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    SYNTHESIS AND CHARACTERIZATION OF NEW

    ALUMINIUM ALLOY WITH MWCNT COATED

    WITH NI-P ELECTROLEES COATING

    A PROJECT REPORT

    Submitted by

    T.SAKTHIVEL (84509144037)

    R.SATHISH (84509144039)

    S.SELVAKUMAR (84509144040)

    U.MUJEPER RAHMAN (84509144505)

    In partial fulfillment for the award of the degree

    of

    BACHELOR OF ENGINEERING

    IN

    MECHANICAL ENGINEERING

    IMAYAM COLLEGE OF ENGINEERING KANNANUR-621206

    ANNA UNIVERSITY: CHENNAI 600025

    MAY 2013

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    BONAFIDE CERTIFICATE

    Certified that this project report SYNTHESIS AND CHARACTERISATION

    OF NEW ALUMINIUM ALLOY WITH MWCNT COATED WITH Ni-P is

    the bonafide work of S.SELVAKUMAR who carried out the project work

    under my supervision.

    SIGNATURE SIGNATURE

    Mr.C.Francis vimalraj. M.Tech., Mr.A.Thiagarajan. M.Tech.,

    HEAD OF THE DEPARTMENT GUIDED BY

    Mechanical department Mechanical department

    Imayam College of engineering Imayam College of engineering

    Kannanur-621206 Kannanur-621206

    Submitted for Anna University viva-voce examination held on ___________

    INTERNAL EXAMINER EXTERNAL EXAMINER

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    ACKNOWLEDGEMENT

    We express our sincere gratitude to Dr.R.Nallusamy. Ph.D., Principal of

    Imayam College of Engineering, Kannanur, Thuraiyur. who gave us the

    opportunity to frame the project to the fullest satisfaction.

    We are extremely grateful to Mr.C.Francis vimalraj. M.Tech,Head of the

    Department of Mechanical Engineering who have been instrumental in guiding

    us, with their valuable suggestions.

    We express our hearty thanks to our supervisor Mr.A.Thiagarajan.

    M.Tech, Department of Mechanical Engineering for his valuable guidance and

    encouragement for the successful completion of this project.

    We would like to express our deep sense of thanks to the entire faculty of

    Mechanical Engineering Department and to all our friends.

    We express our soulful thanks to our dear parents who have been the major

    contributor of inspiration and encouragement to us throughout our project.

    We thank God Almighty for his blessings without which we would have not

    initiated the project.

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    ABSTRACT

    Nanotechnology draws its attention in the current world scenario. Physical

    and chemical properties of materials are tends to changes at nano scale. Among

    various forms of nano materials, carbon nanotube earns a rightful place in the field

    of nanotechnology. Carbon nanotubes are posses excellent electrical properties due

    to its high aspect ratio i.e., length to diameter, typically 103 to 104. Current work

    deals with the synthesis and characterization of aluminium alloy. Reinforced with

    carbon nanotubes are used for the work.

    Aluminium has been widely in aerospace and terrestrial system, more and

    more attention has been paid for expanding the market of its alloy in automotive

    industries and decrease of energy consumption of vehicles. In this proposed project

    work, it is planned to prepare al-al2 o3 alloys using multi wall carbon nano tube.

    After preparation of alloy the material will be tested to evaluate the mechanical

    properties. Nanotubes are dispersed in aluminium alloy, thus prepared are tested to

    increase the mechanical properties and then characterized using XRD and SEM.

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    TABLE OF CONTENTS

    CHAPTER NO. TITLE PAGE NO.

    ABSTRACT i

    LIST OF TABLE v

    LIST OF FIGURE iv

    1 INTRODUCTION

    1.1 Aluminium Alloys 1

    1.2 Advantages 3

    1.3 Applications 3

    2 LITERATURE REVIEW

    2.1 Aluminium Alloy 5

    2.2 Carbon nanotubes 6

    3 POWDER METALLURGY

    3.1 Powder metallurgy 13

    3.2 Advantages 13

    3.3 Procedures 14

    3.3.1 Blending 14

    3.3.2 Compaction 15

    3.3.3 Sintering 17

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    4 EXPERIMENTAL PROCEDURE

    4.1 Compaction Process 19

    4.2 Sintering 24

    4.3 Ni-P Coating 25

    4.3.1 Electroless nickel coating 26

    4.3.2 Electroless Ni-P coating 28

    4.4 Experimental Setup 31

    4.4.1 Electroless Plating Bath 31

    5 CHRACTERIZATION

    5.1 Hardness Test 37

    5.1.1 Rockwell Hardness Test 38

    5.1.2 Vicker Hardness Test

    5.2 Wear 44

    5.3 Compressive Strength

    5.4 Scanning Electron Microscope

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    LIST OF FIGURES

    S.No. FIGURES PAGE NO.

    1 Carbon nanotube structure and helicity 8

    2 Schematic diagram of arc-discharge method 9

    3 Powder metallurgy process 16

    4 Sintering furnace 17

    5 Die 20

    6 Weighing machine 21

    7 Mixing of powder 22

    8 Compression 23

    9 Muffle furnace 24

    10 Scanning electron microscope 33

    11 Internal structure of SEM 35

    12 Rockwell hardness 39

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    LIST OF TABLE

    S.NO DESCRIPTION PAGE NO.

    1 Composition Of Samples 21

    2 Rockwell hardness test 41

    3 Compressive strength 42

    4 composition of chemicals 30

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    INTRODUCTION

    1.1 ALUMINIUM ALLOY

    From Wikipedia, the free encyclopedia

    Cast aluminium alloy rear wheel of Bootie Folding Bicycle

    We see Aluminium used around us everywhere. From aluminium windows

    oraluminium doors you find in your house, to aluminium foil your mom packs

    your sandwiches in, and the decorative aluminium adorning your (thats right)

    aluminium windows; aluminium is widely used in a majority of situations around

    the house. What you probably didnt know that aluminium is an ideal choice in

    several key industries.

    In fact, aluminium is the third most common element in the Earth's crust,

    making it the most abundantly available metal on Earth. Being extremely

    lightweight, aluminium can be used to make lightweight, yet very durable alloys.

