A Major Project Report on

ABRADABLE COATINGS FOR GAS TURBINE

A dissertation work submitted to JNTUH College of Engineering
Hyderabad, in partial fulfillment of the requirement for the award of
the degree of

BACHELOR OF TECHNOLOGY

In
METALLURGICAL ENGINEERING
By
M. ABHINAV (12011A0602)
D. RAJASHEKAR BHUPAL (12011A0624)
T. SOUMYA (12011A0644)

Under the Esteem Guidance of

External Guide Internal Guide

Mr. Bharat K. Pant Dr. S. Devaki Rani
DGM Associate Professor & HOD
Surface Coatings and Dept. of Metallurgical
Treatment Department Engineering
BHEL Corporate R&D JNTUH-CEH

DEPARTMENT OF METALLURGICAL ENGINEERING

JNTUH COLLEGE OF ENGINEERING HYDERABAD
KUKATPALLY, HYDERABAD
2016
 ABRADABLE COATINGS FOR GAS TURBINE
Project report submitted in partial fulfillment of the requirements
for the award of the degree
Bachelor of Technology
In
Metallurgical Engineering
By
M. Abhinav (12011A0602)
D. Rajashekar Bhupal (12011A0624)
T. Soumya (12011A0644)

Done at
Surface Coatings and Treatment (SCT)
BHEL Corporate R&D
Vikas Nagar, Hyderabad -500093

Under the Esteem Guidance of

External Guide Internal Guide

Mr. Bharat K. Pant Dr. S. Devaki Rani
DGM Associate Professor & HOD
Surface Coatings And Treatment Dept. of Metallurgical
Department Engineering
BHEL Corporate R&D JNTUH-CEH

DEPARTMENT OF METALLURGICAL ENGINEERING

JNTUH COLLEGE OF ENGINEERING HYDERABAD
KUKATPALLY, HYDERABAD
2016
 DECLARATION

We, M.Abhinav (12011A0602), D.Rajashekar Bhupal (12011A0624), and

T.Soumya (12011A0644), hereby declare that the project work entitled
ABRADABLE COATINGS FOR GAS TURBINE is carried out by us under the
guidance of Mr. Bharat K. Pant, DGM, SCT Department, BHEL Corporate
R&D, and Dr. S. Devaki Rani, Associate Professor & HOD, Department of
Metallurgical Engineering, JNTUH-CEH, in partial fulfilment of the requirement
of award of degree of B.Tech. in Metallurgical Engineering offered by College of
JNTUH College of Engineering, Hyderabad.

The work is original and has not been submitted for any Degree /Diploma of this or
any other University.

M. Abhinav (12011A0602)

D. Rajashekar Bhupal (12011A0624)

T. Soumya (12011A0644)
 BHARAT HEAVY ELECTRICALS LMITED
CORPORATE RESEARCH AND DEVELOPMENT

SURFACE COATINGS AND TREATMENT LABORATORY

HYDERABAD - 500 093

CERTIFICATE

This is to certify that the project entitled ABRADABLE COATINGS FOR GAS
TURBINE is a bonafide work carried out by M. ABHINAV (12011A0602),
D. RAJASHEKAR BHUPAL (12011A0624) and T. SOUMYA (12011A0644), in
partial fulfillment of the requirements for the award of the degree of Bachelor of
Technology in METALLURGICAL ENGINEERING, from JNTU, HYDERABAD.
This work is carried out under our supervision and guidance of Mr. Bharat K. Pant.

External Guide

Mr. Bharat K. Pant

DGM
Surface Coatings and
Treatment Dept.
BHEL Corporate R&D
 JAWAHARLAL NEHRU TECHNOLOGICAL UNIVERSITY
HYDERABAD
COLLEGE OF ENGINEERING
(AUTONOMOUS)

DEPARTMENT OF METALLURGICAL ENGINEERING

HYDERABAD - 500085

CERTIFICATE

Certified that this is a bonafide record of the dissertation work entitled,

ABRADABLE COATINGS FOR GAS TURBINE, done by M. ABHINAV
(12011A0602), D. RAJASHEKAR BHUPAL (12011A0624), and T. SOUMYA
(12011A0644) submitted to the faculty of Metallurgical Engineering, in partial
fulfilment of the requirements for the Degree of BACHELOR OF TECHNOLOGY
from Jawaharlal Nehru Technological University Hyderabad, College of Engineering
(Autonomous), Hyderabad.

Internal Guide
 Dr. S. Devaki Rani
Associate Professor & HOD,
Dept. of Metallurgical Engineering,
JNTUH-CEH, Hyd-85.

JAWAHARLAL NEHRU TECHNOLOGICAL UNIVERSITY

HYDERABAD
COLLEGE OF ENGINEERING
(AUTONOMOUS)

DEPARTMENT OF METALLURGICAL ENGINEERING

HYDERABAD - 500085

CERTIFICATE

Certified that this is a bonafide record of the dissertation work entitled,

ABRADABLE COATINGS FOR GAS TURBINE, done by M. ABHINAV
(12011A0602), D. RAJASHEKAR BHUPAL (12011A0624), and T. SOUMYA
(12011A0644) submitted to the faculty of Metallurgical Engineering, in partial
fulfillment of the requirements for the Degree of BACHELOR OF TECHNOLOGY
from Jawaharlal Nehru Technological University Hyderabad, College of Engineering
(Autonomous), Hyderabad.
 Head of Department

Dr. S. Devaki Rani

Associate Professor & HOD,
Dept. of Metallurgical Engineering,
JNTUH-CEH, Hyd-85.

ACKNOWLEDGEMENTS

It is our great fortune to have had the opportunity to work on this exciting and
inspiring project in this organization. The learning and experience we have received
here is of inexplicable value to us. It gives us immense pleasure to express our
paramount gratitude to each one of those who made this possible.

We express our he artful thanks to the Principal of JNTUH-CEH, and Dr. S.

Devaki Rani, HOD of Metallurgical Department, for supporting us in visiting this
industry as per our interest.

We would like to thank with deep gratitude Dr. Sukumar Roy, BHEL
Corporate R&D for providing us with this unique opportunity of carrying out our
project at BHEL R&D and also being a great support during the course of the project.

We express our deep sense of gratitude to our guide Mr. Bharat K. Pant,
SCT Department, BHEL Corporate R&D for his constant guidance and
encouragement throughout our work and for all the provisions made to us.

We are thankful and fortunate enough to get constant encouragement, support

and guidance from our project guide, Dr. S. Devaki Rani, Associate professor &
HOD, Dr. K. Srinivasa Vadayar, Smt. R. Sri Rama Devi, and Dr. B. Ramesh
Chandra who helped us in successfully completing our project work.

We whole heartedly thank Dr. A. K. Maiti, LM, SCT Department, and

BHEL Corporate R&D for his motivation and timely support throughout the project.

We extend our sincere gratitude to Mr. Pankaj Joshi Sr. Engineer, SCT
Department, BHEL Corporate R&D and to all the technical staff in SCT
Department BHEL Corporate R&D who helped us enormously in this project.
 We are grateful to Mr. S K Padhee, AGM, HRD & ATE, Mr. Shaji
Verghese, AGM, HRD & ATE and Mrs. Vijaya Rani, Raj Bhasha Ofiicer, HRD
& ATE, BHEL Corporate R&D for rendering their valuable support.

M. Abhinav (12011A0602)

D. Rajashekar Bhupal (12011A0624)

T. Soumya (12011A0644)

CONTENTS

ABSTRACT i

LIST OF FIGURES ii

LIST OF TABLES iii

CHAPTER-1: Introduction 1

CHAPTER-2: Literature Review 4

CHAPTER-3: Materials and Experimental Procedures 27

CHAPTER-4: Results and Discussion 43

CHAPTER-5: Conclusions 46

REFERENCES 48
 ABSTARCT

In thermal power plants, significant improvements in overall efficiencies can be

achieved by reducing the leakage flows in compressor and turbine sections. One way
to minimize these leakages is by the use of thermally sprayed abradable sealing
coatings. This project discusses the development of abradable coating for gas turbine
shroud segments for service temperatures up to 750 C.

The abradable coating is developed using plasma coating technique. Plasma spray
coating is an economical and effective method applied to various machine parts to
reduce the surface degradation. Porosity, bond strength, and micro hardness tests were
performed over the plasma coated samples.

Porosity, bond strength, micro hardness tests results were coming within the bracket
suggested by the previous researchers. The porosity of the coating was in the range of
50%, bond strength values were in between 2500 psi to 3000 psi and hardness
measured was in the range of 60 to 70 on HR15Y scale.

Keywords: Abradable coatings; Abradability; Gas turbine; Plasma spraying.

1
 LIST OF FIGURES

Figure No. Title Page No.

Areas in a gas turbine that is coated with thermally

1.1 sprayed abradable materials. 2

2.1 Conventional plasma spraying process. 22

Schematic illustration of the type of abradable thermal

2.2 spray coating used in the different areas of a turbine and 26
compressor.

3.1 Function of abradable coatings on Labyrinth Seals. 29

3.2 Labyrinth seal rub event. 29

3.3 Function of abradable seals on shrouded rotor and 30

stationary blades.

(A) Abradable coating applied to the outer steam path

seals on the casing.
(B) Abradable coating applied to the inner steam path
3.4 seals on the shrouds of the stationary blades. 31

3.5 View of the plasma spraying unit. 37

3.6 Pictorial view of plasma sprayed coating samples. 37

3.7 Struers Minitom low speed cutting machine. 38

3.8 Positest pull-off adhesion tester. 40

3.9 Rockwell superficial principle. 42

3.10 Rockwell hardness tester. 42

4.1 Optical image at 50X showing uniform porosity. 44

2
 LIST OF TABLES

Table No. Title Page No

2.1 Different surface treatment techniques. 5

2.2 Electroplating Characteristics and Applications 11

2.3 Categorization of common thermal spray processes. 19

3
CHAPTER-1

INTRODUCTION

1
 CHAPTER 1

INTRODUCTION

Abradable thermal spray coatings, also known as clearance control / seal coatings are
successfully used today in aero-engines, industrial and steam turbines, and various
other types of turbo machinery applications to reduce leakage gaps between stationary
and rotating parts in order to improve efficiency (Figure 2.1). Thermally sprayed
abradable coatings have been applied to the compressor sections of jet engines since
the late 1960s and predominantly consist of composite materials deriving their
abradability from the use of low shear strength materials or from porous, friable
coating structures.

The key performance criteria for abradable seal coatings systems are summarized as
follows:
Rub compatibility against blades, knife fins or labyrinth seals under various
conditions
Coating cohesive strength
Oxidation resistance at high temperatures
Corrosion resistance in aqueous or chemical fluid or gases
Resistance to corrosive attack at elevated temperatures
Sintering resistance at elevated temperatures
Thermal shock resistance
Resistance to solid particle erosion

The relevance of these factors is dependent on the type of application and the level of
temperature and chemical exposure to which the abradable coating is exposed.

