International Conference On Engineering Innovations And Solutions (ICEIS-2016)

EXPERIMENTAL INVESTIGATION OF
CERAMIC COATING USING PLASMA SPRAY AND
HVOF METHOD

M.Pradeep, M.Sathyaprabhu, M.E., (Assistant professor),

Dept. of Manufacturing Engineering, Dept. of Manufacturing Engineering,
Erode Sengunthar Engineering College Erode Sengunthar Engineering College,
Erode - 638057, India, Erode - 638057, India

Abstract: Hot corrosion and erosion in boilers and

1. INTRODUCTION
related components are responsible for huge losses, both direct
Erosion is a serious problem in many engineering systems,
and indirect, in power generation; these problems can be
including steam and jet turbines, pipelines and valves used in
prevented by either changing the material or altering the
slurry transportation matter and fluidized bed combustion
environment. Corrosion prevention by the use of coatings for
systems. Gas and steam turbines operate in environments
separating material from the environment is gaining
where the ingestion of solid particles is inevitable. In
importance in surface Engineering. Atmospheric plasma spray
industrial applications and power generation, such as coal
process was used to deposit a yttria stabilized zirconia (YSZ)
burning boilers, fluidized bedsand gas turbines, solid particles
coatings on a stainless steel 304 substrates. High Velocity
are produced during the combustion of heavy oils, synthetic
Oxy-Fuel Spraying (HVOF) a novel variation on combustion
fuels, and pulverized coal. The protection of metals or alloys
spraying, has had a dramatic influence on the field of thermal
against corrosion and wear can be achieved by development
sprayby using non ceramic materials.The thermal fatigue test
and the use of better corrosion, dielectric strength and wear
and salt spray test of the coating was investigated, also
resistant thermal spray coatings.
dielectric strength and sliding wear were investigated.
Scanning electron microscopy (SEM) and high resolution A.STAINLESS STEEL

were employed to examine the surface cross-sectional
morphologies of coatings before dielectric strength, sliding
wear, thermal shock and salt spray test .This coatings was
more effective in salt environment. The plasma spray coatings
of yttria stabilized zirconium (YSZ) coatings and high velocity
oxy-fuel spraying (HVOF) provides good resistance to the
stainless steels to withstand optimum corrosion and wear
properties.
Keywords
HVOF- high velocity oxy-fuel spraying
SEM- Scanning electron microscopy
Stainless steel differs from carbon steel by the amount of
chromium present. Unprotected carbon steel rusts readily
when exposed to air and moisture. Stainless steels contain
sufficient chromium to form a passive film of chromium
oxide, which prevents further surface corrosion by blocking
oxygen diffusion to the steel surface and blocks corrosion
from spreading into the metal's internal structure, and, due to
the similar size of the steel and oxide ions, they bond very
strongly and remain attached to the surface.
1.1. FUNDAMENTALS OF THERMAL SPRAY COATING