    Apart from that, aluminium is a non-magnetic material, making it ideal in some

    industrial uses. It also conducts both heat and electricity nearly as good as copper

    does.

    http://www.tradekey.com/ks-aluminumhttp://www.tradekey.com/ks-aluminum-windowhttp://www.tradekey.com/ks-aluminum-doorhttp://www.tradekey.com/ks-aluminum-foilhttp://www.tradekey.com/ks-aluminum-windowhttp://www.tradekey.com/ks-aluminumhttp://www.tradekey.com/ks-aluminumhttp://www.tradekey.com/ks-aluminumhttp://www.tradekey.com/ks-aluminumhttp://en.wikipedia.org/wiki/File:Bootie_bicycle_3_bootiebike.JPGhttp://en.wikipedia.org/wiki/File:Bootie_bicycle_3_bootiebike.JPGhttp://www.tradekey.com/ks-aluminum-windowhttp://www.tradekey.com/ks-aluminum-doorhttp://www.tradekey.com/ks-aluminum-foilhttp://www.tradekey.com/ks-aluminum-windowhttp://www.tradekey.com/ks-aluminumhttp://www.tradekey.com/ks-aluminumhttp://www.tradekey.com/ks-aluminumhttp://www.tradekey.com/ks-aluminumhttp://www.tradekey.com/ks-aluminum
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    Aluminiumalloys are alloys in which aluminium (Al) is the predominant

    metal. The typical alloying elements

    are copper, magnesium, manganese, silicon and zinc. There are two principal

    classifications, namely casting alloys and wrought alloys, both of which are further

    subdivided into the categories heat - treatable and non-heat-treatable. About 85% of

    aluminium is used for wrought products, for example rolled plate, foils

    and extrusions. Cast aluminium alloys yield cost-effective products due to the low

    melting point, although they generally have lowertensile strengths than wrought

    alloys. The most important cast aluminium alloy system is Al-Si, where the high

    levels of silicon (4.0% to 13%) contribute to give good casting characteristics.

    Aluminium alloys are widely used in engineering structures and components where

    light weight or corrosion resistance is required.[1]

    Alloys composed mostly of aluminium have been very important

    in aerospace manufacturing since the introduction of metal skinned aircraft.

    Aluminium-magnesium alloys are both lighter than other aluminium alloys and

    much less flammable than alloys that contain a very high percentage of

    magnesium.[2]

    Aluminium alloy surfaces will keep their apparent shine in a dry

    environment due to the formation of a clear, protective layer of aluminium oxide.

    In a wet environment, galvanic corrosion can occur when an aluminium alloy is

    placed in electrical contact with other metals with more negative corrosion

    potentials than aluminium.

    Aluminium alloy compositions are registered with The Aluminium

    Association. Many organizations publish more specific standards for the

    manufacture of aluminium alloy, including the Society of Automotive

    Engineers standards organization, specifically its aerospace standards subgroups.

    http://en.wikipedia.org/wiki/Alloyshttp://en.wikipedia.org/wiki/Aluminiumhttp://en.wikipedia.org/wiki/Copperhttp://en.wikipedia.org/wiki/Magnesiumhttp://en.wikipedia.org/wiki/Manganesehttp://en.wikipedia.org/wiki/Siliconhttp://en.wikipedia.org/wiki/Zinchttp://en.wikipedia.org/wiki/Castinghttp://en.wikipedia.org/wiki/Heat_treatmenthttp://en.wikipedia.org/wiki/Extrudinghttp://en.wikipedia.org/wiki/Tensile_strengthhttp://en.wikipedia.org/wiki/Aluminium_alloy#cite_note-ReferenceA-1http://en.wikipedia.org/wiki/Aerospace_manufacturinghttp://en.wikipedia.org/wiki/Aluminium_alloy#cite_note-2http://en.wikipedia.org/wiki/Aluminium_oxidehttp://en.wikipedia.org/wiki/Galvanic_corrosionhttp://en.wikipedia.org/wiki/The_Aluminum_Associationhttp://en.wikipedia.org/wiki/The_Aluminum_Associationhttp://en.wikipedia.org/wiki/Society_of_Automotive_Engineershttp://en.wikipedia.org/wiki/Society_of_Automotive_Engineershttp://en.wikipedia.org/wiki/Alloyshttp://en.wikipedia.org/wiki/Aluminiumhttp://en.wikipedia.org/wiki/Copperhttp://en.wikipedia.org/wiki/Magnesiumhttp://en.wikipedia.org/wiki/Manganesehttp://en.wikipedia.org/wiki/Siliconhttp://en.wikipedia.org/wiki/Zinchttp://en.wikipedia.org/wiki/Castinghttp://en.wikipedia.org/wiki/Heat_treatmenthttp://en.wikipedia.org/wiki/Extrudinghttp://en.wikipedia.org/wiki/Tensile_strengthhttp://en.wikipedia.org/wiki/Aluminium_alloy#cite_note-ReferenceA-1http://en.wikipedia.org/wiki/Aerospace_manufacturinghttp://en.wikipedia.org/wiki/Aluminium_alloy#cite_note-2http://en.wikipedia.org/wiki/Aluminium_oxidehttp://en.wikipedia.org/wiki/Galvanic_corrosionhttp://en.wikipedia.org/wiki/The_Aluminum_Associationhttp://en.wikipedia.org/wiki/The_Aluminum_Associationhttp://en.wikipedia.org/wiki/Society_of_Automotive_Engineershttp://en.wikipedia.org/wiki/Society_of_Automotive_Engineers
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    1.2 ADVANTAGES

    Low cost

    High strength

    Light weight

    Corrosion resistance

    Good electrical conductivity

    Ductility

    Durability

    Thermal conductivity

    1.3 APPLICATIONS

    Automobile

    Aerospace

    Electricity

    Home appliances

    Constructions

    Marine

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    1.4 PROPERTIES OF ALUMINIUM