Figure 1.1: Areas in a gas turbine that is coated with thermally sprayed
abradable materials.

An increase in efficiency by 1 percent on the current installed 2500 GW electricity

base worldwide will lead to a reduction of carbon dioxide emissions by 300 million
tonnes per year, with savings of roughly 100 million tonnes of fossil fuel[1]. This will
effectively reduce the emission of greenhouse gases which in turn will reduce the

2
cause of global warming. A 1 percent increase in the gas turbine efficiency can be
achieved by reducing the tip clearances in the high pressure turbine section. Several
models have been quantified by different authors that correlate the efficiency of a
turbine engine with the tip clearances. A model was presented by Bringhenti and
Barbosa[2] that correlate well with the performance of an existing engine. In this
model the efficiency is calculated by equation 1.
/h
= ref[1-K.( ).(rt/rm)]

Where
k = 1+ 0.586 ( ztip3.63)
is the rotor efficiency with tip clearance effects included
is the tip clearance height
h is the blade span
ztip is the tip Zweifel loading coefficient

It is estimated that an increase in efficiency by 0.5% for a 1000MW plant would save
1 Million dollars per year, along with the reduction in the emission of CO2[3].

For the last several years abradable coatings have been successfully used in gas
turbines as clearance control coatings[4]. There are several classes and categories of
abradable coatings and these coatings have been used successfully in the land and air
based gas turbines[5,6]. These coatings act as sacrificial coatings as they get abraded
upon contact of rotating turbine blades with the coated stationary component, thereby
reducing the leakage of gas in between the blade tip and the stationary component.

Objectives of the present work :

The objectives of the present work can be outlined as:

1. Abradable coating using plasma coating technique and studying the effects of
coating properties on changing the coating parameters for gas turbine for service
temperatures up to 750 0C.
2. Perform porosity, bond strength and micro hardness tests for the coated samples.

3
CHAPTER-2

LITERATURE REVIEW

CHAPTER 2

LITERATURE REVIEW

4
This chapter deals with the literature survey on various aspects of surface treatment,
surface coatings, plasma spraying, the coating materials and their characteristics.

I. SURFACE TREATMENT

SURFACE TREATMENT

THERMO HARDENING
CHEMICAL
1. Flame
1. Carburizng 2. Induction
2. Nitriding 3. Laser
3. Cyaniding 4. Electron Beam
4. Boronizing
5. Chromizing

Table 2.1: Different surface treatment techniques.

THERMO CHEMICAL TREATMENT

Chemical heat treatment is the process used to achieve different properties in core
and steel components. Numerous industrial applications require a hard wear
resistant surface called the case, and a relatively soft, tough inside called the core.
Example: Gears.
They are two different methods. The first method is known as thermochemical
treatment because the surface composition of steel changes by diffusion of carbon
and/or nitrogen and sometimes other elements.
The second method is known has surface hardening, it involves phase
transformation by rapid heating and cooling of the outer surface . The aim of both
methods are same.

1. CARBURIZING

Carburizing is the most widely used method of surface hardening. Here, the
surface layers of a low carbon steel (<0.25) is enriched with carbon up to 0.8-
1.0%. The source of carbon may be a solid medium, a liquid or a gas.

5
 In all cases, the carbon enters the steel at the surface and diffuses into the steel as
a function of time at an elevated temperature. Carburizing is done at 920-950C.
Where Fe(c) represents carbon dissolved in austenite. the rate of diffusion of
carbon in austenite, at a given temperature is dependent upon the diffusion
coefficient and the carbon concentration gradient.
The carburizing equation given previously, is reversible and may proceed to the
left, removing carbon from the surface layer if the steel is heated in an atmosphere
containing carbon dioxide (CO2). This is called decarburization.
Decarburization may be prevented by using an endothermic gas atmosphere in the
furnace to protect the surface of the steel from oxygen, carbon dioxide and water
vapor. An endothermic gas atmosphere is prepared by reacting relatively rich
mixtures of air and hydrocarbon gas (usually natural gas) in an externally heated
generator in the presence of a nickel catalyst.
Carburizing can be done by Pack carburizing, Liquid carburizing, Gas carburizing
and vacuum carburizing.

2. NITRIDING

In contrast to the processes described before, nitriding is carried out in the ferrite
region. Consequently, no phase change occurs after nitriding .
This part to be nitrided should possess the required core properties prior to
nitriding. Pure ammonia decomposes to yield nitrogen which enters the steel.
The solubility of nitrogen in ferrite is small. Most of the nitrogen that enters
thesteel forms hard nitrides (e.g. Fe3N). A typical nitriding steel contains alloying
elements of 1%Al, 1.5%Cr and 0.2%Mo. Al, Cr, and Mo form very hard and wear
resistant nitrides.
The temperature of nitriding is 500-590C. the time for a case depth of 0.02mm is
about 2 hour. In addition with wear resistance, it also increases the resistance of a
carbon steel to corrosion in moist atmospheres.
A common problem encountered in nitriding is the formation of nitride (Fe4N)
on the outer layers of the case , known as the white layer, as it looks white
under the microscope. This layer is very brittle and tends to crack. It must be
removed by final grinding operation. Its formation can be minimized by
maintaining the correct ratio of NH3/H2 in the gas mixture during the heat
treatment.
There are two ways by which white layer can be totally suppressed
i. Floe process or double stage nitriding, where a white layer is first
produced and then decomposed.
ii. Ion nitriding process or Plasma nitriding.

3. CYANIDING

In cyaniding and carbonitriding processes, the surface layer of steel (with 0.3-
0.4%C) is hardened by addition of both carbon and nitrogen.

6
 In this case that contain both carbon and nitrogen are produced in liquid salt baths
(cyaniding) or by use of gas atmospheres (carbonitriding). The temperatures used
are generally lower than those used in carburizing, being between 750-900C.
Exposure is for a shorter time, and thinner cases are produced, up to 0.010in. For
cyaniding and up to 0.030in. For carbonitriding.
Cyaniding is done in a liquid bath of NaCN, with the concentration varying
between 30 and 97%.
Carbon and nitrogen so formed in atomic form diffuse into the steel and give thin
wear resistant layer of the carbonitride -phase.
The temperature used for cyaniding is lower than that for carburizing and in the
range of 800-870C. the time of cyaniding is 0.5-3 hour to produce a case depth of
0.25 mm or less.
Cyaniding process is not suitable for hardening those parts which are subjected to
shock, fatigue and impact because nitrogen addition has adverse effects on such
properties of steels.

4. BORONIZING

Boronizing is one of the recent methods of surface hardening, which may be

applied to any ferrous material but is generally adopted for carbon steels and tool
steels.
In the case of pack process, the components are packed in heat resistant boxes
with mixtures of granules or paste of boron carbide or other boron compounds
with addition of activators and diluents at 900-1000C.
Boron diffuses inwards and iron borides (FeB and Fe2B) layers are formed. On
the outer surface, FeB phase forms, While in the interior, Fe2B phase is formed.
FeB phase is more brittle and is not desirable.
Higher temperatures, longer treatment times and high alloy steels favour the
formation of FeB phase. The boride layers are very hard. The hardness of boride
layers on steel ranges between 1500 and 2100 VHN.
Boride layer depths range from 0.012 to 0.127 mm, depending on material and
application. The treatment time required for a case depth of 0.15 mm is 6hours at
about 900C.
Thick layers (up to 0.127 mm) for abrasive wear
Thin layer (up to 0.025 mm) for adhesive wear and friction reduction
Boronizing increases tool and mold life by improving resistance to abrasive,
sliding and adhesive wear. It reduces the use of lubrication as have low coefficient
of friction. But high process temperature may lead to the distortion of the
component. Moreover, the component shows poor fatigue and corrosion
resistance.

5. CHROMIZING

Like Boronizing process, Chromizing is also used for surface hardening of both
carbon and tool steels.
There are two basic types of chromizing : Pack chromizing and gaseous
chromizing. The components to be chromized are packed with fine chromium
powder and additives.

7
 A typical chromizing mixture consists of 60% Cr or ferro chrome (with carbon
content not exceeding 0.1%), 0.2% ammonium iodide, and 39% kaolin powder.
Diffusion of chromium takes place at 900-1020C, and chromium carbide is
formed on the surface of steel. The treatment time needed for achieving a case
depth of 0.02-0.04 mm is 12 hours at 900-1020C. Hardness of chromium carbide
layer is about 1500 VHN.
HARD CHROMIZING : If the steel, which to be chromized, contains enough
carbon (minimum 0.35%), a corrosion and wear resistant chromium layer will be
formed on the surface of the work-piece during the chromizing treatment.
SOFT CHROMIZING : On steel, with low carbon content (<0.35%), a chromium
carbide layer cannot be formed. Instead a chromium diffusion layer builds up
during the chromizing process which can reach up to 200m in thickness and a
chromium content of upto 35%. The high chromium content endows the work
piece with an excellent resistance against corrosion and oxidation while
maintaining its ductility.
Chromizing leads to excellent corrosion resistance under a variety of severe
conditions. High temperature oxidation resistance is also improved significantly.
Components may undergo bending and flanging operations without spalling.
Hardness of chromium carbide layer is about 1500VHN.

HARDENING

1. FLAME HARDENING

Flame hardening is the simplest form of surface hardening heat treatment.

This process consists of heating the large work-piece, such as crank shaft, axle,
large gear, cam, bending roller, or any other complicated cross-section, by an oxy-
acetylene, or oxyfuel blow pipe, followed by spraying of jet of water as coolant.
After hardening, reheating of the parts is carried out in furnace or oil bath at about
180-200 C for stress relieving.
Normally, case depth up to 3mm can be achieved.
Four methods are generally use for

Flame Hardening
Flame Hardening
a) Stationary (Spot): Torch and work is stationary.
b) Progressive: Torch moves over a work piece.
c) Spinning: Torch is stationary while work piece rotates.
d) Progressive-spinning: Torch moves over a rotating work piece.

2. INDUCTION HARDENING

Induction hardening may be used for local surface heat treatment. Generally, it is
used to surface harden crank shafts, cam shafts, gears, crank pins and axles. In this
process, heating of the component is achieved by electromagnetic induction.
Here, an alternating current of high frequency passes through an induction coil
enclosing the steel part to be heat treated. The induced emf heats the steel. the

8
 depth up to which the heat penetrates and rises the temperature above Ac3 is
inversely proportional to the square root of the AC frequency.
Correspondingly, the hardened depth decreases with increasing frequency in
induction hardening, the heating time is usually a few seconds. Immediately after
heating water jets are activated to quench the surface . Martensite is produced at
the surface, making it hard and wear resistant. The microstructure of the core
remains unaltered. Induction hardening is suitable for mass production of articles
of uniform cross section.

