SYNTHESIS AND CHARACTERIZATION OF NEW ALUMINIUM ALLOY WITH MWCNT COATED WITH NI-P ELECTROLEES COATING

A PROJECT REPORT Submitted by

T.SAKTHIVEL R.SATHISH S.SELVAKUMAR U.MUJEPER RAHMAN

(84509144037) (84509144039) (84509144040) (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

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 Mr.C.Francis vimalraj. M.Tech., HEAD OF THE DEPARTMENT Mechanical department Imayam College of engineering Kannanur-621206

SIGNATURE Mr.A.Thiagarajan. M.Tech., GUIDED BY Mechanical department Imayam College of engineering Kannanur-621206

Submitted for Anna University viva-voce examination held on ___________

INTERNAL EXAMINER

EXTERNAL EXAMINER

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.

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.

TABLE OF CONTENTS CHAPTER NO. TITLE ABSTRACT LIST OF TABLE LIST OF FIGURE 1 INTRODUCTION 1.1 Aluminium Alloys 1.2 Advantages 1.3 Applications 2 LITERATURE REVIEW 2.1 Aluminium Alloy 2.2 Carbon nanotubes 3 POWDER METALLURGY 3.1 Powder metallurgy 3.2 Advantages 3.3 Procedures 3.3.1 Blending 3.3.2 Compaction 3.3.3 Sintering 13 13 14 14 15 17 5 6 1 3 3 PAGE NO. i v iv

EXPERIMENTAL PROCEDURE 4.1 Compaction Process 4.2 Sintering 4.3 Ni-P Coating 4.3.1 Electroless nickel coating 4.3.2 Electroless Ni-P coating 4.4 Experimental Setup 4.4.1 Electroless Plating Bath 19 24 25 26 28 31 31

CHRACTERIZATION 5.1 Hardness Test 5.1.1 Rockwell Hardness Test 5.1.2 Vicker Hardness Test 5.2 Wear 5.3 Compressive Strength 5.4 Scanning Electron Microscope 44 37 38

LIST OF FIGURES S.No. 1 2 3 4 5 6 7 8 9 10 11 12 FIGURES Carbon nanotube structure and helicity Schematic diagram of arc-discharge method Powder metallurgy process Sintering furnace Die Weighing machine Mixing of powder Compression Muffle furnace Scanning electron microscope Internal structure of SEM Rockwell hardness PAGE NO. 8 9 16 17 20 21 22 23 24 33 35 39

LIST OF TABLE S.NO 1 2 3 4 DESCRIPTION Composition Of Samples Rockwell hardness test Compressive strength composition of chemicals PAGE NO. 21 41 42 30

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 or aluminium 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.

Aluminium alloys 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 lower tensile 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.

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

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

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.

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.

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.

Carbon Nanotube Structure

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 obtain highly graphitized MWNTs without using metal catalyst.

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].

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.

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

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 (Cu385 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

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.

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

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

3.2.3 SINTERING DEFINITION

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

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

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

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

Composites no. 1 2 3 4 5

AL2O3 % 5 5 5 5 5

CNT % 0.25 0.5 075 1 1.25

AL Balance Balance Balance Balance 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

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

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 : Diameter of the specimen: 10 mm 20 mm

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

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:

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:

Aerospace machine oil/chemical miscl printing computer

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

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:

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

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

TABLE: chemical composition of the aluminium alloy Al (wt., %) Zn (wt., %) Mn (ppm) Fe (ppm) 9.1 0.64 0.17 0.01

Mg

Balance

TABLE: CEN COATING BATH AND OPERATION NiSO4.6H2O 5.2g/200ml

NaH2PO2. H2O HF CH3COONa.3 H2O NH32HF Thiourea (ppm) PH Temperature Time

6g/200ml 2.4ml/200ml 3.2g/200ml 1.6g/200ml 0.4ml/200ml 9-10, 7, 4-5 87 2 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:

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

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

Material selection

Procurement

Preparation of specimen and pretreatment process

Ni-P coating on the substrate

SEM test and conclusions

SCANNING ELECTRON MICROSCOPE SCANNING ELECTRON MICROSCOPE

The Scanning electron microscope (SEM) is a type of electron microscope that 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, backscattered electrons (BSE), characteristics X-rays, light (cathodoluminescence), and specimen 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.

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)

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

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.

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.

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.

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

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.

TABLES ROCKWELL HARDNESS TEST Table 1: CNT % TIC % AL HARDNESS VALUE (HV) 0.25 0.5 0.75 1 1.25 5 5 5 5 5 Bal Bal Bal Bal Bal 80 85 91 82 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

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 1 2 3 4 Compressive strength (Mpa) 415 431 465 466

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

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

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

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 one of 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

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 between mechanisms with high or low energy density. Wear mechanisms and / or submechanisms 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):

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:

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

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

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.

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.