    Density - 2.7 g/cm

    Melting point - 660 C

    Yield strength 7 to 11 Mpa

    Youngs modulus 70 Gpa

    Poisson ratio 0.35

    Non-magnetic material

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    LITERATURE SURVEY

    2.1 ALUMINIUM ALLOY

    Effect of composition on friction coefficient of Cu-aluminum composites,

    Jaroslav Kovacik, Stefan Emmer, Jozef Bielek, ubomir

    In this paper reveals that that with increasing concentration of aluminium

    with Cu, the coefficient of friction and wear rate decreased. However, in the case

    of low voltage and high current density, it is required to employ materials with a

    very high specific electrical conductivity, good thermal conductivity and low

    friction coefficient. Such conditions are fulfilled only by Cu-Aluminium composite

    materials

    Microstructure of Cu&Al2o3 surface composite on a copper substrate,

    Wenming Songa, b, Gui-rong Yang a, b,, Jin-jun Luc,

    In this paper reveals that the microstructure and hardness of the surface

    infiltrated composite (Cu/ Al2o3) layers produced on copper substrates. High

    electrical and heat conductive copper is widely used in optics, electrical contact

    and heat conducting materials. Their low strength and poor wear resistance are

    required to improve with the developing industry.

    Interfacial design of Cu-based composites prepared by powder metallurgy

    for heat sink applications Th. Schubert ,, B. Trindade , T. Weigarber , B.

    Kieback

    The use of SiC or diamonds particles as reinforcements in copper based

    composites is considered very attractive to meet the increasing demands for high

    performance heat sink materials and packages.

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    Wear and mechanical properties of sintered coppertin composites

    containi graphite or molybdenum disulfide Hirotaka Kato a,, Masahiro Takamaa,

    Yoshiro Iwai b, Kazuo Washida c, Yoshinori Sasaki c

    The lubricant graphite and MoS2 powders were coated with Cu to reinforce

    their bonding to the Cu particles in the composites during sintering. The friction

    and wear properties of the materials were improved

    Wear resistance of WC particle reinforced copper matrix composites, P.K.

    Deshpande, R.Y. Lin

    Tungsten, being a refractory metal, provides some degree of wear and arcing

    resistance when used with copper as an electrical contact material. Its wear

    resistance is better than that of wear-resisting tool steels. Tungsten carbide

    undergoes no phase changes during heating and cooling and retains its stability

    indefinitely.

    Study of wear mechanisms in copper-based Sic (20% by volume)

    reinforced composite, Dhokey a,, R.K. Paretkar b

    Copper-based composites appear to be a promising material for engineering

    applications due to their excellent thermo physical properties coupled with better

    high temperature mechanical properties as compared to pure copper.

    2.2 CARBON NANOTUBE

    Structure plays major role in determining its properties. The material under

    consideration, carbon nanotube is nothing but a rolled sheet of graphite. Graphite

    consists of layer of carbon atoms, within the layers the atoms are arranged at the

    corners of hexagon which fill the carbon plane. The carbon atoms are strongly

    (covalent) bonded to each other and carbon-carbon distance ~0.34mm.

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    Carbon nanotubes are considered to be a rolled single sheet of grapheme [1].

    Grapheme sheets are seamless cylinder derived from honeycomb lattice,

    representing a single atomic layer of crystalline graphite. Single walled carbon

    nanotubes are considered as a cylinder with only one graphene sheet. SWNT are

    completely described by a single vector C (chiral vector)

    C=na1+na2

    Where, n & m are integers, a1 & a2 are unit vectors. The direction of the nanotube

    axis is perpendicular to this chiral vector.

    Multi-walled carbon nanotubes are collection of concentric SENT. MWNT

    may be formed from coaxial cylindrical curved, coaxial polygonized or small

    graphite sheet [2]. The length of chiral vector C is the circumference of the

    nanotube and is given by the relation

    C=a (n2+nm+m2)

    In the case of SWNT, three types of nanotubes exist. They are classified by

    the pair of integers (n, m) which is related to chiral vector. (a) When n=m, the

    nanotube is called arm chair type ( =0 ). (b) When m=0 then it is of zigzag

    type ( =30 ) otherwise, (c) when n m, it is a chiral tubes and takes a value

    between 0 to 30 . The value of (n, m) determines chiralitys of nanotubes and

    affects the optical, mechanical and electronic properties.

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    Carbon Nanotube Structure

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    SYNTHESIS OF CARBON NANOTUBES

    ARC-DISCHARGE METHOD

    Carbon nanotubes were first reported by Sumio Lijima in the carbonaceous

    deposits on the cathode obtained during the DC arc discharge process of a graphite

    electrode in helium gas. The arc discharge method is still the only way to obtainhighly graphitized MWNTs without using metal catalyst.

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    Inert gas such as helium or argon, other ambient gas discharge has been

    extensively used to produce CNTs. Large quantities of CNTs has been produced by

    the presence of metal catalyst such as Ni, Co, Fe, S,Y etc,. In this method, arcing is

    carried out between a stationary anode and rotating cathode. Both the electrodes

    are made of graphite, but the densification differs. The cathode is rotated to

    maximize the yield of the CNT [3].

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    Arc is struck using a DC supply providing 100-150 A/cm2 current densities

    and 20-40 V. the power supply unit is an AC/DC inverter TIG power source.

    Graphite with diameter 11mm (99.7% purity) is used as anode for arcing. Arcing is

    carried out with a rotating graphite disc as counter electrode. A thick copper metal

    plate holds the graphite cathode disc. The cathode disc is rotated and the speed is

    maintained constant (5 rpm to 20 rpm) for each experiment.

    A servo motor feed the anode towards the cathode in order to maintain the

    electrode gap constant (1 mm). During arcing, soot is continuously deposited on

    cathode, which is continuously scraped off using thin blade. In this process

    chamber is operated in open air and without use of additional catalyst.

    PURIFICATION

    Carbon nanotubes produced by arc discharged method contains

    carbonaceous impurities commonly increases with decreases in diameter.

    Carbonaceous impurities include amorphous carbon, fullerenes. Fullerenes can be

    easily removed owing to their solubility in certain organic solvents. Amorphous

    carbon is also relatively easy to eliminate because of its high density of defects,

    which allow it to be oxidized under gentle condition [4].