3. LASER HARDENING

Laser hardening treatment is widely used to harden localized areas of steel and
cast iron machine components. This process is sometimes referred to as laser
transformation hardening to differentiate it from laser surface melting phenomena.
There is no chemistry change produced by laser transformation hardening, and the
process, like induction and flame hardening, provides an effective technique to
harden ferrous materials selectively.
As laser beams are of high intensity, a lens is used to reduce the intensity by
producing a defocused spot of size ranging from 0.5 to 25 mm. proper control of
energy input is necessary to avoid melting.
Laser transformation hardening produces thin surface zones that are heated and
cooled very rapidly, resulting in very fine Martensitic microstructures, even in
steels with relatively low hardenability. High hardness and good wear resistance
with less distortion result from this process.
Laser hardening has the advantage of precise control over the area to be hardened,
an ability to harden reentrant surfaces, very high speed of hardening and no
separate quenching step (the quench is effected by the mass of the unheated
material).
The relationship between depth of hardening and power is as follows.
The disadvantage is that the hardening is shallower than in induction and flame
hardening.

4. ELECTRON BEAM HARDENING

This process is used for hardening those components which cannot be induction
hardened because of associated distortion. Automatic transmission clutch cams
(SAE 5060 steel) are hardened by this processes.
Electron Beam (EB) hardening is like laser treatment, is used to harden the
surfaces of steels. The EB heat treating process uses a concentrated beam of high-
velocity electrons as an energy source to heat selected surface areas of ferrous
parts. Electrons are accelerated and are formed into a directed beam by an EB gun.
After exiting the gun, the beam passes through a focus coil, which precisely
controls beam density levels (spot size) at the work piece surface and then passes
through a deflection coil.
To produce an electron beam, a high vacuum of 10-5 torr is needed in the region
where the electrons are emitted and accelerated. This vacuum environment
protects the emitter from oxidizing and avoids scattering of the electrons while
they are still traveling at a relatively low velocity.

9
 Like laser beam hardening, the EB process eliminates the need for quenchants but
requires a sufficient work piece mass to permit self quenching.
A mass of up to eight times that of the volume to be EB hardened is required
around and beneath the heated surfaces. Electron beam hardening does not require
energy absorbing coatings, as does laser beam hardening.
Normally, case depth upto 0.75 mm can be achieved by this method. A
minicomputer is used to control voltage, current, beam time and focus.

II. SURFACE COATINGS

Plating is the application of a surface finish to another material; it provides the

surfaces of manufactured parts with a number of desirable physical, chemical, and
appearance qualities. Nearly all manufactured or fabricated products made of metal or
having metal components have some type of surface finishing. Plating increases
sturdiness, prevents corrosion, provides hardness, or gives an attractive finish to an
object.

Electroplating is inexpensive, reliable, efficient, and applicable to a wide variety of

shapes and sizes. However, traditional electroplating technologies often result in
uneven surface finishes, and have inherent pollution problems.

Electroless plating has increased in popularity due to improvements in solution

stability, pretreatment cycles, reducing agents, and equipment. In addition, electroless
plating provides uniform thickness and deposits, especially in deep recesses, bores,
and blind holes.

Alternative plating methods such as PVD, CVD, and thermal spraying reduce the
amount of contaminated wastewater produced by plating, but have high unit-plating
costs.

COATING TYPES

There are 46 different processes regulated under metal finishing standards featuring
different technologies, operational steps, inputs, and outputs. Some of the more
common plating technologies are the following:

1. ELECTRODEPOSITED / ELECTROPLATING

Electroplating is used to change the surface properties of a metal part by adding a

metal coating by the action of electric current; it is also called "electrodeposition,".
The object to be coated receives a negative charge and is immersed into a solution that
contains a salt of the metal to be deposited. The metallic ions of the salt carry a
positive charge and are attracted to the object.

Surface pretreatment by chemical or mechanical means is important for

electroplating, as the successful adhesion of the surface coating depends on removing
contaminants and films from the substrate.

10
In addition, the geometric shape and contour of the object affects the thickness of the
deposited layer. Objects with sharp corners and features will have thicker deposits on
the outside corners and thinner ones in the recessed areas, because the current flows
more densely to prominent points than to less accessible areas. This characteristic of
electroplating limits applications with uneven surfaces or that have depressions or
hidden holes.

Some metals used in electroplating are aluminum, brass, bronze, cadmium, copper,
chromium, iron, lead, nickel, tin, and zinc, as well as precious metals such as gold,
platinum, and silver. Different types of coatings can be achieved through control of
parameters such as voltage, amperage, temperature, residence times, and purity of the
bath solutions.

Applications of electroplating are numerous because it is an inexpensive and simple

method; it is used in all aspects of electronics, optics, and the automobile industry
where, for example, chrome plating is used to enhance the corrosion resistance of
metal parts.

Metal Coating Characteristics Typical Applications

Connecting elements, auto
Zinc Excellent corrosion protection for and
steel; economic & safe construction industry, plant
engineering
Alloys zinc, copper, Excellent corrosion protection, Extreme corrosion resistance
and precious metal decorative finish, wear resistant combined with high thermal
stress, e.g., car exhausts,
engine
elements, and electronics
parts
Copper, Nickel, Good corrosion protection, Motor vehicles, plumbing
Chrome decorative finish fittings, steel furniture, shop
fittings
Hard Chrome Extreme hardness, resistance to Hydraulics, mold making,
wear, corrosion protection,
improved vehicles, shafts, and bearings
lubricating properties
Silver, silver alloys Good conductivity for heat and Jewelry, electrical and
electricity, antibacterial,
decorative electronic parts, household
finish with enhanced value. goods
Gold Flexible, non- reactive with other Jewelry, electrical and
elements, good electrical electronic parts, household
conductivity, resistance to
corrosion, goods
enhanced value
Bronze Resistance to wear and corrosion, Bearing shells
flexible
Tin Softness, flexible, solderable Household applicanes,
electronics, printed circuits,
food industry

Table 2.2: Electroplating Characteristics and Applications

11
2. ELECTROLESS NICKEL

Electroless nickel plating operates without electricity; the process action is purely
chemical. Coating is achieved through metal ion exchange using chemical reduction
in a hot aqueous solution.

An electroless nickel coating is uniform; it will not build up on corners or projections.

The deposited metal layer has an even thickness over all surfaces of the component
regardless of its shape; this cannot be achieved with electrodeposited coatings.

Typical thickness of electroless plating can be as thin as .0005" and up to.010".

Electroless coatings, used on a broad range of base materials, provide exceptional
hardness and resistance to wear and corrosion.

Parts to be plated have to be pre-treated, and each type of material requires a specific
pre treatment. The deposit properties of an electroless nickel layer and the
performance of the plated component depend upon the phosphorous content, the
purity, the substrate, the pre treatment, and the thickness of the coating.

Electroless nickel solutions operate in a pH 4 - 9 medium at a temperature of between

77 to 198F (25 - 92C.) The plating speed of the solution is between 2 to 25
micrometers per hour (um/hr) and the deposit thickness generated on the parts
depends upon the operating conditions and time.

Electroless nickel deposits may be heat treated to improve abrasion resistance,

increase hardness, and enhance adhesion. The heat treatment temperature must be
above 464F (240C), and to obtain the maximum hardness, it is necessary to treat
parts at a temperature of 752 F (400C) for 1 hour. Heat treatment achieves hardness
of about 1000 V P N (Vickers) or HK 0.05/HV 0.1 (Knoop).

Coating thicknesses for engineering uses vary from 0.0005 inch to 0.0015 inch (0,012
mm to 0,038 mm) with hardness from approximately 48 to 52 Rockwell C. When the
plating is heat treated approximately 750F (400C) for one hour, the obtainable
hardness varies from 58 to 64 Rockwell C.

The microelectronics industry uses electroless nickel plating to create a barrier

between base metal and the final overplate. Industries such as mining, petroleum,
aerospace, molds and dies, medical, dental, and pharmaceutical, use electroless nickel
plating over steel for its excellent wear and corrosion resistance and for its ability to
provide a coatings with a uniform deposit. Electroless nickel layers of
about 50 um on steel have very good resistance to marine environments. In many
cases, it is possible to use electroless nickel plated steel as a substitute for stainless
steel.

Electroless nickel coatings are resistant to a wide range of chemicals, which makes
them suitable for many applications in the chemical industry, for example, stirrers,
valves, reaction tanks, and covers.

Some benefits of electroless nickel plating are the following:

Superior corrosion resistance.

12
 Natural flexibility, providing excellent mold release properties.
Freedom from porosity..
A solderable, hard coating for light metals.
Overall uniformity of deposit with no edge buildup.

3. ANODIZING

The anodizing process creates a coating both on the surface and into the metal; it is
usually performed on aluminum for protection and cosmetic purposes. Thin coatings,
2 to 25 m (100 to 1000 in) can be coated on most aluminum.

Anodizing refers to the electrochemical oxidation of a metal in a suitable electrolyte

such as sulfuric acid in various concentrations. When the temperature and current
density are controlled, the aluminum oxide develops both on the surface and into the
aluminum. The coating penetrates into the base material as much as it builds up on the
outside. The term "thickness" includes both the buildup and penetration.

Soft anodizing refers to coatings produced in electrolytes that operate at room

temperature. Soft anodize coatings tend to be more porous and can be dyed a wide
variety of colors and then sealed. Since the coating is an integral part of the base
metal, anodic coatings are very durable and not subject to chipping under harsh
service conditions.

In hard anodizing, the electrolytes operate at lower temperatures. The chemical action
on the aluminum oxide is slower, but eventually produces a harder and thicker coating
than soft anodizing.

4. CARBURIZING / CARBONIZING

Carburizing is the introduction of carbon into the surface layer of steel with low
carbon content. The process includes heating the components in a liquid or gaseous
carbon-containing medium. The time and temperature parameters of the treatment
control the depth of penetration of carbon into the surface.

The most typical carburizing temperature is 1750oF, although lower temperatures may
be used to reduce distortion or improve control of the case depth tolerance. Uniform
temperatures must be present to produce uniform carburizing and hardening, and to
control distortion. It is important to maintain the temperature of the steel, rather than
just furnace temperature.

After carburizing, the work is either slow-cooled for later quench hardening, or
quenched directly into various liquids.

The combination of hard surface and soft interior withstands very high stress and
fatigue, and offers low cost and superior flexibility in manufacturing. Gears, ball and
roller bearings, and piston pins are often carburized.

13
5. PVD/CVD

The physical vapor deposition (PVD) method deposits the coating over the entire
object simultaneously, rather than in localized areas.

