–30
g/min), standoff distance, and substrate cooling (e.g., air or water cooling)
are closely monitored to prevent overheating, oxidation, or defects like
unmelted particles or porosity. Maintaining a controlled atmosphere

28
around the spraying area, sometimes using inert shrouds or enclosures,
helps minimize in-flight oxidation of the coating particles.
3.4 FABRICATION OF YSZ COATING VIA PLASMA SPRAY
METHOD

Figure 3.3 Powder morphology of YSZ

The scanning electron microscopy (SEM) characterization of Yttria-
Stabilized Zirconia (YSZ) powder reveals critical details about its
morphology and surface texture, which are essential for evaluating its
suitability in thermal spray coating applications. The SEM image shows
that the YSZ particles are predominantly spherical in shape, a typical
feature of powders produced by spray drying or agglomeration and
sintering processes. The spherical morphology enhances the flowability
and packing density of the powder, which are key parameters for achieving
a consistent and dense coating during plasma spraying. The particle size
appears to be in a relatively uniform distribution, ranging approximately
from 10 µm to over 100 µm, as inferred from the 150 µm scale bar. Such
size uniformity promotes homogeneous melting and deposition during the
spraying process, thereby ensuring a consistent coating thickness and
microstructure. The surface of the particles exhibits a rough or textured

29
appearance, which could be attributed to sintered agglomerates or the
intrinsic crystalline nature of YSZ. This rough texture can enhance
mechanical interlocking during coating, improving the adhesion strength
of the deposited layer.
YSZ is widely recognized for its excellent thermal stability, low
thermal conductivity, and high resistance to thermal shock, making it an
ideal top coat material in thermal barrier coating (TBC) systems used in
gas turbines and aero-engine components. The SEM micrograph confirms
the high purity and integrity of the powder, as there are no visible
contaminants, cracks, or hollow particles. These characteristics are crucial
to preventing porosity and delamination in the final coating. Moreover, the
observed morphology suggests that the YSZ powder will demonstrate
favorable deposition efficiency and coating quality under plasma spraying
conditions. In conclusion, the SEM analysis affirms that the YSZ powder
possesses the optimal morphological features necessary for high-
performance thermal barrier coatings.
The fabrication of Yttria-Stabilized Zirconia (YSZ) coating over
Hastelloy X alloy, pre-coated with a NiCrAlY bond coat, using the plasma
spray method is a sophisticated and multi-step thermal spray process aimed
at developing advanced thermal barrier coating (TBC) systems for high-
temperature applications such as gas turbines, aerospace propulsion
components, and industrial power generation equipment. YSZ, typically
consisting of 7–8 wt.% yttria-stabilized zirconia, is chosen for its
exceptionally low thermal conductivity, high melting point (~2700°C), and
outstanding thermal shock resistance, making it the most widely used
ceramic topcoat in modern TBC systems. The process begins with the
proper preparation of the substrate and bond-coated surface, followed by
selection and preparation of high-quality YSZ powder, optimization of
atmospheric plasma spraying (APS) parameters, careful layer-by-layer

30
deposition of the ceramic topcoat, and finally, rigorous inspection and
testing to ensure performance consistency.
The first critical step involves substrate preparation. After the
NiCrAlY bond coat has been deposited onto the Hastelloy X substrate via
plasma spraying and subsequently heat-treated to develop a uniform
thermally grown oxide (TGO) layer, typically composed of dense α-Al₂O₃,
it is imperative to ensure that the bond coat surface is clean, oxide-free
(except for the intended TGO), and exhibits the right level of surface
roughness to support mechanical interlocking with the YSZ topcoat. A
surface roughness (Ra) between 5–8 µm is ideal for YSZ adhesion. Any
contamination, such as dust, oil, or loose oxide particles, is removed
through mild grit blasting using fine alumina particles or ultrasonic
cleaning in acetone or ethanol. This cleaning ensures the effective
anchoring of the ceramic particles during the spray process.
Once the substrate and bond coat are adequately prepared, the next
phase is the selection and handling of YSZ feedstock powder. High-purity
7–8 wt.% yttria-partially-stabilized zirconia (7YSZ or 8YSZ) powders are
preferred due to their excellent phase stability, thermal insulation
properties, and compatibility with NiCrAlY bond coats. These powders are
typically produced via spray drying and sintering or agglomerated and
sintered processes, resulting in spherical, free-flowing particles with a
uniform size distribution, usually in the range of 10–45 µm. The spherical
morphology enhances feeding consistency and deposition efficiency
during plasma spraying. It is crucial that the YSZ powder is kept dry and
handled in a humidity-controlled environment to prevent agglomeration
and preserve flowability.
The atmospheric plasma spray (APS) system setup is then calibrated
for YSZ deposition. The plasma torch typically uses argon as the primary
plasma gas, with hydrogen or helium as secondary gases to achieve the