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Thermal spraying is a process in which molten, semi-molten To determine the mechanical property such
or solid particles are deposited on a substrate. Consequently, as Thermal shock test for thermal barrier
the spraying technique is a way of generating a stream of coating.
such particles. Coatings can be generated if the particles that To determine the sliding wear of the coated
can plastically deform at impact with the substrate, which may sample materials.
only happen if they are molten and sufficiently rapid.
3. METHODOLOGY
The classification of spray techniques is based on
The objective of this investigation is to evaluate
Combustion flame spraying
plasma sprayed coatings by various tribological tests. The
Two-Wire Electric Arc spray process
experimental work has been planned in the following
Detonation spray process
sequence:
High Velocity Oxy - Fuel process(HVOF)
Atmospheric Plasma spray process (i) Selection of base metal which withstands
Super alloys have been developed for high high temperature and resists corrosion.
temperature applications, but they are not able to meet the
(ii) Preparation of base metal samples for
requirements of high temperature strength, high temperature
coating confirming to ASTM standards.
erosion and corrosion resistance simultaneously. Coatings in
gas turbine serve a variety of purposes, whether in jet engines, (iii) Coating the base metal samples by plasma
land based power generation turbines or marine engines. A spray process.
first requirement to operate turbines at higher temperatures (iv) Metallurgical analysis using Scanning
was, of course improved strength. Unfortunately, these Electron Microscope and coating
conditions also mean severe oxidation/corrosion problems. thickness measurement.
Plasma spray coating is widely used since thick coatings can
(v) Evaluation of the optimum coating
be applied at high deposition rates and due to its excellent
powder composition by Thermal cyclic
surface finish and high adhesion to the substrate. Among the
fatigue test.
various coating powders Yttria Stabilised Zirconia was used
widely different percentage but only few studies on Yttria (vi) Evaluation of various properties such as
Stabilized Zirconia was reported. Also high velocity oxy-fuel micro hardness, porosity and surface
spraying (HVOF) process is to determine the above properties. roughness, corrosion resistance, wear
resistance of coatings.
2. OBJECTIVES (vii) Evaluation of residual stress over the
The objectives of these investigations are coated sample.
To study the surface morphology of the
coated sample by Scanning Electron The objective of this investigation is to evaluate
Microscope. plasma sprayed coatings by various tribological tests. The
To characterize the obtained thermal barrier experimental work has been planned in the
coating by salt spray corrosion test. following sequence:

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The objective of this investigation is to evaluate plasma

sprayed coatings by various tribological tests. The
experimental work has been planned in the
following sequence:
Base Metal: Stainless Steel
Grade: 304

Material

Sample Preparation
Pre Processing Surface Cleaning
Surface Activation

Coating Process Plasma Spray coating + (HVOF)