PVD is a surface modification process that takes place in a vacuum chamber heated at
approximately 750F (400C). The PVD process directs a concentrated, high-energy
plasma onto a metal surface. The thickness of the coating is approximately 2 to 4
microns (0.000079 to 0.00016 inch or 0.002 mm to 0.004 mm), resulting in improved
corrosion resistance.

All PVD hard coating processes combine the following:

A method for depositing the metal
Combination with an active gas, such as nitrogen, oxygen, or methane
Plasma bombardment of the substrate to ensure a dense, hard coating

PVD methods differ in the means for producing the metal vapor and the details of
plasma creation. The primary PVD methods are ion plating, ion implantation,
sputtering, and laser surface alloying.

Chemical vapor disposition (CVD) is a subset of PVD; the variations are in the way
that the gases are converted. CVD occurs in a vacuum chamber filled with a reacting
chemical vapor heated at a temperature of approximately 1650F (900C).

Companies use CVD to improve corrosion and wear resistance, however, the facilities
required to create the extreme temperatures make CVD more expensive than other
processes.

Specialty processes such as PVD/CVD and plasma spray coating are relatively more
expensive plating methods.

6. PLASMA SPRAY COATING

Plasma spray is a high-speed flame spray process that produces a dense, high-quality,
machinable coating. In plasma spray coating, powders are injected into the plasma
stream to melt the material. The molten material is propelled and bonded onto the
substrate.

The coatings thickness is dictated by the size of the feedstock for powders, the size of
the droplets for arc spraying, and the size of the atomized droplets created by the
liquid spray process. Coatings are typically applied to a thickness of 0.003 to 0.010
inches (0.076 to 0.25mm), but can be up to 0.020inches (0.51mm) without detrimental
impact to the coating properties.

Plasma spray coating enhances, protects, and alters surface properties for many
purposes, including dimensional restoration, thermal barriers, conductivity, wear
resistance, and chemical resistance.

Plasma spray coating is used for fiber and textile-like applications where a long-
lasting wear resistant coating is needed. Plasma spray processes are used to coat

14
electronic components, automotive sub assemblies, medical instruments, jet engines,
and other structural parts, as well as orthopedic implants, and consumer products.

COATING MEASUREMENT

Hardness and thickness are important dimensions of plating materials because the
effectiveness, longevity, and cost of the final product depend, not only on the
appropriate selection of coating material, but also on the amount applied, and the final
surface texture.

1. HARDNESS

Hardness is the property of a material that enables it to resist deformation, however, is

not an intrinsic material property dictated by precise definitions in terms of
fundamental units of mass, length, and time. A hardness property value is the result of
a defined measurement procedure.

Hardness tests characterize the materials and determine if they are suitable for their
intended use. All of the hardness tests described in this section involve the use of a
specifically shaped indenter, significantly harder than the test sample. The indenter is
pressed into the surface of the sample using a specific force. Either the depth or size
of the indent is measured to determine a hardness value.

Establishing a correlation between the hardness result and the desired material
property makes hardness tests useful in industrial and R&D applications.

Four major hardness scales described are the following:

Rockwell
Brinell
Vickers
Microhardness (Knoop)

Each of these scales uses a specifically shaped diamond indenter, made from carbide
or hardened steel. The indenter is pressed into the material with a specific force using
a defined test procedure. The hardness values are determined by measuring either the
depth of indenter penetration or the size of the resultant indent. All of the scales are
arranged so that the hardness values increase, as the material gets harder.

Current methods such as Rockwell or Brinell, use a minimum load of approximately 5

grams force (gf.) However, the resulting indentation may be too large for thin film
coating, and the underlying layer interferes with accurate hardness measurement.
Therefore, an ultra-low load hardness test, a microhardness test, was developed for
thin coatings.

Rockwell

The Rockwell test method is the most commonly used hardness test method, since it
is easier to perform and more accurate than other types. Rockwell is used on all
metals except where the test metal structure or surface conditions introduce too much

15
variation, where the indentations is too large for the application, or where the sample
size or shape prohibits its use.

The Rockwell hardness test measures the depth of indentation produced by the
preliminary and total test forces. First, a preliminary test force is applied; this is the
zero or reference position. Next, an additional test force is applied to reach the total
required test force. This additional force is held for a predetermined amount of time
and released, but the preliminary test force still applied. The indenter reaches the final
position at the preliminary force and the distance traveled from the major load
position is measured and converted to a hardness number.

Brinell

The Brinell hardness test method consists of indenting the test material with a
hardened steel or carbide ball. The diameter of the indentation left in the test material
is measured with a low powered microscope. The Brinell harness number is calculated
by dividing the load applied by the surface area of the indentation.

Compared to the other hardness test methods, the Brinell ball makes the deepest and
widest indentation, so the test averages the hardness over a wider amount of material,
which will more accurately account for multiple grain structures and any irregularities
in the uniformity of the material.

The Brinell method is the best for achieving the bulk or macro-hardness of materials
with heterogeneous structures.

Some applications where the Brinell hardness test is used are the following:
Forgings/castings
Heavy truck/bulldozer parts
Engine blocks and heads
Non-homogeneous materials
Rear-end housings
Springs
Variety of large, coarse-surface parts

Vickers

In the Vickers hardness test method, the indenter is a right pyramid with a square base
and an angle of 136 degrees between opposite faces. The two diagonals of the
indentation left in the surface of the material after removal of the load are measured
using a microscope and their average calculated. The area of the sloping surface of the
indentation is calculated. The Vickers hardness is the quotient obtained by dividing
the kgf1 load by the square millimeter area of indentation.

The Vickers test has two force ranges micro (10 to 1000gram) and macro (1 to
100kilogram). The indenter is the same for both ranges, and the Vickers hardness
values are continuous over the total range of hardness for metals (typically HV100 to
HV1000).

16
The advantages of the Vickers hardness test are that extremely accurate readings can
be taken, and only one type of indenter used for all types of metals and surface
treatments. Because of the wide test force range, the Vickers test can be used on
almost any metallic material. The part size is only limited by the testing instruments
capacity.

Microhardness (Knoop)

The Microhardness test method, according to ASTM E-384, specifies a range of loads
using a diamond indenter to make an indentation that is measured and converted to a
hardness value.

There are two types of microhardness indenters, a square base pyramid shaped
diamond used in a Vickers tester and a narrow rhombus shaped indenter for a Knoop
tester. Typically, loads are very light, ranging from a few grams to one or several
kilograms. The term microhardness refers to static indentations made with loads not
exceeding 1 kgf.

The procedure for testing is very similar to that of the standard Vickers hardness test,
except that it is done on a microscopic scale with higher precision instruments.
Precision microscopes used to measure the indentations, have a magnification of
approximately X500, and measure an accuracy of +0.5 micrometers.

Like the Vickers test, the Knoop microhardness test has a wide test force range, and it
can be used on almost any metallic material. The primary application of the
microhardness test is measuring the hardness of a thin film coating.

2. THICKNESS

Coatings applied to base materials provide properties not inherent in the base,
including corrosion and wear resistance, conductivity, color, and solderability. The
amount of coating applied to a material, that is, the coating thickness, is crucial to the
products final use and cost.

This section describes four non-destructive2 methods of measuring coating thickness.

Each method was devised to achieve cost-effective, accurate, and repeatable results,
and is particularly suited to a specific coating(s)/substrate combination.

The four methods described are:

X-Ray fluorescence
Eddy-current
Magnetic induction
Beta backscatter

X-ray Fluorescence

When a material is subjected to x-ray bombardment, some of its electrons will gain
energy and leave the atom, releasing a photon of x-ray energy known as x-ray
fluorescence. The energy level or wavelength of fluorescent x-rays is proportional to
the atomic number of the atom and is characteristic for a particular material. The

17
quantity of energy released will be dependent upon the thickness of the material being
measured.

The X-ray fluorescence unit consists of an x-ray tube and a proportional counter.
Emitted photons ionize the gas in the counter tube proportional to their energy,
permitting spectrum analysis for determination of the material and thickness.

X-ray fluorescence is the most precise measurement method; it is used to measure the
thickness of small-diameter parts, or dual coatings such as gold and nickel over
copper.

Eddy Current

The Eddy current technique is used to nondestructively measure the thickness of

nonconductive coatings on nonferrous metal substrates, for example, paint on
aluminum and acrylic on copper.

Eddy current inspection is based on the principles of electromagnetic induction and

therefore has many similarities to the electromagnetic induction test method.
Magnetically induced eddy currents generate an opposing magnetic field, which alters
the circuit reactance and the output voltage. The change in output voltage is used to
calculate the coating thickness.

Eddy current gauges use a constant pressure probe and display results on an LCD;
they can store measurement results or perform instant analysis of readings, and output
the data to a printer or computer for further examination. The typical tolerance is
1%. Testing is sensitive to surface roughness, curvature, substrate thickness, type of
metal substrate, and distance from an edge.

Some applications of the Eddy current method are the following:

Crack detection
Material thickness measurements
Coating thickness measurements
Conductivity measurements

Magnetic Induction

Magnetic induction is used to measure the thickness of a non-magnetic coating (zinc,

cadmium, paint, powder coating, etc.) over a steel substrate. Most coatings on steel
and iron are measured this way.

A probe system is part of a transformer circuit that reacts to the presence of a

magnetic material. The circuit efficiency and output voltage increase when the probe
is brought near a magnetic surface, providing parameters, which may be used to
measure the distance (coating thickness) from the magnetic surface.

Beta Backscatter

The Beta backscatter method is similar to the X-ray fluorescent in that the area tested
is the target of radiation, and the energy emitted from the surface is measured. Beta

18
rays are electrons emitted from unstable radioisotopes. The electrons penetrate the
plating material and reflect back (back scatter) toward the source. They are collected
and counted with a Geiger-Mueller tube for conversion to coating thickness.

Beta-backscatter measuring technique, in compliance with ASTM B567 specification,

measures many typical thickness applications, including gold on nickel, copper on
epoxy, silver on copper, titanium nitride on steel, and tin-lead alloys. Probe systems
are designed for precise measurement on a variety of surfaces, from small parts
(connectors and pins) to large parts (circuit boards).

III. THERMAL SPRAYING

It is the generic category of surface modification technique that apply consumables in

the form of a finely divided molten or semi molten droplets to produce a coating onto
the substrate kept in front of the impinging jet. The melting of the consumables may
be accomplished in a number of ways, and the consumable can be introduced into the
heat source in wire or powder form. Thermal spray consumables can be metallic,
ceramic or polymeric substances. Any material can be sprayed as long as it can be
melted by the heat source employed and does not undergo degradation during
heating[7]. An interesting aspect of thermal spraying is that the surface temperature
seldom exceeds 20000 C. Hard metal or ceramic coating can be applied to
thermosetting plastics. Stress related distortion problems are also not so significant.
The spraying action is achieved by the rapid expansion of combustion gases (which
transfer the momentum to the molten droplets) or by a separate supply of compressed
air.