31
desired energy and heat transfer characteristics. Commonly, the plasma
torch operates at power levels ranging from 35–50 kW, with gas flow rates
such as Ar: 40–50 L/min and H₂ or He: 8–15 L/min. The powder is
introduced axially into the plasma jet via a carrier gas like argon at a feed
rate of 10–30 g/min. The spray distance—defined as the standoff distance
between the torch nozzle and the substrate—is typically maintained
between 80–120 mm. These parameters are finely tuned to ensure partial
or complete melting of YSZ particles so they can deform into splats upon
impact and solidify rapidly to form a cohesive and dense ceramic layer.
During the actual deposition, the plasma torch is robotically
manipulated over the surface of the NiCrAlY bond-coated Hastelloy X in
a raster or zig-zag pattern to uniformly deposit successive thin layers of
YSZ. This layer-by-layer accumulation results in a total coating thickness
typically ranging from 200 µm to 500 µm depending on the application.
The deposition rate is carefully controlled to prevent excessive heating of
the substrate and to avoid defects such as vertical cracking, delamination,
or excessive porosity. The substrate is often rotated or linearly moved using
a turntable or XYZ motion system to maintain even coating thickness and
torch coverage. Active substrate cooling using compressed air or water-
cooled fixtures is sometimes employed to manage temperature gradients
and avoid stress accumulation. A critical feature of YSZ coatings is the
formation of a columnar or lamellar microstructure, which enhances strain
tolerance and provides the required compliance to accommodate thermal
expansion mismatches during high-temperature service.
In-flight particle diagnostics, such as the use of sensors to monitor
particle velocity and temperature, are often integrated into advanced APS
systems. The ideal in-flight particle temperature for YSZ spraying is
around 2500–3000°C, and the velocity is approximately 200–300 m/s.
These metrics ensure optimal particle melting, splat flattening, and

32
adhesion. Deposition efficiency and coating quality are strongly influenced
by these parameters, and deviations can result in non-uniform coatings,
poor bonding, or premature failure during thermal cycling.
Upon completion of the YSZ topcoat deposition, post-deposition
evaluation and optional thermal treatment steps are carried out. Unlike
bond coats, ceramic topcoats like YSZ are not typically subjected to post-
spray annealing; however, in some cases, thermal exposure in a furnace at
1100–1200°C for a few hours may be applied to relieve residual stresses
and promote partial sintering, which improves mechanical cohesion and
reduces initial porosity. The coated component is then subjected to detailed
characterization and quality control tests. These include microstructural
analysis using scanning electron microscopy (SEM) to observe lamellar
structure, porosity levels (targeting 10–15%), and interface quality
between layers. X-ray diffraction (XRD) is used to confirm the presence of
the desired tetragonal phase of YSZ, which is stabilized by yttria and is
responsible for the coating’s excellent thermal stability.
Adhesion strength tests, such as the ASTM C633 pull-off test, help
quantify the bond strength between the YSZ topcoat and the NiCrAlY bond
coat. Acceptable bond strength values are typically above 15 MPa for
plasma-sprayed ceramic coatings. Porosity is another key metric that is
optimized to achieve a balance between thermal insulation and mechanical
strength. Higher porosity enhances thermal insulation but can compromise
mechanical durability; thus, the porosity is kept within 10–20% based on
application requirements. Thermal cycling and burner rig tests are also
performed to simulate real-world conditions and assess the coating's
resistance to spallation, delamination, and thermal fatigue.
The final coated component, now comprising the Hastelloy X
substrate, a dense and oxidation-resistant NiCrAlY bond coat, and a
thermally insulating YSZ topcoat, is ready for deployment in high-