    Purification methods of CNTs can be basically classified into three

    categories namely chemical, physical and a combination of both. The chemical

    method purifies CNTs based on the idea of selective oxidation where in

    carbonaceous impurities are oxidized at faster rate than CNT and the dissolution of

    metallic impurities by acids. The physical method separates CNTs from impurities

    based on the differences in their physical size, aspect ratio, gravity and magneTIC

    properties etc.

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    The crude deposit scraped from the cathode is crushed using a pestle and

    mortar to obtain fine powders. Then it is heated in open air in closed tubular

    furnace. The samples are oxidized at 550 for 2 hours. Then the tubes are washed

    in distilled water and Toluene so as to remove any water and organic soluble

    impurities. Then the tubes are ultrasonicated in acetone so that they are

    disagglomerated and subsequently dried in air [typically at 110 ] to drive away

    the moisture.

    PROPERTIES OF CNT

    CNT processes many useful and unique properties such as

    High electrical conductivity

    Very high tensile strength

    Very elastic 18% elongation to failure

    Highly flexible can be bent considerably without damage

    High thermal conductivity

    Low thermal co-efficient of expansion

    Highly absorbent

    High aspect ratio (length=1000*diameter)

    Light weight

    The strength of sp2 C-C bonds gives amazing mechanicals properties for

    nanotubes. The stiffness of materials measured terms of its Youngs modulus. The

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    Youngs modulus of CNYs can be as high as 1Tpa, which is approximately five

    times higher than steel. The Ultimate tensile strength of nanotubes can be up to 63

    Gpa, around 50 times than steel.

    Depending upon the structure, CNTs can be metallic or semi conducting.

    Some metallic CNTs have conductivity 1000 times greater than that of copper.

    Carbon nanotubes are very good thermal conductors along the tube axis. It will be

    able to transmit up to 6000Watts per meter per Kelvin at room temperature (Cu-

    385 Watts per meter per Kelvin). The temperature stability of CNT is estimated to

    be up to 2800 in vacuum and about 750 in air.

    POWDER METALLURGY

    Powder is a forming and fabrication technique consisting of three major

    stages. First the primary material is powdered, divided into many small individual

    particles. Next the powder is injected into a mold or passed through a die to

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    produce a weakly cohesive structure very near the dimensions of the object

    ultimately to be manufactured.

    Pressures of 10-50 tons per square inches are economically used. Also, to

    attain the same compression ratio across more complex pieces, it is often necessary

    to use lower punches as well as an upper punch. Finally the end part is formed by

    applying pressure, high temperature, long setting times or any combination thereof.

    Two main techniques used to form and consolidate the powder are sintering

    and metal injection molding. Recent developments have made it possible to use

    rabid manufacturing techniques which use the metal powder for products. Because

    with this technique the powder is melted, and not sintered better mechanical

    strength can be accomplished.

    3.1 ADVANTAGES OF POWDER METALLURGY

    1) No or only little amount of cutting and machining

    2) High utilization rate of materials, over 95%;

    3) Sizes of parts are consistent and stable;

    4) Materials can be adjusted according to customers requirements;

    5) Based on customers needs, surface parts are processed improving

    strength and hardness

    6) As for mass production, compared to machining, powder metallurgy high

    efficiency, low cost.

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    3.2 PROCEDURE TO BE CARRIED IN POWDER METALLURGY

    The steps involved in making aluminium alloy by powder metallurgy

    are

    Blending

    Compaction

    Sintering

    3.2.1 BLENDING

    Powders are to be blended or mixed properly for obtaining the required

    properties after sintering. In this process the powder and blender are mixed

    together very finely. A lubricant is also employed some times to reduce the friction

    and hence obtaining a finer mixing. The lubricant should be removed of the die

    before submitting it for sintering as the process of lubricant may change the

    properties of the object. Many types of blends are used for the manufacturing of

    various parts by powder metallurgy technique.

    The metal powder is mixed with lubricant and optional alloying elements to

    form a homogeneous blend. 0.5-1.5% lubricant is normally added in the mix, and

    metallic sterrate and waxes are commonly used lubricants. The main function of

    lubricant is to reduce the friction between the powder mass and the surfaces of the

    tool, die walls, core rods etc

    This assists the achievement of uniform density from top to bottom of the

    compact of equal importance is the fact that the reduction of friction also makes it

    easier to eject the compact. As an alternative to pre alloyed powders, alloying

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    elements can be added the mix powders. The most commonly used alloying

    element is carbon, which is added as graphite powder.

    3.2.2 COMPACTION

    Compacting is done for shaping of the powder in to the required shape. In

    this the mixed mixer is subjected to pressure and due to the application of pressure

    the gap between the molecules gets reduced and the powder becomes compact and

    gains sufficient strength to with stand ejection and handling.

    Pressures applied on the powder should be strictly regulated as if low

    pressures then the part generated will be very fragile in nature. If the pressure

    applied is more then there may be a deformation of tool. In general a pressure of 1

    to 150 nm2

    Simply this method used to make a shaped specimen like a cake and it will

    be easily brokened by hands when heating then the specimen will become stronger.

    The following figure explains the working methodology of the compaction

    process

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    3.2.3 SINTERING

    DEFINITION

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    The thermal treatment of a powder is compact at a temperature below the

    melting point of the main constituent, for the purpose of increasing its strength by

    bonding together.

    SINTERING ATMOSPHERES

    The operation is almost invariably carried out under a protective atmosphere,

    because of the large surface areas involved, and at temperatures between 60 and

    90% of the melting-point of the particular metal or alloys.

    SINTERING FURNACE

    Control over heating rate, time, temperature and atmosphere is required for

    reproducible results. The type of furnace most generally favored is an electrically

    heated one through which the compacts are passed on a woven wire mesh belt. The

    belt and the heating elements are of a modified 80/20 Nickel/chromium alloy and

    give a useful life a temperature up to 1150 . For higher temperatures walking

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    beam furnaces are preferred, and these are increasingly being used as the demand

    for higher strength in sintered parts increases. Silicon carbide heating elements are

    used can be operated up to 1350 . For a special purposes at still higher

    temperature molybdenum heating elements can be used, but special problems are

    involved, notably the readiness with which molybdenum forms a volatile oxide.