THERMAL SPRAY PROCESSES

GAS COMBUSTION ARC PROCESSES

PROCESSES
1. Electric arc
1. Oxy-fuel/ wire 2. Plasma arc
2. Oxy-fuel / powder
3. Detonation gun
4. HVOF

Table 2.3: Categorization of common thermal spray processes.

19
Table 2.2 shows the common thermal spray processes fitting into the above mentioned
categories. The plasma spraying process is discussed briefly in the following.

IV. PLASMA SPRAYING

Until the 1950s, matter was thought to exist in only three forms i.e. solid, liquid, and
gas. But all that changed when a Danish engineer discovered plasma. But what is
plasma?

Plasma is matter that exists in the form of ions and electrons. Basically, it is a gas
thats been electrified charged with freely moving electrons in both the negative and
positive state.

The situation is actually a resultant of further energy being given to a gas which
causes the breaking free of negatively charged electrons from the nucleus. On a
deeper level, plasma can be described as a gas thats been partially ionized. It is a
mixture of neutral atoms, atomic ions, electrons, molecular ions, and molecules
present in excited and ground states. The charges (positive and negative) balance each
other therefore; a good number of these charges are electrically neutral.

The charged particles present in plasma are responsible for its high electrical
conductivity. Since plasma consists of electrons, molecules or neutral gas atoms,
positive ions, UV light along with excited gas molecules and atoms, it carries a good
amount of internal energy. And when all these molecules, ions and atoms come
together and interact with a particular surface, plasma treatment is initiated. Hence, by
selecting a gas mixture, pressure, power etc. the effects of plasma treatment upon any
surface can also be specified or precisely tuned.

How plasma treatment is performed?

A plasma treatment is usually performed in a chamber or enclosure thats evacuated

(Vacuum plasma). The air within the chamber or enclosure is pumped out prior to
letting gas in. The gas then flows in the enclosure at a low pressure. This is done
before any energy (electrical power) is applied. It is imperative to know that plasma
treatment performed at low temperature can easily process materials that are heat
sensitive. These types of plasma are sometimes referred to as cold plasma. Plasma
treatment is mainly used for cleaning, surface activation, deposition, and etching - if
you are interested in knowing more about plasma etching (plasma etch) we
recommend you read our article about plasma etching.

Useful for pretreatment of surfaces.

On an industrial level, plasma treatments are used for treating surfaces of various
materials prior to any coating, printing or adhesion. Therefore, it can also be referred
to as a kind of pretreatment of surfaces. Treatment with plasma removes any foreign

20
contaminants present on the surface of a material making it more suitable for further
processing. Materials like plastics are prone to lose any type of printing or coating
done on their surfaces because of their glossy texture unless treated. Plastics are made
up of polypropylene and are homopolar which means that they do not bond that
easily.

Applying plasma treatment on such surfaces can result in an effective pretreatment of

surface activation before any gluing, printing or lacquering could take place.
Similarly, materials like ceramics and glass can also be treated with plasma. Usually,
industrial oxygen is used in plasma treatment as a process gas, hence receiving the
title of oxygen plasma. However, atmospheric air is also used in many plasma surface
treatments referred to as atmospheric plasma. Depending on the type of material that
is being treated with plasma, effects can remain prominent for just a few minutes or
even months.

Plasma spraying is the most versatile thermal spraying process and the general
arrangement is shown in Figure 2.1. An arc is created between tungsten tipped copper
cathode and an annular copper anode (both water cooled). Plasma generating gas is
forced to pass through the annular space between the electrodes. While passing
through the arc, the gas undergoes ionization in the high temperature environment
resulting plasma. The ionization is achieved by collisions of electrons of the arc with
the neutral molecules of the gas. The plasma protrudes out of the electrode
encasement in the form of a flame. The consumable material, in the powdered form, is
poured into the flame in metered quantity. The powders melt immediately and absorb
the momentum of the expanding gas and rush towards the target to form a thin
deposited layer. The next layer deposits onto the first immediately after and thus the
coating builds up layer by layer. The temperature in the plasma arc can be as high as
10,000C and it is capable of melting anything. Elaborate cooling arrangement is
required to protect the plasmatron (i.e., the plasma generator) from excessive heating.

The equipment consists of the following modules.

The plasmatron: It is the device which houses the electrodes and in which the plasma
reaction takes place. It has the shape of a gun and it is connected to the water cooled
power supply cables, powder supply and gas supply hose.

The power supply unit: Normally plasma arc works in a low voltage (40-70
volts) and high current (300-1000 Amperes), DC ambient. The available power
(AC, 3-phase, 440 V) must be transformed and rectified to suit the reactor. This is
taken care of by the power supply unit.

The powder feeder: The powder is kept inside a hopper. A separate gas line
directs the career gas which fluidizes the powder and carries it to the plasma arc.
The flow rate of the powder can be controlled precisely.

21
 The coolant water supply unit: It circulates water into the plasmatron, the power
supply unit, and the power cables. Units capable of supplying refrigerated water
are also available.

The control unit: Important functions (current control, gas flow rate control etc.)
are performed by the control unit. It also consists of the relays and solenoid valves
and other interlocking arrangements essential for safe running of the equipment.
For example the arc can only be started if the coolant supply is on and water
pressure and flow rate is adequate.

THE REQUIREMENTS FOR PLASMA SPRAYING:

Roughness of the substrate surface: A rough surface provides a good coating

adhesion. A rough surface provides enough room for anchorage of the splats
facilitating bonding through mechanical interlocking. A rough surface is generally
created by shot blasting technique. The roughness obtained is determined by shot
blasting parameters, i.e., shot size, shape and material, air pressure, standoff
distance between nozzle and the job, angle of impact, substrate material etc.

Cleanliness of the substrates: The substrate to be sprayed on must be free from

any dirt or grease or any other material that might prevent intimate contact of the
splat and the substrate. For this purpose the substrate must be thoroughly cleaned
(ultrasonically, if possible) with a solvent before spraying. Spraying must be
conducted immediately after shot blasting and cleaning.

Cooling water: For cooling purpose distilled water should be used, whenever
possible. Normally a small volume of distilled water is recirculated into the gun
and it is cooled by an external water supply from a large tank. Sometime water
from a large external tank is pumped directly into the gun.

Process Parameters in Plasma Spraying : In plasma spraying one has to deal

with a lot of process parameters, which determine the degree of particle melting,
adhesion strength and deposition efficiency of the powder. Deposition efficiency
is the ratio of amount of powder deposited to the amount fed to the gun. An
elaborate listing of these parameters and their effects are reported in the
literature[8].

22
 Figure 2.1: Conventional plasma spraying process
Some important parameters and their roles are listed below:

Arc power: It is the electrical power drawn by the arc. The power is injected in to
the plasma gas, which in turn heats the plasma stream. Part of the power is
dissipated as radiation and also by the gun cooling water. Arc power determines
the mass flow rate of a given powder that can be effectively melted by the arc.
Deposition efficiency improves to a certain extent with an increase in arc power,
since it is associated with an enhanced particle melting[9]. However, increasing
power beyond a certain limit may not cause a significant improvement. On the
contrary, once a complete particle melting is achieved, a higher gas temperature
may prove to be harmful. In the case of steel, at some point vaporization may take
place lowering the deposition efficiency.

Plasma gas: Normally nitrogen or argon doped with about 10% hydrogen or
helium is used as a plasma gas. The major constituent of the gas mixture is known
as primary gas and the minor is known as the secondary gas. The neutral
molecules are subjected to the electron bombardment resulting in their ionization.
Both temperature and enthalpy of the gas increase as it absorbs energy. Since
nitrogen and hydrogen are diatomic gases, they first undergo dissociation
followed by ionization. Thus they need higher energy input to enter the plasma
state. This extra energy increases the enthalpy of the plasma. On the other hand,
the mono-atomic plasma gases, i.e. argon or helium, approach a much higher
temperature in the normal enthalpy range. Good heating ability is expected from
them for such high temperature. In addition, hydrogen followed by helium has a
very high specific heat, and therefore is capable of acquiring very high enthalpy.
When argon is doped with helium the spray cone becomes quite narrow which is
especially useful for spraying on small targets.

Carrier gas: Normally the primary gas itself is used as a carrier gas. The flow rate
of the carrier gas is an important factor. A very low flow rate cannot convey the
powder effectively to the plasma jet, and if the flow rate is very high then the
powders might escape the hottest region of the jet. There is an optimum flow rate

23
 for each powder at which the fraction of unmelted powder is minimum and hence
the deposition efficiency is maximum.

Mass flow rate of powder: Ideal mass flow rate for each powder has to be
determined. Spraying with a lower mass flow rate keeping all other conditions
constant results in under utilization and slow coating buildup. On the other hand, a
very high mass flow rate may give rise to an incomplete melting resulting in a
high amount of porosity in the coating. The unmelted powders may bounce off
from the substrate surface as well keeping the deposition efficiency low.

Torch to base distance: It is the distance between the tip of the gun and the
substrate surface. A long distance may result in freezing of the melted particles
before they reach the target, whereas a short standoff distance may not provide
sufficient time for the particles in flight to melt. The relationship between the
coating properties and spray parameters in spraying alpha alumina has been
studied in details. It is found that the porosity increases and the thickness of the
coating (hence deposition efficiency) decreases with an increase in standoff
distance. The usual alpha-phase to gamma-phase transformation during plasma
spraying of alumina has also been restricted by increasing this distance. A larger
fraction of the unmelted particles go in the coating owing to an increase in torch to
base distance.

Spraying angle: This parameter is varied to accommodate the shape of the

substrate. In coating alumina on mild steel substrate, the coating porosity is found
to increase as the spraying angle is increased from 30 to 60. Beyond 60 the
porosity level remains unaffected by a further increase in spraying angle. The
spraying angle also affects the adhesive strength of the coating. The influence of
spraying angle on the cohesive strength of chromia, zirconia 8-wt% yttria and
molybdenum has been investigated, and it has been found that the spraying angle
does not have much influence on the cohesive strength of the coatings.

V. THE TECHNOLOGY BEHIND ABRADABLE COATINGS

The abradability of the abradable thermal spray coating is its capability to readily
and sacrificially wear away in the event of contact by a mating rotating part, creating
debris that is soft and tiny in order to find its way out without eroding other parts of
the engine. The mating part will normally not experience any loss of material or, if
loss of material is experienced, it is usually negligible. Some abradable alloys resist
erosion by the flow of gases and are resistant to corrosion, oxidation and other
degradation mechanisms.
The abradable materials and structures reduce tip clearances by allowing the blades to
cut / abrade into the material without causing damage (overheating and wear) to the
blade tips. The ideal abradable will be characterized by a concentration of all wear in
the seal and no wear on the blade for a given rotor displacement. This allows the rotor
to cut into the stator without any reduction in blade length which, in turn, would lead
to increased unsealed gaps. Thus, the general rule is that abradable counterpart
coating should be softer than the dynamic rubbing component material to prevent

24
abrasive wear and/or friction-induced overheating of the dynamic component as much
as possible.