33
temperature applications. In jet engine turbines, for instance, these
multilayer coatings significantly improve component life by reducing the
temperature of the underlying metal substrate by up to 150–200°C, thus
allowing higher combustion temperatures for improved engine efficiency.
In power plants, they help reduce oxidation, corrosion, and creep,
extending the operational life of critical components.
The fabrication of YSZ coatings over Hastelloy X with an
underlying NiCrAlY bond coat via the atmospheric plasma spray method
is a well-engineered and precise thermal spray process designed to deliver
high-performance thermal barrier systems. Each stage of the process—
from surface preparation and powder selection to deposition control and
post-spray testing—plays a critical role in defining the coating's structural
integrity, adhesion, and thermal resistance. The resulting multilayered
system offers superior protection for superalloy components operating
under extreme thermal and mechanical stresses, ensuring long-term
performance, efficiency, and reliability in demanding industrial
environments.
3.5 HOT OXIDATION TEST
The oxidation test is a critical evaluation method used to assess the
high-temperature oxidation resistance of plasma-sprayed NiCrAlY and
YSZ coatings over Hastelloy X. In this context, the test simulates
prolonged exposure of the coated alloy to oxidizing environments at
elevated temperatures, typically ranging from 900°C to 1100°C, to mimic
actual service conditions encountered in gas turbines and power plants. The
main goal is to determine the coating's ability to prevent or delay oxygen
diffusion to the substrate, thereby reducing oxide scale formation and
minimizing material degradation. The double-layered coating system—
comprising a metallic bond coat of NiCrAlY and a ceramic topcoat of
YSZ—offers synergistic protection. During the oxidation test, the samples

34
are typically placed in a muffle furnace for isothermal or cyclic oxidation
studies. In isothermal testing, samples are continuously held at a set
temperature for a fixed duration, while in cyclic testing, they are repeatedly
heated and cooled to simulate real operational fluctuations. The mass gain
of the samples is recorded at regular intervals using a high-precision
balance, as the formation of oxides on the surface correlates with weight
change.
The effectiveness of the NiCrAlY bond coat in oxidation resistance
stems from its ability to form a stable and adherent alumina (Al₂O₃)
thermally grown oxide (TGO) layer upon exposure to high temperatures.
This TGO acts as a diffusion barrier against further oxygen penetration,
thus protecting both the bond coat and the underlying substrate. The
inclusion of yttrium in the bond coat composition enhances the adherence
and continuity of the alumina scale, reducing the chances of spallation and
crack initiation. On the other hand, the YSZ topcoat provides an insulating
barrier that minimizes the thermal gradient and protects the bond coat from
direct exposure to hot gases, further limiting oxidation rates. Scanning
Electron Microscopy (SEM) and Energy Dispersive Spectroscopy (EDS)
of the oxidized cross-sections reveal the formation of a uniform and dense
TGO layer between the NiCrAlY and YSZ interfaces. Cracking,
delamination, or excessive TGO growth are indicators of poor oxidation
performance, whereas a thin, adherent TGO is desirable.
Results from oxidation tests typically show that the duplex-coated
samples exhibit significantly lower mass gains compared to uncoated or
single-layer coated Hastelloy X. This demonstrates the superior oxidation
resistance conferred by the synergistic action of the NiCrAlY and YSZ
layers. The coating system also resists microstructural degradation such as
grain boundary oxidation, pore formation, and matrix weakening, which
commonly affect unprotected superalloys. Moreover, the duplex structure

35
remains intact over extended durations of oxidation, reflecting excellent
adhesion and thermal stability. These results confirm that the plasma-
sprayed NiCrAlY and YSZ coatings effectively enhance the high-
temperature oxidation resistance of Hastelloy X, making them suitable for
components operating in aggressive oxidative environments.

3.6 HOT CORROSION TEST

Hot corrosion testing is essential for evaluating the resistance of
plasma-sprayed NiCrAlY and YSZ coatings over Hastelloy X to
aggressive environments containing molten salts such as sodium sulfate
(Na₂SO₄) and vanadium pentoxide (V₂O₅), which are typically present in
marine, combustion, and industrial environments.