    Molybdenum furnaces must operate in a pure hydrogen atmosphere. This process

    is carried out for increasing the strength and also the hardness of the part. In this

    part is subjected to heating without any pressure for certain period of time under

    highly controlled conditions.

    Sintering is concerned with

    a. Diffusion

    b. Densification

    c. Recrystallization and grain growth

    EXPERIMENTAL PROCEDURE

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    EXPERIMENTAL PROCEDURE IN POWDER COMPACTION AND

    SINTERING

    4.1 COMPACTION PROCESS

    AIM

    To compact the powder in certain composition by using micro controlled

    compression machine.

    POWDER USED

    1. ALUMINIUM METAL POWDER (PURE)

    2. AL2O3

    3. MWCNT

    LUBRICANT

    Zinc sterrate is used as the lubricant the percentage of zinc sterrate is 0.9-1%

    as per Hoganas metallurgy manual. The mechanism employed is try lubrication

    BINDERS

    Ethanol is used as a binders or additives in order to dispersed CNT

    uniformly with (AL+ AL2O3)

    METAL PURCHASED

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    The materials are purchased in material form for fabrication by powder metallurgy

    process. Aluminium the base matrix material, titanium carbide and CNT is added

    for enchasing strength. Zinc sterrate is added for lubrication and bonding between

    the composites.

    DIE

    COMPOSITION OF POWDER

    Raw materials used in the experiments are high purity aluminium (>99.9%), AL2O3

    and CNT.

    The additions of CNT are 0.25%, 0.5%, 0.75% and 1% (mass fraction). The

    chemical compositions of the test composites are listed in table 1.

    METAL COMPOSITION TABLE

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    Composites no. AL2O3 % CNT % AL

    1 5 0.25 Balance

    2 5 0.5 Balance

    3 5 075 Balance

    4 5 1 Balance

    5 5 1.25 Balance

    WEIGHTING INDEX

    Required amount of aluminium, AL2O3, MWCNT along with zinc sterrate is

    weighed with digital weighing machine. The blend is prepared for different

    compositions of each powder material are weighted individually for the required

    composition using digital weighing scale.

    MIXING (BLENDING) OF POWDERS

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    The measured blend is taken in a glass beaker and stirred walk with the help

    of a stirrer made by glass. The stirring has to be done properly to get the

    homogeneous mixture.

    FILLING THE DIE

    The prepared blend is poured into the die and filled to the desired level.

    Using filler the blend is filled thoroughly into the die for better compaction.

    COMPACTION

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    The die is placed safely into the MCTM machine. The load is then applied

    gradually to the die for compaction.

    EXTRUSION OF THE SPECIMEN

    Extruded specimens (green sample)

    The dimensions of the extruded specimens are measured using vernier

    caliper.

    Length of the specimen : 10 mm

    Diameter of the specimen: 20 mm

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    COATING

    The extruded specimens are coated with aluminium to prevent the green

    compact from oxidation. There after the specimen must be handled carefully

    because it having the chance of getting brokened easily it likes a cake piece and

    this should heated in the muffle furnace for getting the expected specimen what

    really we want.

    4.2 SINTERING

    The bonding of adjacent surface of particles is in compact by heating.

    Sintering strengthens a powder and mass and normally produces densification, and

    in powdered metals, Recrystallization. The specimens are placed in a fine sand

    bath and it uniformly distributes the heat to the specimen. The specimens are

    submerged in the sand and the bath containing the specimens is placed inside

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    muffle furnace for sintering process. The sintering temperature should be below

    1the melting point of magnesium. Since chosen 500oC whereas the melting point

    magnesium is 650oC. After reaching the desired temperature, furnace is kept for 3

    hours.

    The sand bath containing the specimens is withdrawn after 12 hours

    SPECIMEN AFTER SINTERING

    The specimens are checked for damage like cracks and deformation by

    physical observation. No cracks are found. Thus required specimens are obtained.

    The specimens are tested in order grasp the properties like the tribological and

    mechanical.

    4.3 ELECTROLESS COATING:

    Electroless coating processes deposit metallic coating on a substrate without

    the use of an external voltage or current. They are commonly referred to as

    chemical metal deposition because the electrons required to bring about the

    discharge of metal ions are produced by a chemical reaction in solution. Deposition

    of metal is made from solution containing reducing agents .Such deposits from

    only on certain catalytically active surfaces (autocatalytic deposition).The electrons

    needed to reduce the metal ions are provided by the reducing agents R which

    surrender n electrons, while getting oxidized to R(n+).The simplified from of the

    reaction which describes the Electroless process is given as follows:

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    It is properly named autocatalytic, because the oxidation of the reducing

    agent can start or become self-sustained only at the deposition metal surface.

    Plating can be done on non-catalytic base materials, after suitable activation of the

    surface involved. Electroless deposits of nickel, copper, gold, silver, cobalt,

    palladium etc. and of alloys involving one or more of these metals have been

    produced in this process on various metallic and non-metallic substrates. In

    contrast to electroplating, Electroless plating does not involve electric field

    distribution. As a consequence uniformity of coating thickness could be achieved

    even on intricate part geometries.

    4.3.1 ELECTROLESS NICKEL COATING:

    As already mentioned, a number of metals like nickel, copper, gold, cobalt,

    palladium, silver etc. can be deposited by Electroless process. However, the bulk

    of the deposits produced today are based on nickel. It has excellent mechanical and

    electrochemical properties such as hardness, wear, abrasion and corrosion

    resistance. Mainly due to this it has excellent commercial potential across a wide

    Aerospace

    machine

    oil/chemical

    miscl

    printing

    computer

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    spectrum of industrial application in the field of electronics, computers, aircraft

    parts, textile industry, automobiles, valves, dies etc.

    ADVANTAGES:

    Major advantages of Electroless coating over the electro deposition

    process include:

    Formation of a uniform deposit on irregular surfaces

    Direct deposition on conductors and surface activated non-conductors

    Formation of less porous deposits

    Good wear resistance

    Good corrosion resistance.