Coating Composition
8%Y2O3 + 92% ZrO2
+ Non oxide materials

Properties Evaluation

Thermal Salt Spray Coating Dielectric

Fatigue test Corrosion test Thickness Withstand tests

Results and Discussions

Conclusions

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 International Conference On Engineering Innovations And Solutions (ICEIS-2016)
3.1. SELECTION OF BASE METAL
Super alloys are metallic materials for service at
high temperatures, particularly in the hot zones (turbine
blades) of gas turbines. Such materials allow the turbine to
operate more efficiently by withstanding higher temperatures.
These high pressure turbine blades are made up of Nickel and
Chromium. Since Stainless steel contains Nickel and
Chromium and also it is commercially available, the base
metal is taken as stainless steel. Stainless Steel 304 grades are
taken as base metal since it withstands high temperature and
resists corrosion. Stainless Steel 304 grades are economical.
Table 3.1 Chemical Composition Grade 304 Stainless Steel
Cr Ni Mn C S Si P
18- 8- 2.00 0.03 0.030 1.00 0.045
20 12
3.2 .SPECIMEN PREPARATION
Stainless steel is taken as a specimen material.
Different samples of varying size were taken for analysis. The
samples with dimension are shown in Figure 4.1.The metallic
substrate should be treated before coating. The substrate is
usually covered with grease that protects the surface against
corrosion. The grease was removed in the cleaning process.
Cleaned pieces are shaped in order to obtain desired
dimensions to avoid sharp angles that are difficult to be
coated.
The remaining area other than the area to be
coated was covered with masks during spraying. At last,
immediately prior to the deposition process, the surface has to
be activated. Without activation, the coating would not adhere
to the substrate surface. Activation by abrasive grit blasting,
i.e. roughening, is the most frequently applied process
nowadays.
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Fig 3.1 Rectangular Samples With Dimensions
(1) SURFACE CLEANING
Degreasing of new metal substrates was done by
using organic solvent acetone. The process was carried out in
a clean room and the remaining liquid was carefully recycled.
Every care was taken to protect the operator from hazardous
exposure. surface cleaning can be carried out as a wet or dry
process depending on the nature of the soiling present, the
product, the process and the type of production equipment dry
cleaning is used mainly for process where dry are particulate
products are handled. Wet cleaning is employed whenever
possible due to their high efficiency of the wet cleaning
process
(2) SUBSTRATE SHAPING
Shaping is the process of working with metals to
create individual parts, assemblies are large scale structures.
The term covers the wild range of work from large ships and
bridges. It therefore includes a correspondingly wide range of
skills and process tools. The substrates need to be shaped in
order to meet the dimensional specifications. The adherence
becomes lower because of the high concentration of thermal
stresses inside the coatings sprayed in such places. Substrate
shaping was done by wire cutting method.
(3) PLASMA SPRAY COATING
Among the different coating systems, the plasma
spray process is commonly used to protect the hardware
operating in high temperature environments, such as
combustor liners and gas turbine blades, from excessive high
heat fluxes and temperature. Plasma spraying uses metal in
powder form. The coating materials in the form of a powder
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is passed into a plasma jet in which powder particles are
melted and accelerated towards the surface to be coated.
plasma spraying is one of the most versatile hot
facing technique available for the application of coating
materials used to protect components from abrasive wear,
adhesive wear erosion wear or surface fatigue and corrosion
(such as that caused by oxidation are sea water generally any
material which does not decomposed, vaporise, sublimate, or
dissociate on heating can be plasma spray. Repeatedly a large
of metallic and non-metallic materials (metals, alloys,
ceramics, and polymers) can be deposited by the plasma
spraying.
3.3. PLASMA SPRAY OPERATING PARAMETERS
Table 3.2 Plasma Spray Operating Parameters
Operating Parameters
Plasma gun 3 MB Gun, 40 Kw
Inert gases Argon, Hydrogen
Argon :- 80- 90 LPM
Flow Rate
Hydrogen:- 15 to 18 LPM
6. Sliding wear tests.
3.5. THERMAL CYCLIC FATIGUE TEST
Thermal cyclic fatigue test was performed on a
muffle furnace as shown in Figure. The optimum Yttria
stabilized Zirconia composition has to be identified in order to
withstand the high temperature and resist corrosion. Initial
weight of coated sample was noted. Coated sample were kept
inside the furnace. The coated sample were heated to steady
state temperature of 980C and maintained for 1 hr. The
sample was cooled to room temperature within 10 minutes.
The temperatures will be noted the number of cycles till
coating starts to peel off temperature. Initial weights of each
coated samples were noted. Coated samples were kept inside
the furnace. The coated samples were heatedto steady state
temperature of 980C within 10 minutes and maintained for 45
minutes. The samples were cooled to room temperature within
10minutes. The cooling was done by air. The cycle was
repeated for 100times. The test was performed at Strength of
materials Lab, Department of Mechanical Engineering,
Mahendra Institute of Technology.

Powder Feed 40-50 gms/rein 3.6. COATING THICKNESS MEASUREMENT

Coating thickness measurement was measured
Type of Nozzle GH Nozzle
by the Scanning Electron Microscope. The scanning electron
Electric current in Amps 500 Amps microscope offers high quality imaging with high resolution.
Voltage 70 Volts Commonly, the microscope can be operated in two modes.
They are secondary electron imaging (SEI) and backscattered
Machine Type Metco MN plasma spray system
electron imaging (BEI).
The SEI-mode is generally used for imaging the
3.4. TESTING OF COATINGS surfaces of structures. In the BEI-mode, the obtained images
Five specimen of each coating composition was contrast depends on the atomic number of the structure under
taken for each test. After the completion of coatings over the the electron beam. The higher the average atomic weight the
samples, they were subjected to various tests such as: brighter the region will appear in the BSE image. Images of
1. Thermal Cyclic Fatigue test coated samples are roughly composed of three regions; the
2. Coating thickness measurement base metal, the coating layer and the background. These
3. Microstructure Analysis (SEM) structures differ in contrast due to the different average atomic
4. Salt spray test weight.
5. Dielectric strength tests.