The two most important properties of a good abradable coating material are hardness
and lubricity. The materials must not be so hard as to cause wear of the mating part
but, in the same sense, not so soft as to be easily eroded by wear particles in the gas
stream. Lubricity allows the rubbing material to cut smoothly into the abradable
coating and not tear away large pieces of the coating.

The following matrix materials are commonly used to embed the abradable particles
(the exact composition of the materials is proprietary to the developers) and they are
all also softer than the traditional steel, titanium alloy or nickel alloy blades or
knife/fin seal materials used in turbomachinery:
Aluminium-Silicon materials for low temperature applications include a polymer
to generate porosity when burnt-out in subsequent heat treatment (sacrificial
phase).
MCrAlY (M=Cobalt, Nickel or Cobalt/Nickel, Chromium Aluminium Yttrium)
for mid-range temperatures in the compressor stages.
Yttrium-stabilised Zirconia (high temperature ceramic material) for high
temperature turbine Sections.

These materials may also include solid lubricants and release agents that assist with
the ease of separation of the abradable particles.

VI. THERMAL SPRAYING OF ABRADABLE COATINGS

Abradable coatings can either be applied by the flame (combustion) spray process or
the atmospheric plasma spray process. The atmospheric plasma spray process is a
higher temperature process than the flame spray process, which means that materials
with higher melting points can be applied with the atmospheric plasma spray process.

The abradable coatings typically applied using the flame spray process includes:

Nickel Graphite hardness of coating varies according to the ratio of nickel to

graphite and is suitable for rub incursions against steel and nickel alloy blades,
knives or labyrinth seals. Also suited for incursion against titanium blades
provided the coating has the correct sprayed hardness.

NiCrAl -Bentonite suitable for rub incursions against steel and nickel alloy
blades, knives and labyrinth seals used in steam turbine balance piston
applications. This coating is considered too abrasive for titanium blade
applications with the risk of blade tip oxidation and titanium fire generation.

NiCrFeAl Boron Nitride the boron nitride in this coating assists with
oxidation resistance and also acts as a solid lubricant that assists cutting processes
during blade incursions.

25
The abradable coatings typically applied using the atmospheric plasma spray
process includes:

Aluminium and Aluminium Bronze alloy/polymers these coatings combine

the desired properties of the soft shearable and heat resistant polymers with the
higher strength shearable alloys and are also used for rub incursions.

MCrAlY-Boron Nitride/Polymers coatings like CoCrAlY (Cobalt-Chromium-

Aluminium-Yttrium) have improved oxidation and corrosion resistance compared
to other Nickel-Chromium base abradable materials up to a maximum temperature
of 650C and in [other] some cases up to 750C.

Ceramic Zirconia base abradables these coatings have excellent thermal shock
resistance, toughness and sintering resistance and the coating structure and
properties created during thermal spraying makes this coating resistant to thermal
shock.

Figure 2.2: Schematic illustration of the type of abradable thermal spray

coating used in the different areas of a turbine and compressor

Figure 2.2 shows different abradable coatings and blade materials used at the different
operating temperatures. It is shown that as the operating temperature increases, the
sophisticated abradable coating and blade material also changes in order to withstand
the higher operating temperatures.

ORIGINAL EQUIPMENT MANUFACTURING SPECIFICATIONS AND

APPROVALS:

Several OEMs have developed material approvals and specifications specifically for
the application of different types of abradable thermal spray coatings to turbines and
compressor components. OEMs like Rolls-Royce, Pratt Whitney, Honeywell,
General Electric, Siemens and Volvo all have their own specifications for the type of
abradable to be applied to the different parts of turbines and compressors (low and
high temperature, as well as the different base materials).

26
Thermalspray has coated several components from the turbomachinery industry with
an aluminium polyester abradable thermal spray coating. The components include:

Labyrinth seals
Impeller eye and boss landings
Balance drums

CHAPTER-3

27
 MATERIALS AND
EXPERIMENTAL
PROCEDURES

CHAPTER-3

MATERIALS AND EXPERIMENTAL PROCEDURES

Coating deposition by plasma spraying involves a number of process variables, which

contribute in a large way to the quality of the coating. During spraying, various
operating parameters are determined mostly based on past experience. It therefore
does not provide the optimal set of parameters for a particular objective. In order to
obtain the best result with regard to any specific coating quality characteristic,
accurate identification of significant control parameters is essential. Deposition
efficiency of any coating is a characteristic which not only rates the effectiveness of
the spraying method but also is a measure of the coatability of the material under
study. This chapter is devoted to analyze the experimentally obtained results on the
deposition efficiency of alumina-titania coatings made at different operational

28
conditions.

I. ABRADABLE COATING APPLICATIONS FOR GAS

TURBINES
In steam turbines, abradable coatings should be applied to shaft seals, balance piston
seals and seals over shrouded blades. Application to all of these areas ensures a
complete solution that will maximize efficiency gains by reducing leakage flows
through labyrinths.

FUNCTION OF ABRADABLE COATINGS ON LABYRINTH SEALS:

The coating process is very flexible and can be applied to the stator of a labyrinth seal
system of any configuration. Coating thickness can be adapted to provide ideal
clearances between rotating seal fins and the stationary component. In addition, a
variety of material choices are available for different seal applications that can be
sprayed consistently with coating properties that minimize or eliminate seal fin
damage in the event of a rub.

LABYRINTH SEAL RUB EVENT:

Ideal abradability is schematically depicted below for a hypothetical labyrinth seal

system. Upon displacement, the rotor can come into contact with and rub against the
casing.

Without an abradable coating, as shown in Case 1, the rotor fins are worn and reduced
in length, which gives rise to an increased clearance of 1 that is much larger in size
than the initial design clearance of 0 around the entire circumference. This results in
deterioration of labyrinth seal efficiency.

Open Labyrinth Full Labyrinth

(Constant height)

Labyrinth with High Stepped Labyrinth

and Low Fins

Stator Rotor Abradable Coating

29
 Figure 3.1: Function of abradable coatings on Labyrinth Seals.

Case 0: Seal and Fin Condition Case 1: Seal and Fin condition
Before Rub Interaction Without Abradable Coating After
Rub Interaction

Static seal

Abradable
coating

Rotating fins

Case 2:
When anSeal
idealand Fin Condition
abradable coatingWith Abradable
is used, Coating
as shown After2,Rub
in Case the Interaction.
fins on the rotor
can cut cleanly into the stator without any reduction in rotor diameter or fin height.
Figure
initial 3.2: Labyrinth
position, the design seal rub event.
tip clearance of 0 is maintained around the circumference.

Both cases are boundary scenarios. In practice, mixed forms with some seal and some
fin wear will usually be observed. In general, fin wear up to 5 % of the total geometric
overlap of the rotor and stator, i.e., the total incursion depth, is acceptable.

FUNCTION OF ABRADABLE COATINGS ON SHAFT AND

BALANCE PISTON SEALS:

Application of an abradable coating to shaft and balance piston seal segments reduces
the effective clearance between members of the seal system, thereby creating a soft
clearance. Without the abradable coating, the effect is an in-creased hard clearance
between the components continuously automated applications.

30
 FUNCTION OF ABRADABLE SEALS ON SHROUDED ROTOR AND
STATIONARY BLADES:

Abradable coatings are also applied in the labyrinths that seal the steam path over
shrouded blades. The abradable is applied to both the turbine casing to provide
sealing of the rotor blades and to the shroud tips of the stationary blades to provide
sealing against the rotor.

Casin
g Abradable coating

Non cutting seal

strips
Blade shroud fins

Abradable
coating
Cutting seal
strips Rotor Rotor blasde

Figure 3.3: Function of abradable seals on shrouded rotor and stationary blades

31
 Figure 3.4:
A. Abradable coating applied to the outer steam path seals on the casing.
B. Abradable coating applied to the inner steam path seals on the shrouds of the
stationary blades.

ABRADABLE MATERIALS TECHNOLOGY:

Coatings applied in steam turbine sealing applications are deposited as a coating

system consisting of an oxidation-resistant bond coat and an abradable top coat. In
order to function properly in a high pressure steam environment, both coatings need
to resist steam oxidation for extended periods of time.

The bond coat is carefully chosen to minimize thermal expan-sion mismatch between
the abradable top coat and the base material while enhancing coating bond strength. It
also acts as an oxidation resistant barrier layer. Within the abradable top coat, the
metallic matrix phase provides structural integri-ty while the filler phase enhances
abradability. Controlled po-rosity levels within the top coat also serve to enhance
abrad-ability and can be adjusted for differences in application.

II. COMMON CERAMIC COATINGS

Today a variety of materials, e.g., carbides, oxides etc., belonging to the above
category are available commercially.
(i) Carbides: WC, TiC, SiC, ZrC, Cr2C3 etc.
(ii) Oxides: Al2O3, Cr2O3, TiO2, ZrO2 etc.
The choice of a material depends on the application. However, the ceramic coatings
are very hard and hence on an average offer more abrasion resistance than their
metallic counterparts.

CARBIDE COATINGS:

Amongst carbides, WC is very popular for wear and corrosion applications[10]. The
WC powders are clad with a cobalt layer. During spraying the cobalt layer undergoes
melting and upon solidification form a metallic matrix in which the hard WC particles
remain embedded. Spraying of WC-Co involves a close control of the process
parameters such that only the cobalt phase melts without degrading the WC particles.
Such degradation may occur in two ways:

Oxidation of WC leading to the formation of CoWO4 and WC2.

Dissolution of WC in the cobalt matrix leading to a formation of brittle phases like
CoW3C which embrittles the coating.

An increase in the spraying distance and associated increase of time in flight lead to a
loss of carbon and a pickup of oxygen. As a result the hardness of the coating
decreases. An increase in plasma gas flow rate reduces the dwell time and hence can
control the oxidation to some extent. However, it increases the possibility of cobalt

32
dissolution in the matrix[11]. The other option to improve the quality of such coating
is to conduct the spraying procedure in vacuum.

