Tribological Investigtions on Al-Al3Ti In-Situ Metal Matrix Composite by IJIRST

IJIRST –International Journal for Innovative Research in Science & Technology| Volume 3 | Issue 01 | June 2016 ISSN (online): 2349-6010

Tribological Investigations on Al-Al3Ti In-situ Metal Matrix Composite Veeresha G Assistant Professor Department of Mechanical Engineering New Horizon College of Engineering, Bangalore-560103, Karnataka, India

Abstract In the present study, an attempt has been made to prepare and characterize Al-Al3Ti metal matrix composites with varying percentage of in-situ Al3Ti (3, 5 and 7%). The composites were prepared by the reaction commercial purity aluminum 99.7% and K2TiF6 salt at a reaction temperature of 800 °C. The prepared samples were characterized by optical microscopy. The wear tests were conducted on all the prepared samples by varying parameters like wt. % of Al3Ti particles, normal pressures, sliding speeds. Mechanical properties were assessed using computerized universal testing machine, Brinell hardness tester, Surface roughness tester and micro hardness tester. The worn surfaces were examined by optical microscopy after wear test.Al-3Ti, Al5Ti and Al-7Ti alloys were prepared and effect of Ti content on hardness, tensile strength, volumetric wear rate and surface roughness were examined. Experimental alloys were fabricated by salt route method. Volumetric wear rate of the reinforced Al3Ti, Al-5Ti and Al-7Ti alloys at room temperature were measured. The present results suggest that the wear resistance of AlAl3Ti composites increases with increase in percentage of Al3Ti particles compared to pure aluminum. In addition, the improvement in mechanical properties of the composite was observed in Al-5Ti composite when compared to Al-3Ti and Al-7Ti and to the pure Al. Better tribological properties of these alloys can be achieved at Al-5Ti. Keywords: Al-Al3Ti, Intermetallic compounds, Hardness, Tensile strength, Volumetric wear rate, sliding speed, Surface roughness, frictional force _______________________________________________________________________________________________________ I.

INTRODUCTION

For structural application of moving components, the tribological properties (friction and wear) are considered to be one of the major factors controlling the performance. In recent years, lightweight metal matrix composites (MMC) have received wider attention for their technological application, such as automotive parts etc. This paper reports the tribological behavior of Al based composites reinforced with in situ TixAly and Al2O3 particles. The wear experiments were performed on a newly designed fretting tribometer to evaluate the role of intermetallic particulates on the wear performance of in situ composites against bearing steel under the ambient conditions of temperature (22–25 °C) and humidity (50–55% RH). Based on the topographical observation of the worn surfaces the plausible wear mechanisms are discussed. An important result is that Al-based composites with 20 vol% reinforcement exhibit an extremely low coefficient of friction of 0.2 under unlubricated conditions. Also, around five times lower wear volume is measured with 20 vol% composites when compared to unreinforced Al. During past two decades, requirements for specific property material for advanced aerospace and automobile application have escalated since conventional alloy systems are not suitable there. Attempts to enhance the performance characteristics of monolithic materials by reinforcement with high strength/ high stiffness second phase are therefore required. By selecting the appropriate reinforced constituents of a material that is volume fraction, shape and size. It is possible to design alloys with enhanced strength and stiffness. Polymers, ceramics or metals such as aluminum, magnesium, titanium, copper and nickel alloys serve as matrix materials with whiskers (SiC), monofilaments (SiC, B, W), fiber (SiC, Al 2O3, graphite) and particulate (SiC, Al2O3, Al3Ti) acting as reinforcement. These reinforcements normally strengthen the matrix as they are stronger than the matrix alloys. Due to the presence of hard particles these metal matrix composites (MMCs) are currently being considered as promising tribological materials with applications in the aerospace, aircrafts and in a particular automotive industries. The high strength to weight ratio and wear resistance of aluminum MMCs makes the substitution of steel engine parts such as pistons, liners, clutches, pulleys rockers and pivots by MMCs parts in automobiles. This results in improved engine efficiency a reduction in noise and friction. Aluminum based particulate reinforced metal matrix composites have emerged as an important class of high performance materials for use in aerospace, automobile, chemical and transportation industries because of their improved strength, high elastic modulus and increased wear resistance over conventional base alloys. Recently, in situ techniques have been developed to fabricate aluminum-based metal matrix composites [1-4], which can lead to better adhesion at the interface and hence better mechanical properties. Owing to low density, low melting point, high specific strength and thermal conductivity of aluminum, a wide variety of ceramic particulates such as SiC, B4C, Al2O3, TiC and graphite have been reinforced into it. Among these particulates, Al3Ti has emerged as an outstanding reinforcement. This is due to the fact that Al 3Ti is stiff, hard and more importantly, does not react with aluminum to form any reaction product at the interface between the reinforcement and