Figure 3.4 Hot Corrosion test

Unlike simple oxidation, hot corrosion involves complex
electrochemical reactions and the formation of molten salt phases that
aggressively attack the surface, penetrate through coatings, and cause
accelerated degradation of both the coating and the substrate. In a standard
hot corrosion test, the surface of the coated sample is coated with a salt
mixture (usually 75% Na₂SO₄ + 25% V₂O₅ by weight) and subjected to
high temperatures (typically 850°C to 950°C) in a furnace under cyclic or

36
continuous heating conditions for a fixed number of hours. The corrosive
salt mixture melts and reacts with the coating materials, and the extent of
damage is assessed through weight change measurements, surface
morphology analysis, and microstructural examination.
The NiCrAlY bond coat plays a crucial role in resisting hot corrosion
through the formation of a stable alumina scale, which blocks the
penetration of aggressive species. Chromium in the bond coat also
contributes to corrosion resistance by forming protective chromium oxide
layers. However, these oxide layers can be vulnerable in molten salt
environments due to the fluxing action of vanadium or sulfur compounds,
which can dissolve protective scales. Here, the outer YSZ topcoat provides
an additional layer of defense by acting as a thermal and chemical barrier,
thereby delaying the interaction of corrosive salts with the underlying bond
coat. The YSZ layer’s porosity and microcracks—commonly introduced
during plasma spraying—can sometimes act as diffusion paths for molten
salts, but when optimized, these features also enhance strain tolerance and
delay catastrophic failure. The combination of these two layers ensures that
even if the topcoat is partially penetrated, the bond coat maintains its
protective function.
Following the test, detailed analysis using SEM, EDS, and X-ray
diffraction (XRD) typically reveals that coated samples experience
significantly less surface spallation, crack propagation, and corrosion
product formation compared to uncoated samples. The bond coat shows
limited sulfidation and vanadate attack, and the TGO layer remains largely
stable and adherent. The mass gain rate remains low, indicating minimal
material consumption due to corrosion. In contrast, uncoated Hastelloy X
or samples without the ceramic topcoat show extensive surface
degradation, pitting, and spallation of oxide scales due to the aggressive
chemical attack. The double coating also improves the structural integrity

37
and adhesion under thermal cycling, which is crucial for hot corrosion
resistance under real-world fluctuating thermal conditions.
Overall, the hot corrosion test results validate the superior protective
capabilities of the NiCrAlY and YSZ double coating system on Hastelloy
X. The synergistic effect of a chemically resistant, alumina-forming bond
coat and a thermally stable, corrosion-inert ceramic topcoat effectively
suppresses the infiltration and chemical attack by molten salts. This makes
the duplex coating highly suitable for components in marine turbines, coal-
fired boilers, and other high-temperature systems where hot corrosion is a
major concern.

CHAPTER 4
RESULTS AND DISCUSSION

4.1 SEM CHARACTERIZATION OF COATINGS

38
 Figure 4.1 Cross sectional characterization of coatings via SEM
The scanning electron microscopy (SEM) characterization of the
thermally sprayed coating system comprising a Hastelloy X substrate, a
NiCrAlY bond coat, and a Yttria-Stabilized Zirconia (YSZ) top coat
reveals essential insights into the coating architecture, layer integrity, and
interfacial bonding quality, which are critical parameters influencing the
thermal and mechanical performance of thermal barrier coatings (TBCs).
The SEM cross-sectional image clearly delineates the three distinct
regions: the dense and uniform substrate at the bottom, the relatively
homogeneous bond coat in the middle, and the porous YSZ top coat on the
surface. This typical TBC architecture is designed to enhance the thermal
protection of components operating in extreme environments such as
turbine engines, aerospace combustors, and high-temperature reactors.
The substrate, Hastelloy X, is a nickel-based superalloy renowned
for its exceptional high-temperature strength, corrosion resistance, and
oxidation resistance. The SEM micrograph indicates a compact and flaw-
free microstructure, which is essential for supporting the overlying coating

39
system and enduring the mechanical and thermal loads encountered in
service. No visible cracks, pores, or delamination are observed within the
substrate, confirming its structural integrity and suitability as a base
material for TBC application.
Immediately above the substrate lies the bond coat layer, composed
of NiCrAlY. This metallic interlayer plays a crucial role in enhancing
adhesion between the ceramic top coat and the metallic substrate while also
serving as a diffusion barrier and oxidation-resistant layer. The bond coat
appears dense and relatively defect-free in the SEM image, with a uniform
thickness across the cross-section. The good metallurgical bonding
between the bond coat and the substrate indicates that the plasma spraying
parameters were optimized to promote adequate interfacial cohesion. The
smooth transition from the substrate to the bond coat also suggests minimal
thermal or residual stress concentrations, which can otherwise lead to
premature coating failure under cyclic thermal loading.
The NiCrAlY bond coat facilitates the formation of a thermally
grown oxide (TGO) layer, primarily consisting of alumina (Al₂O₃), at the
interface between the bond coat and the YSZ top coat during high-
temperature exposure. Although the TGO layer is not directly visible in the
SEM image, its presence is implicitly supported by the clear separation
between the bond coat and the top coat. The growth and stability of the
TGO layer are pivotal in determining the coating system's longevity, as
excessive growth can induce stress buildup and spallation.
The YSZ top coat, deposited via atmospheric plasma spraying
(APS), exhibits a highly porous, lamellar microstructure characteristic of
ceramic coatings formed by this technique. The porosity observed in the
YSZ layer, including microcracks and inter-splat boundaries, is
advantageous as it contributes to the low thermal conductivity of the
coating, thereby enhancing thermal insulation. Additionally, this