Often carbides like TiC, TaC and NbC are provided along with WC in the cermet to
improve upon the oxidation resistance, hardness, and hot strength. Similarly the
binder phase is also modified by adding chromium and nickel with cobalt. The wear
mechanism of plasma sprayed WC-Co coatings depends on a number of factors, e.g.,
mechanical properties, cobalt content, experimental conditions, mating surfaces, etc.
The wear mode can be abrasive, [12]adhesive or surface fatigue. The coefficient of
friction of WC-Co (in self mated condition) increases with increasing cobalt content.
A WC-Co coating when tested at a temperature of 450C exhibits signs of melting.
The wear resistance of these coatings also depends on porosity. Pores can also act as
source from where the cracks may grow. Thermal diffusivity of the coatings is another
important factor. In narrow contact regions, an excessive heat generation may occur
owing to rubbing. If the thermal diffusivity of the coating is low the heat cannot
escape from a narrow region easily resulting a rise in temperature and thus failure
occurs owing to thermal stress. The wear mechanism of WC-Co nano-composite
coating on mild steel substrates has been studied in details[13,14]. The wear rates of
such coatings are found to be much greater than that of commercial WC-Co
composite coating, presumably owing to an enhanced decomposition of nano-particles
during spraying. Wear has been found to occur by subsurface cracking along the
preferred crack paths provided by the binder phase or failure at the inter-splat
boundary. Coatings of TiC or TiC+ TaC with a nickel cladding are alternative
solutions for wear and corrosion problems. High temperature stability, low coefficient
of thermal expansion, high hardness and low specific gravity of these coatings may
outperform other materials, especially in steam environment. Instead of nickel, nickel
chromium alloy can serve as the matrix material. The mode of wear can be adhesive,
abrasive, surface fatigue or micro-fracture depending on operating conditions[15,16].

OXIDE COATINGS:

Metallic coatings and metal containing carbide coatings sometime are not suitable in
high temperature environments in both wear and corrosion applications. Often they
fail owing to oxidation or decarburization. In such case the material of choice can be
an oxide ceramic coating, e.g., Al2O3.Cr2O3, TiO2, ZrO2 or their combinations.
However, a high wear resistance, and chemical and thermal stability of these materials
are counterbalanced by the disadvantages of low values of thermal expansion
coefficient, thermal conductivity, mechanical strength, fracture toughness and
somewhat weaker adhesion to substrate material. The thickness of these coatings is
also limited by the residual stress that grows with thickness. Therefore, to obtain a
good quality coating it is essential to exercise proper choice of bond coat, spray
parameters and reinforcing additives.

CHROMIA (CR2O3) COATINGS:

These coatings are applied when corrosion resistance is required in addition to

abrasion resistance. It adheres well to the substrate and shows an exceptionally high

33
hardness 2300 HV 0.5 kg[17,18]. Chromia coatings are also useful in ship and other
diesel engines, water pumps, and printing rolls. A Cr2O3- 40 wt% TiO2 coating
provides a very high coefficient of friction (0.8), and hence can be used as a brake
liner. The wear mode of chromia coatings has been investigated under various
conditions. Depending on experimental conditions, the wear mode can be abrasive,
plastic deformation, micro-fracture or a conglomerate of all of these[19]. This
material has also been tested under lubricated conditions, using inorganic salt
solutions (NaCl, NaNO3, Na3PO4) as lubricants and also at a high temperature. The
wear rate of self-mated chromia is found to increase considerably at 450C, and
plastic deformation and surface fatigue are the predominant wear mechanisms. Under
lubricated condition, the coatings exhibit tribo-chemical wear. It has also been tested
for erosion resistance[20].

ZIRCONIA (ZRO2) COATINGS:

Zirconia is widely used as a thermal barrier coating. However, it is endowed with the
essential qualities of a wear resistant material, i.e., hardness, chemical inertness, etc.
and shows reasonably good wear behaviour. In the case of a hot pressed zirconia
mated with high chromium containing iron (martensitic, austenitic, or pearlitic), it has
been found that in course of rubbing the iron transfers on to the ceramic surface and
the austenitic material adheres well to the ceramic as compared to their martensitic or
pearlitic counterparts[21]. The thick film improves the heat transfer from the contact
area keeping the contact temperature reasonably low; thus the transformation of ZrO2
is prevented. On the other hand with the pearlitic or martensitic iron the material
transfer is limited. The contact temperature is high enough to bring about a phase
transformation and related volume change in ZrO2 causing a stress induced spalling.
In a similar experiment the wear behaviour of sintered, partially stabilized zirconia
(PSZ) with 8 wt% yttria against PSZ and steels has been tested at 200C. When
metals are used as the mating surface, a transferred layer soon forms on the ceramic
surface (coated or sintered). In ceramic-ceramic system the contact wear is abrasive in
nature. However, similar worn particles remain entrapped between the contact
surfaces and induce a polishing wear too. In the load range of 10 to 40 N, no
transformation of ZrO2 occurs. However, similar tests conducted at 800C show a
phase transformation from monoclinic ZrO2 to tetragonal ZrO2. The wear debris of
ZrO2 sometimes get compacted in repeated loading and gets attached to the worn
surface forming a protective layer. During rubbing, pre-existing or newly formed
cracks may grow rapidly and eventually interconnect with each other, leading to a
spallation of the coating. Introduction of alumina as a dopant, has been found to
improve the wear performance of the ceramic significantly. Here plastic deformation
is the main wear mode. The wear performance of zirconia at 400C and 600C has
been reported in the literature[22]. At these temperatures the adhesive mode of wear
plays the major role.

ALUMINA (AL2O3) - TITANIA (TIO2) COATINGS:

Titania coating is known for its high hardness, density, and adhesion strength. It has
been used to combat abrasive, erosive and fretting wear either in essentially pure form
or in association with other compounds. The mechanism of wear of TiO2 at 450C
under both lubricated and dry contact conditions has been studied[23,24] . It has been
found to undergo a plastic smearing under lubricated contact, where as it fails owing

34
to the surface fatigue in dry condition. TiO2-stainless steel couples in various speed
load conditions have also been investigated in details[25]. At a relatively low load, the
failure is owing to the surface fatigue and adhesive wear, whereas at a high load the
failure is attributed to the abrasion and delamination associated with a back and forth
movement. At a high speed, Fe3O4 forms instead of Fe2O3. The TiO2 top layer also
softens and melts owing to a steep rise in temperature, which helps in reducing the
temperature subsequently. The performance of the plasma sprayed pure TiO2 has been
compared with those of Al2O3 40 wt% TiO2 and pure Al2O3 under both dry and
lubricated contact conditions[26]. TiO2 shows the best results. TiO2 owing to its
relatively high porosity can provide good anchorage to the transferred film and also
can hold the lubricants effectively.

Alumina is obtained from a mineral called bauxite, which exists in nature as a number
of hydrated phases, e.g., boehmite (-Al2O3, H2O), hydragillate, diaspore (-Al2O3.
3H2O). It also exists in several other metastable forms like , , , , and X[27].
-Al2O3 is known to be a stable phase and it is available in nature in the form of
corundum. In addition, -Al2O3 can be extracted from the raw materials by fusing
them. The phase transformation during freezing of the plasma sprayed alumina
droplets has been studied in details[28,29]. There are several advantages of alumina as
a structural material, e.g., availability, hardness, high melting point, resistance to wear
and tear etc. It bonds well with the metallic substrates when applied as a coating on
them. Some of the applications of alumina are in bearings, valves, pump seals,
plungers, engine components, rocket nozzles, shields for guided missiles, vacuum
tube envelops, integrated circuits, etc. Plasma sprayed alumina-coated railroad
components are presently being used in Japan[30].

Properties of alumina can be further complemented by the particulate (TiO2, TiC) or

whisker (SiC) reinforcement. TiC reinforcement limits the grain growth, improves
strength and hardness, and also retards crack propagation through the alumina matrix.
The sliding wear behaviour of both monolithic and SiC whisker reinforced alumina
has been studied[31]. The whisker reinforced composite has been found to have good
wear resistance. The monolithic alumina has a brittle response to sliding wear,
whereas the worn surface of the composite reveals signs of plastic deformation along
with fracture. The whiskers also undergo pullout or fracture.
TiO2 is a commonly used additive in plasma sprayable alumina powder. TiO2 , has a
relatively low melting point and it effectively binds the alumina grains. However, a
success of an Al2O3 - TiO2 coating depends upon a judicious selection of the arc
current, which can melt the powders effectively. This results in a good coating
adhesion along with high wear resistance[32]. The wear performance of Al2O3 and
Al2O3 -50 wt% TiO2 has been reported in the literature[33]. In dry sand abrasion
testing, alumina outperformed others presumably owing to its high hardness . In dry
sliding at low velocity range, the tribocouple (ceramic and hardened stainless steel)
exhibits stick-slip[34]. At relatively high speed range, the coefficient of friction drops
owing to the thermal softening of the interface. The wear of alumina is found to
increase appreciably beyond a critical speed and a critical load. Alumina has been
found to fail by plastic deformation, shear and grain pullout. In dry and lubricated
sliding as well, the mixed ceramic has been found to perform better than pure
alumina.

A coating of Al2O3 -50 wt% TiO2 is quite porous and hence is quite capable of

35
holding the transferred metallic layer which protects the surface. Wear performance of
such coatings can further be improved by a sealing of the pores by polymeric
substances. A low thermal diffusivity of the alumina coatings results in a high
localized thermal stress on the surface. The mode of wear of alumina is mainly
abrasive. The pore size and pore size distribution also play a vital role in determining
the wear properties. The Al2O3 - TiO2 coating has a high thermal diffusivity and
hence it is less prone to wear.

III. MATERIALS

SAMPLE: The samples over which coatings are done is a super alloy.

COATING MATERIAL:

Bond Coat: AMDRY 956, Ni-Cr-Al-Y alloy powder for plasma thermal spray
application. The particle size of the powder is -106 +53 microns. The composition
of the powder is as follows: Ni 22Cr 10Al 1.0Y.

Top coat: Metco 601NS, CoNiCrAlY with polyester and BN. The particle size of
the powder used is- 176 +11 microns. The composition of the Metco 2043 is as
follows: Co 25Ni 16Cr 6Al 0.3Y 4BN 15 Polyester.

Boron nitride provides solid lubrication for an improved abradability and polyester
component is introduced to achieve the high porosity level desired for abradable
purpose.

IV. PLASMA SPRAYING PROCEDURE

THERMAL SPRAYING OF ABRADABLE PLASMA COATING:

In the present work the abradable coating is done by thermal spraying technique using
an 80 KW plasma spray system with a Sulzer Metco 9 MB gun. The spray parameters
are given below. Thickness measurement during coating process was done using
electromagnetic induction based gauge Elcometer 456.