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matrix. There are a few routes to synthesis Al–Al3Ti composites, but in-situ approach is particularly suitable. Apart from the Al 3Ti exothermic nature with Al, its clean interface resulting from absence of oxidation during the creation of reinforcement offers its potential as a wear resistant composite. Its strong bonding with the Al matrix has been verified to be the control factor that affects the wear improvement of the composite. In situ composites are multiphase materials where the reinforcing phase is synthesized within the matrix during composite fabrication. Titanium Aluminide, which belongs to the refractory transition metal Aluminde, is well known for its stiffness and hardness. Furthermore it has good toughness and a high melting point and a good corrosion resistance. The Al 3Ti additions greatly increases the stiffness, hardness and wear resistance and decrease the coefficient of thermal expansion while reducing the electrical and thermal conductivity much less than the addition of the most other ceramic reinforcement. Furthermore Al 3Ti is a nucleating agent for aluminum, which of significance for the grain refining of Al. Therefore recently Al 3Ti reinforced Al matrix composite have been studied. Most process employed in the synthesis of MMCs involve the incorporation of ceramic particles into the matrices via solid state (diffusion bonding, powder metallurgy, co extrusion, plasma spray, chemical and physical vapour deposition) and liquid state (squeeze casting) fabrication techniques. In these processes preexisting ceramic particles incorporated into the aluminum matrices. The major draw backs in these process involves the difficulties encountered in incorporating the fine ceramic enforcements into the matrices, agglomeration and poor wetting between particles and matrices. To overcome this problem and to increase the bonding strength between the particles and the matrix, the exothermic reaction process is good way to produce in situ ceramic particulates in the fabrication of Al based, Ti based, Ni based and other type based MMCs. Some commercial examples of in situ processing routes are lanxide’s DIMOX and PRIMEX, Martin Marientta’s XD synthesis, self-propagating high temperature synthesis, mechanical alloying, reactive gas injection, and reactive infiltration. One of the major drawback of these in situ composite is highly porous nature of the products. A new technology has been developed for the preparation of Al-Al3Ti in situ composites. In this process K2TiF6and KBF4 salts are mixed in molten Al. An exothermic reaction takes place to produce a dispassion of Al 3Ti particles. This is a single step and cheap casting process. This is a practical method for making wear structural parts. Hence the present study is taken up for preparing Al- Al3Ti in situ composites with varying percentage of Al3Ti particle. II. LITERATURE REVIEW As compared to most other aluminum -rich intermetallic phases, Al3Ti is very attractive because it has higher melting point (1460ºc) and relatively low density (3.91 g/cm3).The presence of Al3Ti particles can increase the creep strength of the alloy significantly (In Al-Al3Ti).By considering load sharing effect Al3Ti, an analysis based on continuum mechanics approach has been conducted. The threshold stress for creep in these composites was found to