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3.7. MICRO STRUCTURE ANALYSIS
The Scanning Electron Microscope (SEM) uses a
focused beam of high-energy electrons to generate a variety of
signals at the surface of solid specimens. The signals that
derive from electron-sample interactions reveal information
about the sample including external morphology chemical
composition, and crystalline structure and orientation of
materials making up the sample. A ranging from
approximately 1 cm to 5 microns in width can be imaged in a
scanning mode using conventional SEM techniques
(magnification ranging from 20X to approximately 30,000X,
spatial resolution of 50 to 100 nm).
The scanning electron microscope (SEM) is used
to scan the coated specimen Yttria Stabilized Zirconia (8%
Y2O3 + 92% ZrO2). The surface morphology is determined by
the use of scanning electron microscope. It explains the
arrangement of particles on the coated surface and also gives
the morphology of the cross-section and explains the adhesion
of the coating to the substrate and determines any crack has
been identified between the coating and substrate. Accelerated
electrons in an SEM carry significant amounts of kinetic
energy, and this energy is dissipated as a variety of signals
produced by electron-sample interactions when the incident
electrons are decelerated in the solid sample. These signals
include secondary electrons that produce SEM images,
backscattered electrons (BSE), diffracted backscattered
electrons, photons, visible light and heat. Secondary electrons
and backscattered electrons are commonly used for imaging
samples. Secondary electrons are most valuable for showing
morphology and topography on samples and backscattered
electrons are most valuable for illustrating contrasts in
composition in multiphase samples.
X-ray generation is produced by inelastic
collisions of the incident electrons with electrons in discrete
orbitals of atoms in the sample. As the excited electrons
return to lower energy states, they yield X-rays that are of
afixed. Thus, characteristic X-rays are produced for each
element in a mineral that is "excited" by the electron beam.
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SEM analysis is considered to be "non-destructive"; that is, X-
rays generated by electron interactions do not lead to volume
loss of the sample, so it is possible to analyse the same
materials repeatedly. Essential components of all SEMs
include Electron Source, Electron Lenses, Sample Stage,
Detectors for all signals of interest, Display or Data output
devices and the infrastructure requirements include Power
Supply, Vacuum System, Cooling system, Vibration-free
floor, Room free of ambient magnetic and electric fields.
SEMs always have at least one detector usually a secondary
electron detector, and most have additional detectors. The
specific capabilities of a particular instrument are critically
dependent on the detectors which it accommodates.
3.8. SALT SPRAY TEST
The salt spray test is a standardized and popular
corrosion test method. Used to check corrosion resistance of a
material and surface coatings. Usually the materials to be
tested are metallic and finished with a surface coating which is
intended to provide a degree of corrosion production to the
underlying metal. Salt spray test is an accelerating corrosion
test that provides a corrosive attack to coated sample in order
to predict a suitability of the coating in use a protective
finish.A neutral salt spray test (NSS) is performed to
determine qualitative resistance to corrosive attack on the
product this test is commonly employed on protective coated
products. Coatings are exposed to a corrosive atmosphere
under controlled conditions for different durations. Resistance
to corrosive attack is used to assess the quality of coating
against the condition of the test.
The acetic acid salt spray test (ASTM B 117) is also used for
testing inorganic and organic coatings, but is particularly
applicable to the study or testing of decorative chromium
plating and cadmium plating on steel or zinc die castings, as
well as for the evaluation of product quality. This test can be
as short as 16 hours, although it normally ranges from 144 to
500 hours or more. Similar to the neutral salt spray test, a 5%
sodium chloride solution is used, but the solution is adjusted to
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a pH range of 6.5 to 7.2 by the addition of acetic acid. The
temperature of the salt spray chamber is controlled to the same
temperature range
as for neutral salt spray.

Fig 3.2 Process Of Neutral Salt Spray Test

3.9. SALT SPRAY TEST PARAMETERS

Table 3.3 Salt Spray Test Parameters

REQUIREMENTS RESULTS
PARAMETERS

pH solution 6.5 to 7.2 6.72 7.02

Air pressure 12 to 18 psi 12 16 psi

Concentration of sodium 5.1 5.6

chloride 5%+/-1 %

Collection of solution per 1.2 1.6

hour 1 2 ml ml

34.8
Chamber temperatures 35+/-2c 35.6c

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