Process parameters that were kept constant during the trials are as follows:
Plasma Gun: 9 MB
Primary gas as Ar: 100 FMR
Secondary Gas H2: 10 FMR
Arc Current: 475 Amps

Bond Coat:

Parameter Operating Range

Current 475 A DC
Voltage 55 V DC
Primary Plasmagen gas (Argon) flow rate 100 scfn
Secondary Plasmagen gas (Helium) Flow rate 7 scfn

36
 Nozzle to substrate distance (Stand-off distance) 125 mm
Scan speed 300 mm/s
Powder rpm 4

Thickness after 4 passes = ~60m (~15m/pass)

Thickness after another 4 passes with powder rpm 6 = ~90m (~m/pass)
Thickness after another 4 passes with powder rpm 6 = ~m (~m/pass)
Total thickness = 130m

Top Coat:

Parameter Operating Range

Current 450 A DC
Voltage 55 V DC
Primary Plasmagen gas (Argon) flow rate <100
Secondary Plasmagen gas (Helium) Flow rate <8
Nozzle to substrate distance (Stand-off distance) 50 mm
Scan speed 500 mm/s
Powder rpm 6

After 6 passes thickness = 360-390m

Net thickness = 230-250m

37
Figure.3.5: View of the plasma spraying unit

Figure.3.6: Pictorial view of plasma sprayed coating samples

V. CHARACTERIZATION
1. POROSITY AND MICROSTRUCTURE

The steps involved in determining porosity of sample are as follows:

Cross Sectioning Of The Sample:

Operation:

The work piece is fastened in a holder mounted on a movable arm. This arm acts as a
steel yard with two weights, one of which balances the specimen holder with
specimen, the other being used to set the exact cutting pressure. During the cutting
operation the arm is guided down over the cut-off wheel. When the cutting operation
is finished the cut-off wheel stops and the specimen falls into a basket in the cool ant
tank thus protecting the specimen from drying and making retrieval easy.

38
Figure3.7: Struers Minitom low speed cutting machine.

Hot Mounting:

Mounting of specimens is usually necessary to allow them to be handled easily. It also

minimizes the amount of damage likely to be caused to the specimen itself.

The mounting operation accomplishes three important functions:

It protects the specimen edge and maintains the integrity of a materials surface
features
Fills voids in porous materials and
Improves handling of irregular shaped samples, especially for automated
specimen preparation.

Grinding:

Surface layers damaged by cutting must be removed by grinding. Mounted specimens

are ground with rotating discs of abrasive paper flushed with a suitable coolant to
remove debris and heat, for example wet silicon carbide paper. The coarseness of the
paper is indicated by a number: the number of grains of silicon carbide per square
inch. So, for example, 180 grit paper is coarser than 1200.

The grinding procedure involves several stages, using a finer paper (higher number)
for each successive stage. Each grinding stage removes the scratches from the
previous coarser paper. This is more easily achieved by orienting the specimen
perpendicular to the previous scratches, and watching for these previously oriented
scratches to be obliterated. Between each grade the specimen is washed thoroughly
with soapy water to prevent contamination from coarser grit present on the specimen
surface. Typically, the finest grade of paper used is the 1200, and once the only

39
scratches left on the specimen are from this grade, the specimen is thoroughly washed
with water, followed by alcohol and then allowed to dry.

Polishing:

Polishing discs are covered with soft cloth impregnated with abrasive diamond
particles and an oily lubricant. Particles of two different grades are used : a coarser
polish - typically with diamond particles 6 microns in diameter which should remove
the scratches produced from the finest grinding stage, and a finer polish typically
with diamond particles 1 micron in diameter, to produce a smooth surface. Before
using a finer polishing wheel the specimen should be washed thoroughly with warm
soapy water followed by alcohol to prevent contamination of the disc.

Etching:

Etching is used to reveal the microstructure of the metal through selective chemical
attack. It also removes the thin, highly deformed layer introduced during grinding
and polishing.

In alloys with more than one phase, etching creates contrast between different regions
through differences in topography or reflectivity. The rate of etching is affected by
crystallographic orientation, the phase present and the stability of the region. This
means contrast may arise through different mechanisms therefore revealing different
features of the sample.

Ideally the surface to be examined optically should be flat and level. If it is not, the
image will pass in and out of focus as the viewing area is moved across the surface. In
addition, it will make it difficult to have the whole of the field of view in focus - while
the centre is focused, the sides will be out of focus. By using a specimen leveling
press (shown below) this problem can be avoided, as it presses the mounted specimen
into plasticize on a microscope slide, making it level. A small piece of paper or cloth
covers the surface of the specimen to avoid scratching.

2. BOND STRENGTH

In accordance with ASTM D4541-95 and ISO 4624, the PosiTest Pull-Off Adhesion
Tester evaluates the adhesion (pull-off strength) of a coating by determining the
greatest tensile pull off force that it can bear before detaching. Breaking points,
demonstrated by fractured surfaces, occur along the weakest plane within the system
consisting of the dolly, adhesive, coating layers and substrate.

Pull Off Tester Theory Of Operation:

Portable pull-off adhesion testers measure the force required to pull a specified
diameter of coating away from its substrate. This measured pull-off force provides a
direct indication of the strength of adhesion between the coating and the substrate. By
eliminating sources of pull-off variation, such as unintended bond failures between
the adhesive and poorly prepared dollies, adhesion test results become even more
meaningful and predictable.

40
The major components of a pull-off adhesion tester are a pressure source, a pressure
gage and an actuator. During operation, the flat face of a pull stub (dolly) is adhered
to the coating to be evaluated. After allowing for the bonding adhesive to cure, a
coupling connector from the actuator is attached to the dolly. By activating the
pressure source, pressure is slowly increased to the actuator within the system. When
the pressure in the actuator becomes larger than the bond strength between the coating
and the substrate, separation occurs and the actuator-dolly assembly lifts the coating
from the substrate (refer to Figure5.1). The maximum pressure indicator of the
systems pressure gauge provides a direct reading of the pressure at which the pull-off
occurred.

Figure 3.8: Positest pull-off adhesion tester

Dolly And Surface Preparation:

Dolly preparation:

To remove oxidation and contaminants, place the included abrasive pad on a flat
surface and rub the base of the dolly across the pad 4-5 times.
As required, remove residue left from the abrading process using a dry cloth or
paper towel.

Coating surface preparation:

Lightly roughen the coating using the included abrasive pad.

To promote the bond between the dolly and the coating, degrease the area of the
coating to be tested using alcohol or acetone to remove any oil, moisture or dust.

41
Pull Testing:

The bond strength was measured as per ASTM D4541 using Positest pull-off adhesion
tester and a dolly of 20 mm diameter. The dolly was glued to the sample using HTK
Ultra Bond 100 adhesive, cured in the oven at 120 degrees Celsius for 120 minutes
and air cooled for at least 6 hours.

3. HARDNESS MEASUREMENTS AS PER HR15Y

Rockwell Hardness Test Theory:

The Rockwell Superficial hardness test method consists of indenting the test material
with a diamond cone (N scale) or hardened steel ball indenter. The indenter is forced
into the test material under a preliminary minor load F0 usually 3 kgf. When
equilibrium has been reached, an indicating device that follows the movements of the
indenter and so responds to changes in depth of penetration of the indenter is set to a
datum position. While the preliminary minor load is still applied an additional major
load, is applied with resulting increase in penetration. When equilibrium has again
been reach, the additional major load is removed but the preliminary minor load is
still maintained. Removal of the additional major load allows a partial recovery, so
reducing the depth of penetration. The permanent increase in depth of penetration, e,
resulting from the application and removal of the additional major load is used to
calculate the Rockwell Superficial hardness number.

HR = E - e

F0 = preliminary minor load in kgf

F1 = additional major load in kgf
F = total load in kgf
e = permanent increase in depth of penetration due to major load F1, measured in
units of 0.001 mm
E = a constant of 100 units for diamond and ball indenters
HR = Rockwell hardness number
D = diameter of steel ball

Figure 3.9: Rockwell superficial principle.

42
Rockwell superficial scales are used to test materials too thin or small for the regular
scales or outside the regular ranges. Generally Diamond Indenters are used for hard
materials while Ball Indenters are used on soft materials. The HR 15 N scale is useful
for testing hard thermal spray coatings like ceramics and carbides, while at the other
extreme the HR 15 Y scale is used to test very soft abradable coatings.

Figure 3.10:
Rockwell
hardness
tester

CHAPTER-4

43
 RESULTS AND
DISCUSSION

CHAPTER 4

RESULTS AND DISCUSSION

I. POROSITY AND MICROSTRUCTURE

The metallographic examination of the coated sample was done after cross sectioning
on a Struers Minitom low speed cutting machine using diamond cutting wheel and
subsequently hot mounting using Bakelite. The sample was diamond ground and
polished to 0.5 micron.

44
Figure 4.1: Optical image at 50X showing uniform porosity.

The porosity of the coating after heat treatment was in the range of 50%.

II. BOND STRENGTH

The bond strength was measured as per ASTM D4541 using Positest pull-off adhesion
tester and a dolly of 20 mm diameter. The dolly was glued to the sample using HTK
Ultra Bond 100 adhesive, cured in the oven at 120 degrees Celsius for 120 minutes
and air cooled for at least 6 hours.

Bond strength values obtained were in between 2500 psi to 3000 psi.

III. HARDNESS MEASUREMENTS AS PER HR15Y

Abradable coatings are comparatively softer and the hardness of abradable coatings is
measured using Rockwell superficial hardness on HR15Y scale, which uses a 12.7
mm carbide ball as indenter and hence the hardness measurements are not taken on
the cross sectioned samples; rather hardness is done directly on top of the coated base
metal sample. For this purpose the coating thickness is kept around
2 mm.

The overall average hardness measured was in the range of 60 to 70 on HR15Y scale.

45
CHAPTER-5

46
 CONCLUSIONS

CHAPTER 5

CONCLUSIONS

Thermal spray abradable coatings play a major role in the operating efficiency of
turbo machinery. Abradable coatings can be tailored to provide the required clearance
control, depending on the base material as well as the location of the coated
component in the turbines.

In steam turbines, abradable coatings should be applied to shaft seals, balance piston
seals and seals over shrouded blades. Application to all of these areas ensures a
complete solution that will maximize efficiency gains by reducing leakage flows
through labyrinths.

47
 The bond coat is carefully chosen to minimize thermal expansion mismatch between
the abradable top coat and the base material while enhancing coating bond strength.
Within the abradable top coat, the metallic matrix phase provides structural integrity
while the filler phase enhances abradability. Controlled porosity levels within the top
coat also serve to enhance abradability and can be adjusted for differences in
application.

Plasma spray coating is an economical and effective method applied to various

machine parts to reduce the surface degradation. It is gaining importance in many
critical areas of application due to the fact that it provides increased design flexibility
and its high deposition rate, so that the parts made up from a combination of materials
with widely differing physical and chemical properties could be employed.

The porosity of the coating after heat treatment was in the range of 50%.

Bond strength values obtained were in between 2500 psi to 3000 psi.

The overall average hardness measured was in the range of 60 to 70 on HR15Y scale.

Applying abradable sealing technology to steam turbines results in increased power

output and efficiency, or reduced fuel consumption. Both scenarios result in reduced
CO2 emissions, and in the case of coal-fired and oil-fired plants, reduced SO2
emissions.

References:

1. Dieter Sporer, Scott Wilson, Mitchell Dorfman. Ceramics for abradable shrouds
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