increase with increasing Al-Al3Ti composite. The presence of Al3Ti phase is very effective in increasing the stiffness of Al alloys. Alloy with fine two- phase Al-Al3Ti structure and significant Al3Ti content have been successfully produced by MA process. The young’s modulus of Al 3Ti phase has been determined to be 176GPa.The mechanical Alloying (MA) Al-Al3Ti alloys are characterized by very fine grain size and the presence of large volume fraction of fine dispersions of Al 3Ti, Al4C3, and Al2O3 particles. The size range of both the Al3Ti particles and the Al grains are 100-500 nm. According to the characteristics of the microstructure , MA Al-Ti alloy may be considered as a fine Al-Al3Ti two phase composite , in which the Al matrix further strengthened by the fine dispersoids of carbide and oxide. The fine carbide and oxide particles are mainly responsible for the fine grain structure as well as microstructural stability of the Aluminum matrix. The Al-Al3Ti composites have been shown to exhibit attractive combinations of low density (2.8g/cm3), high modulus, elevated temperature strength, thermal stability, and corrosion resistance. The young’s modulus of Al-Al3Ti composites was shown to increase to increase linearly with the content of Al 3Ti, that the increment is 1.1GP for every 1 volume % addition A The Al-Al3Ti composites exhibit good elevated temperature strength 115-155MPa, at 698K.A series of Al-Al3Ti composites of various Al3Ti content were prepared from Al and Titanium powders of commercial purity by mechanical Alloying (MA) [1]. Al3Ti intermetallic compounds were known as ductile materials with low toughness that causes some restriction in many applications. Since 1980, in order to increase the usage of these compounds and obtain tougher materials, they were used as reinforcements in metal matrix composites. During the last few decades, most researches have focused on ceramic reinforced aluminum metal matrix composites (MMCs). But there were some limitations in the fabrication process. These limitations include large differences between the coefficient of thermal expansions (CTE) of Al matrix and the ceramic reinforcements, and also high brittleness of ceramics. Intermetallic compounds which have low density and high modulus were a convenient choice when compared to ceramics. Since Al intermetallic compounds such as Al3Tihave highly close CTE compared with Al and lower brittleness compared to the ceramics, they can be a better choice than ceramics to overcome the mentioned obstacles. These prominent properties caused intermetallic compounds and mainly in this study, Al3Ti proves to be an attractive reinforcement for Al base metal matrix composites. Al3Ti with the density of 3.3 g/cm3, high melting mechanical properties. Al3Ti particles that form through in situ method are bonded strongly to the Al matrix due to the thermodynamic equilibrium. This strong bond is due to the good compatibility of a-Al having FCC crystal structure and tetragonal Al 3Ti. Due to the high melting temperature of Al3Ti, the most appropriate fabrication methods are powder metallurgy, such as hot pressing (HP), hot extrusion, and hot isostatic pressing (HIP) at temperatures close to the melting point of Al (660°C). These in situ generated particles increase the strength and modulus of the composite, which would significantly improve its wear resistance [2].