40
microstructural feature improves strain tolerance by allowing the coating
to accommodate thermal expansion mismatches between the underlying
metal and the ceramic layer. The thickness of the YSZ top coat appears
sufficient to provide substantial thermal protection, and its uniformity
across the section indicates proper deposition control.
Despite its advantages, the porous nature of the YSZ top coat also
poses challenges in terms of mechanical strength and erosion resistance.
The SEM image does not show any signs of delamination or interfacial
cracking, suggesting that the coating was applied under well-controlled
process parameters, ensuring adequate adhesion. Furthermore, the rough
interface between the YSZ and bond coat may contribute positively to
mechanical interlocking, reinforcing the bond between the layers.
The overall coating system, as revealed by SEM, highlights the
success of the layered TBC architecture in providing a functional barrier
against heat and oxidation while maintaining structural cohesion under
service-like conditions. The integrity of the interfaces between the YSZ top
coat, the NiCrAlY bond coat, and the Hastelloy X substrate is critical in
ensuring thermal shock resistance, resistance to spallation, and extended
service life. No microstructural defects such as delamination, voids at the
interfaces, or severe cracks were visible in the cross-sectional image,
attesting to the quality of the coating process and the compatibility of the
materials used.
The SEM characterization also underscores the role of each
constituent in this TBC system. Hastelloy X, with its excellent high-
temperature mechanical properties, forms a stable and robust base. The
NiCrAlY bond coat, due to its oxidation resistance and alumina-forming
ability, effectively mitigates interdiffusion and supports the growth of a
stable TGO, while also enhancing the adhesion of the top ceramic coat.
The YSZ top coat, stabilized typically with 7-8 wt% Y₂O₃, offers high

41
thermal resistance and accommodates thermal strains through its
engineered porosity and splat morphology.
Moreover, the image provides a basis for further advanced
microstructural analysis, such as elemental mapping via energy-dispersive
X-ray spectroscopy (EDS), phase analysis via X-ray diffraction (XRD),
and mechanical evaluations such as hardness and adhesion strength testing.
These additional characterizations, in conjunction with SEM, offer
comprehensive insights into the performance of the TBC system.
In summary, the SEM cross-sectional analysis of the Hastelloy
X/NiCrAlY/YSZ coating system confirms the successful implementation
of a thermally sprayed thermal barrier coating with excellent structural
integrity, optimal layer adhesion, and a favorable microstructure. The
ceramic YSZ top coat, with its porous and crack-tolerant morphology, the
dense and oxidation-resistant NiCrAlY bond coat, and the robust Hastelloy
X substrate together form a well-engineered thermal protection system
capable of withstanding extreme thermal and oxidative conditions
encountered in advanced gas turbine engines and aerospace applications.

4.2 SEM CHARACTERIZATION OF YSZ COATING

The scanning electron microscopy (SEM) images of nanostructured
yttria-stabilized zirconia (YSZ) coatings provide significant insights into
the surface morphology and grain characteristics of the coating material at
the nanoscale.

42
 Figure 4.2 SEM characterization of YSZ coating

The two SEM micrographs, captured at different magnifications

(with scale bars of 500 nm and 200 nm, respectively), clearly depict the
fine, granular surface texture and the agglomerated morphology of YSZ
nanoparticles. This nanostructured surface morphology is indicative of a
high surface area and is essential for enhancing the thermal and mechanical
performance of thermal barrier coatings (TBCs).
The left image, at a lower magnification, shows that the YSZ coating
is composed of densely packed, uniformly distributed nano-grains. These
grains appear spheroidal to polyhedral in shape, with minimal porosity or
intergranular gaps. Such morphology implies that the coating possesses a
compact microstructure, which is critical for maintaining structural
stability under thermal stress. The reduced grain size increases grain
boundary density, which can influence properties such as thermal
conductivity and mechanical strength. Smaller grains contribute to lower
thermal conductivity due to enhanced phonon scattering at grain