    DISADVANTAGES:

    The major drawback of EN coating is its high cost of production

    due to various factors such as:

    Cost of chemical used

    Wastage in the form of nickel bearing sludge

    Poor nickel recovery from the bath etc

    Electroless nickel bath decomposition

    Due to these reasons, the EN coating process efficiency is reported to

    be poor order of only 50%

    4.3.2 ELECTROLESS NICKLE PHOSPHOROUS:

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    Electroless Nickel Phosphorous (EN) coatings have been used

    either as protective or decorative coating in industries such as electronics,

    computer, aerospace, printing, automotive, textile, plastics, optics, paper and food

    (parker, 1972). Some of the outstanding characteristics of EN coatings are superior

    corrosion and wear resistance, excellent uniformity, wide range of thickness, good

    solder ability, improved mechanical and physical properties (Baudrand,1978).EN

    deposition is carried out with:

    A. Nickel chloride and/or nickel sulphate as the source of nickel

    B. Sodium hypophosphite or sodium pyrophosphate as the reducing agent

    C. A salt of an organic acid as a buffer

    D. A mild complexing agent for nickel.

    Deposits from these reducing agents contain a maximum of 14

    wt., % phosphorus. Hydrazine hydrate is also used as a reducing agent for

    production of high purity nickel deposits. For the controlled deposition of the

    metal, numbers of parameters like temperature of deposition, pH of the bath,

    concentration of the reducing agent etc., are to be monitored closely during

    deposition. Improper control of one or more of these parameters might result in

    deposits with widely fluctuating properties. For better stability and utility of the

    plating bath, specific stabilizers and complexing agents are employed.

    4.3.3 EXPERIMENTAL DETAILS:

    PREPARATION OF SPECIMEN:

    The substrate material used ALUMINIUM alloy with a size

    25mm10mm. The chemical composition of the alloy is given below. The samples

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    were abraded with emery sheet upto 2000SiC paper before the pretreatment

    processes.

    TABLE: chemical composition of the aluminium alloy

    Al (wt., %) 9.1

    Zn (wt., %) 0.64

    Mn (ppm) 0.17

    Fe (ppm) 0.01

    Mg Balance

    TABLE: CEN COATING BATH AND OPERATION

    NiSO4.6H2O 5.2g/200ml

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    NaH2PO2. H2O 6g/200ml

    HF 2.4ml/200ml

    CH3COONa.3 H2O 3.2g/200ml

    NH32HF 1.6g/200ml

    Thiourea (ppm) 0.4ml/200ml

    PH 9-10, 7, 4-5

    Temperature 87 2

    Time 1hr

    The bath of 200ml contains the above chemicals mixed. The

    pH should not be more or less than 4-10.

    4.4 EXPERIMENTAL SETUP:

    4.4.1 MATERIALS PROCURED:

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    4.4.2 ELECTROLESS PLATING BATH:

    The electrolyte bath was heated indirectly through an electrically heated

    water bath. The temperature of the water bath was controlled by an ON/OFFF

    relay and Proportional Integral Derivative (PID) controller. Temperature of the

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    electrolyte bath was monitored using a thermometer. The experimental setup is

    show in the Fig. The pH of the electrolyte bath was maintained at 4-10 by adding

    sodium hydroxide solution. The total volume of the plating bath was 200ml. The

    coating duration is 1 hour after which the bath decomposes as shown.

    IMPLEMENTATION OF EXPERIMENT

    SCANNING ELECTRON MICROSCOPE

    SCANNING ELECTRON MICROSCOPE

    Materialselection

    Procurement

    Preparation of specimen and

    pretreatment process

    Ni-P coating on the substrate

    SEM test and conclusions

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    The Scanning electron microscope (SEM) is a type of electron microscopethat images the sample surface by scanning it with a high-energy beam of electrons

    in a raster scan pattern. The electrons interact with the atoms that make up the

    sample producing signals that contain information about the samples surface

    topography, composition and other properties such as electrical conductivity.

    The types of signals produced by an SEM include secondary electrons, back-

    scattered electrons (BSE), characteristics X-rays, light (cathodoluminescence), andspecimen current and transmitted electrons. Secondary electrons detectors are

    common in all SEMs, but it is rare that a single machine would have detectors for

    all possible signals. The signals result from interactions of the electron beam with

    atoms at or near the surface of the sample.

    In the most common or standard detection mode, secondary electron

    imaging or SEI, the SEM can produce very high-resolution images of a sample

    surface, revealing details about less than 1 to 5 nm in size. Due to the very narrow

    electron beam, SEM micrographs have a large depth of field yielding a

    characteristic three-dimensional appearance useful for understanding the surface

    structure of a sample.

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    Because the intensity of the BSE signal is strongly related to the atomic

    number (Z) of the specimen, BSE images can provide information about the

    distribution of different elements in the sample. For the same reason, BSE imaging

    can image colloidal gold immune-labels of 5 or 10 nm diameter which would

    otherwise be difficult or impossible to detect in secondary electron images in

    biological specimens.

    Characteristics X-rays are emitted when the electron beam removes an inner

    shell electron from the sample, causing a higher energy electron to fill the shell and

    release energy. These characteristics X-rays are used to identify the composition

    and measure the abundance of elements in the sample.

    INTERNAL STRUCTURE OF SCANNING ELECTRON MICROSCOPE

    A source (electron gun) of the electron beam which is accelerated down the

    column.

    A series of lenses (condenser and objective) which act to control the

    diameter of the beam as well as to focus the beam of the specimen

    A series of apertures (micron-scale holes in a metal film) which the beam

    passes through and which affect properties of that beam.

    Controls for specimen position (x,y,z height) and the orientation (tilt,

    rotation)

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    An area of beam/specimen interaction that generates several types of signals

    that can be detected and processed to produce an image or spectra.

    High magnification SEM images of some of the rod like structures showing

    different CNT configurations

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    MICROSTRUCTURE OF AL ALLOY WITH TIC

    a) AL alloy + 0.25% CNT shows the uniform description throughout the

    sample.

    b) AL alloy +0.5% CNT spot out of CNT

    c) AL composites +0.75% CNT crater formation in the sample

    d) AL composites +1% CNT formation of agglomeration over the AL alloy.

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    HARDNESS

    The metals handbook defines hardness as resistance of metal to plastic

    deformation, usually by indentation. However the term may also refer to stiffness

    or temper or to resistance to scratching, abrasion, or cutting. It is the property of a

    metal, which gives it the ability to resist being permanently, deformed (bent,

    broken, or have its shape changed), when a load is applied. The greater hardness of

    the metal, the greater resistance it has to deformation.