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Kuruvilla et.al have fabricated the in-situ particulate reinforced aluminum composite by hot pressing and reacting sintering Ti , Al and B powders. They reported that Al3Ti particulates with a size of about 1µm were formed in-situ in the aluminum matrix. In addition, there also existed some irregularly shaped Al3Ti particles (about 1 vol. %) with a size of several tens of micrometers in the in-situ composites, it is expected that a reduction in the particles would have an influence on properties of the composites, it is expected that a reduction in the particle size of the reinforcement would lead to improvements in strength, assuming all others things (shape, chemistry and distribution) are equal [3]. Carpenter et.al used molten salt (K2TiF6 and KBF4) reactive casting process to produce a dispersion of TiB 2 particles in Aluminum matrix. They found out three distinct size distributions of particulates (or rods): (a) coarse, with diameters (or length) 5-10µm. (b) fine, 1-2µm in size and (c) minute, about 10nm diameters. The coarse particles are composed of Al 3Ti and finer particles appeared to be randomly oriented and homogeneously distributed in the matrix. They have reinforced aluminum based metal matrix composites (MMCs), the automotive industries has identified a number of application for these materials [4]. III. EXPERIMENTAL DETAILS Material preparation: First of all Al-3wt%Ti, Al-5Ti and Al-7wt%Ti composites were prepared by reaction of halide salt such as K2TiF6 with molten Al in the resistance furnace. The process parameters such as reaction temperature of 800C and reaction time 60min were used in the present study. Initially commercial purity aluminium (99.7%) was heated to 800 0C in the resistance furnace. Once the required temperature was attained, the pre heated halide salts were added to the melt. The reaction between molten Al and the halide salts is generally vigorous and highly exothermic. Melt was stirred for 60min with zirconium coated steel rods to mix the halide salts with commercial purity aluminium (CPAl). After the completion of reaction, the spent salt was decanted from the surface of molten alloy and the melts were poured into the cylindrical graphite mould to prepare master alloys. Resistance Furnace Specifications: Power Rating - 6KW Supply 3 phase, 440V Max. Temperature 1300°C Capacity – 5KG Microstructure studies: The castings (25 mm ф and 100 mm length) were sectioned at a height of 25 mm from the bottom. A specimen of 5 mm height was cut from the section, which was left after 25 mm from the bottom surface of the casting. One surface of the specimen was initially polished using belt grinder and then a series of waterproof emery papers with increasing fineness to remove any of the scratches present. Final polishing was carried out on a disc polisher using 400 – mesh alumina powder until the mirror finishes and scratch free surface was obtained. Polished samples were cleaned with soap solution and distilled water and then the polished specimens were taken for optical microscopy. Experimental Procedure: Physical tests have been conducted on Al-3Ti, Al-5Ti, and Al-7Ti materials like Hardness, Tensile and surface roughness to understand the material properties. Hardness Test: The hardness test was conducted on brinell hardness tester. All Brinell tests use a carbide ball indenter. The test procedure is first the indenter is pressed into the sample by an accurately controlled test force. The force is maintained for a specific dwell time, normally 10 - 15 seconds. After the dwell time is complete, the indenter is removed leaving a round indent in the sample. The size of the indent is determined optically by measuring two diagonals of the round indent using either a portable microscope or one that is integrated with the load application device. The Brinell hardness number is a function of the test force divided by the curved surface area of the indent. The indentation is considered to be spherical with a radius equal to half the diameter of the ball. The average of the two diagonals is used in the following formula to calculate the Brinell hardness.