43
boundaries, which is desirable for TBC applications where thermal
insulation is required.
The right image, at higher magnification, reveals more detailed
features of the YSZ nanostructure. The grains exhibit a highly faceted
surface and a degree of interconnectivity that suggests partial sintering
during the coating deposition. The surface roughness and irregular grain
shapes contribute to improved mechanical interlocking when applied over
a bond coat or substrate. Moreover, the presence of nano-pores or
interstitial voids between grains can provide strain tolerance during
thermal cycling, which is a critical feature for preventing spallation in TBC
systems.
The nanostructured nature of the YSZ coatings as seen in the SEM
images reflects the effectiveness of the chosen deposition method, likely a
variant of plasma spraying or sol-gel processing tailored for nanomaterials.
The retained nano-features after deposition indicate that the thermal input
during the coating process was well-controlled, preventing excessive grain
growth and preserving the intended nanostructure. This is crucial because
the high-temperature stability of nanostructured YSZ directly influences
the coating's long-term performance in service conditions, such as those in
aerospace or power generation turbines.
Furthermore, the SEM analysis confirms the high surface-to-volume
ratio and homogeneous distribution of grains, which not only improves the
thermal insulation but also enhances the coating’s resistance to erosion and
cracking. The fine grains contribute to a higher hardness, while the
presence of intergranular spaces facilitates accommodation of thermal
strains, thereby improving the coating’s toughness and resistance to
delamination.
The SEM characterization of the nanostructured YSZ coating
highlights its dense, uniform, and nano-granular morphology, which is

44
essential for high-performance thermal barrier applications. The nanoscale
features, including small grain size, intergranular connectivity, and
controlled porosity, contribute to the coating’s superior thermal insulation,
mechanical stability, and durability under thermal cycling. These structural
attributes affirm the potential of nanostructured YSZ coatings as advanced
materials for next-generation thermal barrier systems.

4.3 SEM CHARACTERIZATION OF YSZ COATING AFTER

OXIDATION TEST

Figure 13 SEM characterization after oxidation test

The SEM characterization of the YSZ (Yttria-Stabilized Zirconia)

coating after the oxidation test at 1100°C, as shown in the provided
micrographs, reveals significant microstructural changes that occurred due
to prolonged high-temperature exposure. These changes critically impact
the performance and durability of the thermal barrier coating (TBC)
system. Image (a) displays a low-magnification cross-sectional view of the
multilayer coating, including the YSZ top coat, the NiCrAlY bond coat,
and the Hastelloy X substrate. A prominent network of cracks is visible at

45
the YSZ-bond coat interface, indicative of thermal mismatch stress and
possible delamination initiation zones. The cracks result from repeated
thermal cycling and the differential thermal expansion coefficients of the
YSZ and bond coat, which create mechanical stresses that accumulate over
time. The relatively large crack observed suggests that the interface
integrity has been compromised, which may reduce the coating’s overall
protective function.
Image (b), captured at higher magnification, further highlights the
critical degradation mechanisms occurring at the interface and within the
bond coat. The crack in the YSZ layer is more clearly defined, showing
that it propagates along the top coat and bond coat interface, exacerbated
by the formation of the thermally grown oxide (TGO) layer. The presence
of TGO is evident between the bond coat and YSZ, where it has developed
due to oxidation of aluminum and other reactive elements in the bond coat
during high-temperature exposure. While a thin, continuous TGO layer is
desirable to provide oxidation resistance, excessive TGO growth and
associated stresses can lead to delamination and spallation of the top coat.
The TGO layer observed here appears irregular and relatively thick,
indicating advanced oxidation and possibly cyclic thermal exposure. Such
growth can create significant internal stress due to volumetric changes,
leading to cracking and pore formation.
The image also shows the formation of oxide phases within the bond
coat, which may not be homogeneous. These oxides, along with the
observed pores, are indicative of internal oxidation and localized
degradation. The pores could result from the volatilization of certain
elements or the evolution of gas during the oxidation process, which
weakens the mechanical structure of the bond coat. The identified oxides
may include alumina and other complex spinels that form due to the
reaction of Ni, Cr, and Al with oxygen at elevated temperatures.