    In mineralogy the property of matter commonly described as the resistance

    of a substance to being scratched by another substance. In metallurgy hardness is

    defined as the ability of a material into resist plastic deformation.

    The dictionary of metallurgy defines the indention hardness as the resistance

    of a material to indention. This is the usual type of hardness test

    HARDNESS MEASUREMENT METHODS

    There are three types of tests used with accuracy by the metals industry; they

    are the Brinell hardness test the Rockwell hardness test and the wickers hardness

    test. Since the definition of metallurgic ultimate strength and hardness are rather

    similar, it can generally be assumed that the strong metal s also a hard metal. The

    way the tree of these hardness tests measure a metals hardness is to determine

    metals resistance to the penetration of a non-deformable ball or cone.

    The tests determine the depth which such a ball or cone will sink into the

    metal, under a given load, within a specific period of time.

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    The following are the most common hardness test methods used in todays

    technology;

    1. Rockwell hardness test

    2. Brinell

    3. Vickers

    4. Knoop

    5. Shore

    ROCKWELL HARDNESS TEST

    The Rockwell scale is a hardness scale based on the indentation hardness of

    a material. The Rockwell test determines the hardness by measuring the depth of

    penetration of an indenter under a large load compared to the penetration made by

    a preload. There are different scales, denoted by a single letter that use different

    loads are indenters. The result is a dimensionless number noted as HRA, where A

    is the scale letter. When testing metals, indentation hardness correlates linearly

    with tensile strength. This important relation permits economically important non

    destructive testing of bulk metal deliveries with light weight, even portable

    equipment, such as hand-held Rockwell hardness testers.

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    TESTING MACHINE

    INTRODUCTION

    The Rockwell scale is a hardness scale based on the indentation hardness of

    a material. The Rockwell test determines the hardness by measuring the depth of

    penetration of an indenter under a large load compared to the penetration made by

    a preload. There are different scales, denoted by a single letter that use different

    loads are indenters. The result is a dimensionless number noted as HRA, where A

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    is the scale letter. When testing metals, indentation hardness correlates linearly

    with tensile strength. This important relation permits economically important non

    destructive testing of bulk metal deliveries with light weight, even portable

    equipment, such as hand-held Rockwell hardness testers.

    OPERATION

    The determination of the Rockwell hardness material involves the

    application of a minor load followed by a major load, and then noting the depth of

    penetration, vis a vis, hardness value directly from a dial, in which a harder

    material gives a higher number. The chief advantage of Rockwell hardness is its

    ability to display hardness values directly, thus obviating tedious calculations

    involved in other hardness measurement techniques. It is typically used in

    engineering and metallurgy. Its commercial popularity arises from its speed,

    reliability, robustness, resolution and small area of indentation.

    In order to get a reliable reading the thickness of the test piece should be at

    least 10 times the depth of indentation. Also, readings should be taken from am flat

    perpendicular surface, because convex surfaces give loser readings. A correction

    factor can be used if the hardness of a convex surface must be measured.

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    TABLES

    ROCKWELL HARDNESS TEST

    Table 1:

    CNT % TIC % AL HARDNESSVALUE

    (HV)

    0.25 5 Bal 80

    0.5 5 Bal 85

    0.75 5 Bal 91

    1 5 Bal 82

    1.25 5 Bal 84

    COMPRESSIVE STRENGTH

    DEFINITION

    Compressive strength is the capacity of a material or structure to withstand

    axially directed pushing forces. When the limit of Compressive strength is reached,

    materials are crushed. Concrete can be made to have high Compressive strength,

    e.g. many concrete structures have Compressive strengths in excess of 50Mpa,

    whereas a material such as soft sandstone may have Compressive strength as low

    as 5 or 10Mpa.

    Compressive strength is often measured on a universal testing machine,

    these ranges from very small table top systems to ones with over 53 MN capacities.

    Measurements of Compressive strength are affected by the specific test method

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    and conditions of measurement. Compressive strengths are usually reported in

    relationship to a specific technical standard.

    COMPRESSION

    On an atomic level, the molecules or atoms are forced apart when in tension

    where as in compression they are forced together. Since atoms in solids always try

    to find an equilibrium position, and distance between other atoms, forces arise

    throughout the entire material which appose both tension and compression.

    The phenomena prevailing on an atomic level are therefore similar. On a

    macroscopic scale, these aspects are also reflected in the fact that the properties of

    most common materials in tension and compression are quite similar.

    TABULATION

    Sample Compressive strength (Mpa)

    1 415

    2 431

    3 465

    4 466

    STRESS STRAIN DIAGRAM

    By definition, the Compressive strength of a material is that value of

    uniaxial Compressive stress reached when the material fails completely. The

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    Compressive strength is usually obtained experimentally but means of a

    Compressive test. The apparatus used for this experiment is the same as that used

    in a tensile test however, rather than applying a uniaxial tensile load; a uniaxial

    Compressive load is applied. As can be imagined, the specimen (usually

    cylindrical) is shortened as well as spread laterally. A stress-strain curve is plotted

    by the instrument and would look similar to the following;

    The difference in values may therefore be summarized as follows;

    1. On compression, a specimen wills shorten. The material will tend to spread

    in the lateral direction and hence increase the cross sectional area.

    2. In a compression test the specimen is clamped at the edges. For this reason,

    a frictional force arises which will appose the lateral spread.

    WEAR

    INTRODUCTION

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    In materials science, wear is erosion or sideways displacement of material

    from its derivative and original position on a solid surface performed by the action

    of another surface.

    Wear is related to interactions between surfaces and more specifically the

    removal and deformation of material on a surface as a result of mechanical action

    of the opposite surface the need for relative motion between two surfaces and

    initial mechanical contact between asperities is an important distinction between

    mechanical wear compared to other process with similar outcomes.