Fig. 3.1: Schematic diagram of the hardness test

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Table - 3.1 Brinell Hardness Number Sl. No Specimen BHN(Kg/mm2) 1 Al-3Ti 68.33 2 Al-5Ti 73.33 3 Al-7Ti 70

Tensile Test: The tensile test was conducted on the Universal Testing Machine(UTM). The test specimen overall length is 12mm.The D/L ratio is 1:8 i.e mean diameter is 8mm and gage length is 64mm. The test procedure is first to measure the mean diameter and nominal length. After that insert the specimen in the UTM and attach the extensometer. Selected a load range for UTM that will accommodate the maximum anticipated load during the test. Applied the load slowly, obtaining simultaneous readings of load from the UTM and elongation from the extensometer. When the extensometer nears its range, removed. Then continue monitoring the elongation of the specimen until fracture occurs. Attempt to obtain the load at fracture. After failure, fit the broken valves together and measure the final â&#x20AC;&#x153;gageâ&#x20AC;? length, and the smallest diameter.

Fig. 3.2: Typical tensile specimen, showing a reduced gage section and enlarged shoulders.

For Al-3Ti, Before breaking, Mean diameter= 8.073 mm Gage length= 64.5 After breaking, Mean diameter= 8 mm Gage length= 66 mm Peak load= 6.025 KN Displacement at Fmax= 11.090 mm Breaking load= 1.520 KN Maximum Displacement = 11.250 mm Area= 51.170 mm2 Ultimate stress= 0.118 KN/mm2 Elongation= 2.326% Reduction in area= 1.727% For Al-5Ti, Before breaking, Mean diameter= 8.01 mm Gage length= 61.9 mm After breaking, Mean diameter= 7.7 mm Gage length =65 mm Peak load= 5.503 KN Displacement at Fmax= 7.780 mm Breaking load= 0.215 KN Maximum displacement= 7.990 mm Area= 50.412 mm2 Ultimate stress= 0.109 KN/mm2 Elongation= 5.008% Reduction in area= 7.591% For AL-7Ti, Before breaking, Mean diameter= 8.046 mm Gage length= 62.8 mm After breaking, Mean diameter= 7.9 mm Gage length= 66.3 mm Peak load= 4.568 KN

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Displacement at Fmax= 8.900 mm Breaking load= 0.915 KN Maximum displacement= 8.940 mm Area= 50.790 mm2 Ultimate stress= 0.090 KN/mm2 Elongation= 5.573% Reduction in area= 3.452% Wear Test: Wear tests were conducted on pin on disc machine. The disc was made up of low carbon alloy steel (diameter 210mm) with hardness value about HRc 65. Five variables noted during the experiments were normal load, frictional force on the specimen, weight loss of the specimen due to wear, rotational speed and wearing time. Wear loss of the specimen was calculated by weighing the specimen before and after the each experimental on electronic analytical balance. All the wear tests were carried out at room temperature without any lubrication. Twelve experiments were conducted under operational conditions of two loads and two speeds. The process was repeated and compared the estimated values. Variables considered: Following wear test variables were selected. Sliding distance = 3000 m Sliding speed = 1 m/s, 3 m/s Load= 1 Kg, 3 Kg Estimation of speed and time for the experimental sliding speed: D- Diameter of wear track= 90 mm d- Diameter of wear pin= 10 mm v- Sliding speed (m/s) N- Rotational speed of wear disc (rpm) V= π ×D×N/1000×60 N= v×1000×60/π×D = 1×1000×60/π×90 = 212 rpm N= 3×1000×60/ π ×90 = 636 rpm For present investigation sliding distance, s= 3,000 m is considered. S= πDNT Where T= time in minutes T= s/π×D×N = 3,000/π×90×212 = 50 min T= 3,000/ π ×90×636 = 17 min Estimation of Experimental Results Specimen 1 2 3 4 5 6 7 8 9 10 11 12

Al-3Ti

Al-5Ti

Al-7Ti

Load (Kg) 1 1 3 3 1 1 3 3 1 1 3 3

Normal Pressure (MPa) 0.1248 0.1248 0.3747 0.3747 0.1248 0.1248 0.3747 0.3747 0.1248 0.1248 0.3747 0.3747

Sliding spee(m/s) 1 3 1 3 1 3 1 3 1 3 1 3

Frictional force (N) 9.9 9.7 13.8 3.8 5.5 5.8 11.5 17 5.2 10.3 12 14.8

Weight loss(Kg) 0.0000313 0.00001861 0.00005752 0.00029601 0.00002927 0.00001794 0.00005883 0.00003381 0.00002897 0.00002273 0.0000664 0.00003729

Volume loss(m3) 1.16E-8 3.703E-7 2.13E-8 1.096E-7 1.084E-8 6.644E-9 2.28E-8 1.25E-8 1.073E-8 8.418E-9 2.459E-8 1.381E-8

Volumetrc wearrate (m3/m) 3.864E-12 1.234E-10 7.101E-12 3.65E-11 3.615E-12 2.225E-12 7.26E-12 4.174E-12 3.57E-12 2.806E-12 8.197E-12 4.603E-12