46
 Overall, the SEM analysis after oxidation at 1100°C illustrates the
degradation mechanisms common in TBCs under high-temperature service
environments. The prominent crack propagation, thick TGO formation,
oxide growth within the bond coat, and associated porosity highlight the
failure risks when the coating system is subjected to prolonged thermal
loading. These observations suggest that while the YSZ coating can
initially provide excellent thermal insulation, its long-term stability heavily
relies on controlling TGO growth, maintaining a strong interface with the
bond coat, and minimizing crack formation through optimized coating
process parameters and material selection. In practical applications, these
findings underscore the importance of developing advanced bond coat
formulations and applying tailored heat treatment or sealing techniques to
enhance the oxidation resistance and mechanical integrity of the TBC
system during extended high-temperature operation.

4.4 SEM CHARACTERIZATION AFTER HOT CORROSION TEST

The SEM characterization of the Yttria-Stabilized Zirconia (YSZ)
thermal barrier coating (TBC) after the hot corrosion test provides critical
insights into the structural integrity and failure mechanisms under
aggressive corrosive environments. The micrograph clearly shows a
multilayer system consisting of a porous YSZ top coat, a metallic bond
coat, and a metallic substrate. A prominent horizontal crack is observed at
the interface between the YSZ top coat and the bond coat, suggesting a
significant loss of adhesion due to the corrosive attack.

47
 Figure 14 SEM characterization after hot corrosion test

This delamination is typically attributed to the chemical interactions

between the corrosive species and the bond coat elements, leading to the
formation of a thick, brittle, and uneven corrosion product layer at the
interface. Hot corrosion is known to initiate primarily in the bond coat,
where the interaction with molten salts such as sulfates (often Na₂SO₄ and
V₂O₅ in industrial gas turbine or marine environments) leads to the
depletion of aluminum and other reactive elements. As a result, a non-
protective oxide scale forms instead of a stable alumina layer,
compromising the oxidation and corrosion resistance of the coating. This
degraded oxide scale becomes brittle and spallable, promoting the
nucleation and propagation of cracks. In the provided image, the wide
crack running parallel to the interface is a direct consequence of such
corrosive degradation, facilitated by thermomechanical stresses and phase
transformations within the oxide scale and the bond coat.

48
 The YSZ layer itself appears porous and rough, which, although
typical for thermal insulation, can become a liability under hot corrosion
conditions. The pores and microcracks in YSZ may serve as pathways for
corrosive agents to penetrate and react with the underlying bond coat.
Furthermore, the thermal mismatch between the ceramic YSZ and the
metallic bond coat under cyclic thermal and chemical loads results in strain
accumulation at the interface, exacerbating the delamination process. The
degradation products formed during hot corrosion tests typically exhibit
poor mechanical cohesion and significantly reduce the adhesion strength
between the layers.
In addition, the bond coat displays early signs of internal oxidation
and corrosion-induced damage. The presence of corrosion products (not
visually labeled here but inferable from typical hot corrosion behavior) can
lead to volume changes and stress buildup, contributing to coating failure.
These reactions not only weaken the bond coat mechanically but also
consume protective elements like Al, thereby reducing the long-term
corrosion resistance of the TBC system. The substrate appears largely
unaffected in the image, suggesting that the bond coat still provides a
certain level of protection; however, the severe cracking indicates that the
TBC is near the end of its effective life.
The SEM micrograph after the hot corrosion test highlights the
critical role of the bond coat in maintaining the structural and functional
integrity of the TBC system. The severe interfacial cracking and porous
top coat morphology underline the vulnerability of such coatings in
corrosive environments at high temperatures. Future improvements may
focus on enhancing the corrosion resistance of the bond coat, optimizing
the YSZ deposition process to reduce porosity, and developing more
chemically stable ceramic top coats. These advancements would be

49
essential for extending the service life of TBCs in harsh industrial
applications such as gas turbines and marine engines.