    The definition of wear may include loss of dimension from plastic

    deformation if it is originated. However, plastic deformation such as yield stress is

    excluded from the wear definition if it doesnt incorporates a relative sliding

    motion and contact against another surface despite the possibility for material

    removal, because it then lacks the relative sliding action of another surface. Impact

    wear is in reality a short sliding motion where two solid bodies interact at an

    exceptional short time interval. Previously due to the fast execution, the contact

    found in impact wear was referred to as an impulse contact by the nomenclature.

    Impulse can be described as a mathematical model of a synthesized average on the

    energy transport between two travelling. Cavitations wear is a form of wear where

    the erosive medium or counter-body is a fluid. Corrosion may be included in wear

    phenomenon but the damage is amplified and performed by chemical reactions

    rather than mechanical action.

    MEASUREMENT

    A standard result review for wear tests, defined by the ASTM international

    and respective subcommittees such as committee G-2, should be expressed as loss

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    of material during wear in terms of volume. The volume loss gives a truer picture

    than weight loss, particularly when comparing the wear resistance properties of

    materials with large differences in density. For example, a weight loss of 14 g in a

    sample of tungsten carbide +cobalt (density=14000 kg/m3) and a weight loss of 2.7

    g in a similar sample of aluminium alloy (density=2700 kg/m3) both result in the

    same level of wear (1 cm3) when expressed as a volume loss. The inverse of

    volume loss can be used as a comparable index of wear resistance. Standard wear

    tests are only used for comparative material ranking as a specific test parameter as

    stipulated in this method. For more realistic values of material deterioration in

    industrial applications it is necessary to conduct wear testing under conditions

    simulating the exact wear process.

    The working life of an engineering component is expired when dimensional

    losses exceed the specified tolerance limits. Wear, along with other aging

    processes such as fatigue and creep in association with stress concentration factors

    such as fracture toughness causes materials to progressively degrade, eventually

    leading to material failure at an advanced age. Wear in industrial application is oneof a limited number fall factors in which on object losses its usefulness and

    economic implication can be of enormous value to the industry.

    TYPES

    The study of process of wear is the part of the discipline tribology. The complex

    nature of wear has delayed its investigations and resulted in isolated studies

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    towards specific wear mechanism or process. Some commonly referred to wear

    mechanisms include

    1. Adhesive wear

    2. Abrasive wear

    3. Surface fatigue

    4. Fretting wear

    5. Erosive wear

    A number of different wear phenomenonss are also commonly encountered and

    presented in the literature. Impact cavitations, diffusive and corrosive wear are all

    such examples. These wear mechanisms, however, do not necessarily act

    independently and wear mechanisms are not mutually exclusive. Industrial wear

    are commonly described as incidents of multiple wear mechanisms occurring in

    unison. Another way to describe industrial wear is to define clear distinctions in

    how different friction mechanisms operate, for example distinguish betweenmechanisms with high or low energy density. Wear mechanisms and / or sub-

    mechanisms frequently overlap and occur in a synergistic manner, producing a

    greater rate of wear than the sum of the individual wear mechanisms.

    HARDNESS TESTING MACHINE (VICKERS HARDNESS TEST):

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    Hardness test for evaluating the influence o different percentage of

    surfactants SLS, C-TAB in hardness of the specimen coated.

    The Vickers hardness test method consists of indenting the material with

    a diamond indenter, in the form of a right pyramid with a square base and an angle

    of 136 degrees between opposite faces subjected to a load of 1to 100 kgf. The full

    load is normally applied for 10 to 15 seconds. 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 kgf load by the square mm area of indentation.

    HARDNESS TEST FOR FOLLOWING MODULES:

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    SLS (sodium lauryl sulphate):

    Fig: micro hardness Vs concentration of SLS

    Increase in concentration of SLS increases the hardness.

    SLS gives maximum hardness when added at 0.8 g/l

    SURFACE ROUGHNESS TEST:

    SURFACE ROUGHNESS TESTING MACHINE (PERTHOMETER):

    A perthometer is a measuring instrument for the characterization of

    the roughness of surfaces.

    The perthometer functions similarly as a second record player. With a

    palpation point one drives on the surface of a solid body along. The unevenness

    are led from the probe into the equipment and converted there into electrical

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    signals. These signals serve for the determination of different characterisTIC

    values. Which characterize the surface roughness?

    SLS (sodium lauryl sulphate):

    INFERENCE:

    Increase in concentration of SLS increases the surface roughness to a

    certain point and then it decreases due to agglomeration of particles.

    SLS gives maximum surface roughness when added at 0.6 g/l

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    RESULT

    Rockwell hardness test in table and fig: 14 shows the hardness value

    increase gradually 26% from AL composites (AL+TIC) sample to 0.25% CNT,

    from 0.25% CNT to 0.75% CNT is increasing after that the hardness value is 35%

    decreasing from 0.75% CNT and above, because of as agglomeration reaction.

    CNT particles interact with each other leading to cluttering of particles and

    consequently settling down. Eventually the densities of CNT particles in the melt

    start decreasing there by lowering the hardness value.

    .

    RESULT AND CONCLUSION

    FROM MWNTS SUNTHESIS, THE FOLLOWING CONCLUSION

    ARE DRAWN

    The production MWNTs are made very simple and cost effective.

    More yield was attained by the simplified arc discharge technique

    Economic analysis of the synthesis of MWNTs shows the technique

    used in the present research is very cheap with better yield than the

    conventional technique.

    The results prove that MWNTs are good in quality and easily mixes

    with matrix powders with less agglomeration that lead to enhanced

    properties.

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    FROM MWNTS REINFORCED AL ALLOYS, THE FOLLOWING

    CONCLUSIONS DRAWN:

    The hardness are improved considerably with the addition of CNTs,

    but the relatively less

    When CNT concentration is beyond 1 wt%

    The decrease in the properties is due to the agglomeration of CNTs

    due the vander-waals force of attraction between each nanotubes

    particles

    The hardness indentation study reveals that hardness increased with

    the addition of MWNTs it may be due to CNTs and grains refine

    technique, which associated with the addition of CNTs

    Compression strength of the material will increase with the addition

    of CNT and corresponding the there will be decrease in the wear rate.

    Concentration of MWNTs added to newly formulated alloys increase

    the corrosion resistance increased due the passivatuion and galvanic

    properties of CNTs.

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