For Al-3Ti, (1) Volume loss= Weight loss/Density = 0.0000313/2700 = 1.16E-8 m3 Volumetric wear rate = Volume loss/Sliding distance = 1.16E-8/3,000

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= 3.864E-12 m3/m (2) Volume loss= Weight loss/Density = 0.0000186/2700 = 3.703E-7 m3 Volumetric wear rate = Volume loss/Sliding distance = 3.703E-7/3,000 = 1.234E-10 m3/m (3) Volume loss= Weight loss/Density = 0.00005752/2700 = 2.13E-8 m3 Volumetric wear rate = Volume loss/Sliding distance = 2.13E-8/3,000 = 7.1012E-12 m3/m (4) Volume loss= Weight loss/Density = 0.0000296/2700 = 1.0966E-7 m3 Volumetric wear rate= Volume loss/Sliding distance = 1.0966E-7/3,000 =3.65E-11 m3/m For Al-5Ti, (1) Volume loss= Weight loss/Density = 0.00002927/2700 = 1.084E-8 m3 Volumetric wear rate = Volume loss/Sliding distance = 1.084E-8/3,000 = 3.613E-12 m3/m (2) Volume loss= Weight loss/Density = 0.00001794/2700 = 6.644E-9 m3 Volumetric wear rate= Volume loss/Sliding distance =6.644E-9/3,000 =2.214E-12 m3/m (3) Volume loss= Weight loss/Density = 0.00005883/2700 = 2.178E-8 m3 Volumetric wear rate = Volume loss/Sliding distance =2.178E-8/3,000 = 7.26E-12 m3/m (4) Volume loss= Weight loss/Density = 0.00003381/2700 = 1.252E-8 m3 Volumetric wear rate= Volume loss/Sliding distance = 1.252E-8/3,000 = 4.174E-12 m3/m For Al-7Ti, Volume loss= Weight loss/Density = 0.00002897/2700 = 1.0729E-8 m3 Volumetric wear rate = Volume loss/Sliding distance = 1.0729E-8/3,000 = 3.576E-12 m3/m (2) Volume loss= Weight loss/Density = 0.00002273/270 = 8.418E-9 m3 Volumetric wear rate= Volume loss/Sliding distance =8.418E-9/3,000 =2.806E-12 m3/m (3) Volume loss= Weight loss/Density = 0.0000664/2700 = 2.459E-8 m3

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Volumetric wear rate = Volume loss/Sliding distance =2.459E-8/3,000 = 8.197E-12 m3/m (4) Volume loss= Weight loss/Density = 0.00003729/2700 = 1.381E-8 m3 Volumetric wear rate= Volume loss/Sliding distance = 1.381E-8/3,000 = 4.603E-12 m3/m Surface Roughness Test: The surface roughness test was conducted on the SJ-201P surface roughness tester. Set up the SJ-201P (attaching/detaching the drive unit/detector, and cable connection, etc.) according to the feature of the work piece to be measured. Select either the AC adapter or built-in battery as the power supply. Modify the measurement conditions as necessary. Calibration is a means of adjusting the detector gain so that the SJ-201P can yield correct measurements. This can be easily performed by measuring a supplied precision roughness specimen. Measure the roughness specimen and display the result. Measurement results can be saved, printed, outputted as SPC data, and communicated with a personal computer via RS-232C interface. After measurement, store the SJ-201P safely by detaching the drive/detector unit, etc. Recharge the built-in battery as required. Surface Roughness (Ra) Sl. No 1 2 3 4 5 6 7 8 9 10 11 12

Specimen Al-3Ti

Al-5Ti

Al-7Ti

Load(Kg) 1 1 3 3 1 1 3 3 1 1 3 3

Sliding speed(m/s) 1 3 1 3 1 3 1 3 1 3 1 3

Perpendicular to Ra(µm) 2.713 4.33 3.33 3.146 1.96 2.17 3.553 2.67 2.163 2.41 2.37 1.173