4.5 VICKERS HARDNESS

The hardness comparison between uncoated and Yttria-Stabilized

Zirconia (YSZ) coated Hastelloy X demonstrates a substantial
improvement in surface mechanical properties due to the plasma spray
coating process. Hastelloy X, a nickel-based superalloy known for its
excellent oxidation resistance and high-temperature strength, is widely
used in aerospace and industrial applications. However, its surface
hardness can be a limiting factor in wear-intensive environments. To
address this limitation, YSZ coatings were applied using the plasma spray
method, which allows for the deposition of dense, well-adhered ceramic
layers capable of withstanding extreme thermal and mechanical loads.
In the present analysis, the hardness of the uncoated Hastelloy X was
recorded at approximately 240 Vickers Hardness Number (VHN),
indicating the base material’s inherent hardness level. In contrast, the YSZ-

50
coated specimen exhibited a significantly increased hardness value of
around 680 VHN. This improvement is attributed to the high hardness and
wear resistance properties of YSZ ceramics, which effectively protect the
underlying substrate from deformation and abrasive wear. The thermal
barrier nature of the YSZ coating also contributes to the stability of the
surface layer under elevated temperatures, thus preserving the hardness
over extended service life.
The enhanced surface hardness is further supported by the
microstructural integrity offered by the plasma spray technique, which
ensures good coating density and adhesion. The ceramic coating acts as a
shield, absorbing and distributing mechanical loads more effectively than
the uncoated surface. This makes YSZ-coated Hastelloy X highly suitable
for demanding applications involving friction, erosion, or high thermal
gradients. Overall, the significant increase in hardness with YSZ coating
confirms the coating's potential to improve the operational durability and
performance of Hastelloy X components, making it a promising solution
for advanced engineering applications.

51
 CHAPTER 5
CONCLUSION

The present investigation focused on the structural integrity and

degradation mechanisms of a thermal barrier coating (TBC) system
comprising a Hastelloy X substrate, a NiCrAlY bond coat, and a Yttria-
Stabilized Zirconia (YSZ) top coat. Both the bond coat and top coat were
applied via the plasma spray technique—a widely adopted method in
thermal barrier applications due to its ability to produce layered, adherent
coatings with controlled porosity. Post-deposition, the coated system was
subjected to high-temperature oxidation and hot corrosion tests to simulate
extreme service conditions encountered in gas turbines and other high-
temperature industrial components. Scanning Electron Microscopy (SEM)
characterization was carried out to understand the microstructural
evolution and damage characteristics resulting from these thermal and
chemical exposures.
The SEM analysis following the oxidation test at 1100 °C revealed
the formation of a thermally grown oxide (TGO) layer between the YSZ
top coat and the NiCrAlY bond coat. The presence of a TGO is expected
and generally considered beneficial up to a certain thickness, as it serves
as a barrier to oxygen diffusion. However, excessive growth of TGO
introduces residual stresses due to the mismatch in thermal expansion
coefficients, often leading to cracking at or near the interface. Indeed,
visible microcracks and delamination zones were observed in the SEM
images, indicating partial failure of the coating system under prolonged
thermal exposure. Additionally, oxidation of the NiCrAlY layer led to the
depletion of Al, compromising the formation of a stable alumina scale and
potentially reducing the long-term protective capability of the bond coat.

52
 Following the hot corrosion test, more severe degradation features
were observed. The SEM micrographs showed a wider crack at the YSZ–
bond coat interface and increased porosity in the YSZ layer. The hot
corrosion environment, typically induced by molten salts such as Na₂SO₄
and V₂O₅, exacerbates degradation by disrupting the formation of
protective oxides and accelerating bond coat consumption. In this case, the
depletion of Al from the NiCrAlY bond coat was accompanied by the
formation of non-protective oxides and corrosion-induced spallation
zones. These effects compromised the structural cohesion between layers,
further enlarging interfacial cracks and promoting delamination. The YSZ
layer, although inherently resistant to thermal cycling, was penetrated by
corrosive species through its porous network, allowing the underlying
layers to undergo chemical attack.
The microstructural damage observed from both oxidation and hot
corrosion tests demonstrates the critical role of bond coat integrity and
microstructural optimization in prolonging the service life of TBC systems.
While plasma spraying offered a good initial adherence and layered
structure, it also introduced microstructural features like porosity and splat
boundaries that can become initiation sites for failure under aggressive
conditions. The use of Hastelloy X as a substrate provided mechanical
stability and oxidation resistance, but the overall durability of the TBC
system was limited by the degradation of the bond coat and subsequent
delamination at the interface.
In conclusion, the SEM characterization underscores the necessity
for improving bond coat oxidation and corrosion resistance, optimizing top
coat microstructure, and minimizing porosity through advanced processing
or post-treatment techniques. These enhancements are essential for
developing robust TBC systems capable of withstanding prolonged
exposure to high-temperature oxidation and hot corrosion environments.

53
54
 CHAPTER 6
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