VPN Test: The VPN test was conducted on the micro Vickers hardness tester after the wear test. The test procedure is first press the START key on the scales section then add the test load, the (LOADING) lights up. After completing the exertion of the first test load, the delay time (DWELL) LED lights up, at this time, the T on the LED screen will according to the number of time elapsed counter clockwisely. When the delayed time arrives, then test load is unloaded, and the unloading test load (UNLOADED) LED lights up. Before LED is extinguished, it is not allowed to turn the indenter to measure the changeover handle, else it will affect the precision (or accuracy) measured for indentation. Turn the changeover handle clock wisely, and make the 40 X objective lens in the front part of the main body. Then is measured, the diagonal length from the micrometer eyepiece. Before measurement, first turn clock wisely the drum wheel on the right side of micrometer eyepiece, so as to make the two calibrated lines observed in the eyepiece moving mutually closely. When the edges of two calibrated lines draw closely (overlapped), the right penetrating gap gradually diminishes, once the two calibrated lines are in a threshold state of no light gap, then press the ‘CL’ key to clear to zero at display of D1. First turn the left side drum wheel and make the calibration line to one corner of the indentation. Next, turn the right side drum wheel, then the two calibration lines are separated, and make the right side calibration line align to the diagonal of the indentation correctly, press at once the button at the lower part of the micrometer eyepiece and input. It will display D1 on the display screen. When the right side drum wheel rotates, figures after D1 on the LED screen flare, it means that the result has not yet been input. After the result has been input, there will be no more flare, and the cursor turns to D2. According to the method as mentioned above, measure and determine the length of another diagonal again. At this time, the HV hardness value on the LCD screen will be displayed automatically. Hardness Value Sl. No 1 2 3 4 5

Specimen Al-3Ti Al-5Ti

Load(Kg) 1 1 3 3 1

Sliding speed(m/s) 1 3 1 3 1

D1 148 104 118 113 119

D2 191 120 153 154 122

Distance 0.1 0.1 0.1 0.1 0.1

HV 0.1570772 0.3737331 0.2395335 0.0374579 0.3147956

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6 7 8 9 10 11 12

Al-7Ti

1 3 3 1 1 3 3

3 1 3 1 3 1 3

89 145 70 127 64 93 65

86 144 80 131 54 93 51

0.1 0.1 0.1 0.1 0.1 0.1 0.1

0.6123244 0.2217083 0.8126063 0.2711897 1.2634 0.5352439 1.376137

IV. RESULTS AND DISCUSSION Wear and physical test have been conducted on the materials Al-3Ti, Al-5Ti and Al-7Ti with varying percentage of Ti from 3 to 7%. Ti is used in Al base alloy. It is well known that by the addition of Ti in the alloy the hardness and wear resistance will increase. . By knowing this property the physical tests like Hardness, Tensile, surface roughness and wear tests have been carried out to understand the material behavior. Microstructure Studies: The microstructural study starts with the optical microscopy. All the cast samples, after polishing have been studied using image analyzer to observe the microstructure. The image analyzer photomicrographs of Al-3Ti, Al-5Ti and Al-7Ti alloys are shown in figs 4.1 and 4.2. It is observed that as the percentage of Ti increases the volume fraction of the Ti increased in the micrographs.

(A)

(B)

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(C)

Microstructure of different wt% of Ti: (a) Al-3Ti (b) Al-5Ti and (c) Al-7Ti with spot Magnification of 650x.

(A)

(B)

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(C)

Microstructure of different wt% of Ti: (a) Al-3Ti (b) Al-5Ti and (c) Al-7Ti with spot Magnification of 2000x

(A)

(B)

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(C)

(D)

EDX spectrum of (a) Al-3Ti (b) Al-5Ti and (c) Al 5Ti specimens taken on Al3Ti -particles. Hardness Test: Hardness is resistance of material to plastic deformation caused by indentation. Sometimes hardness refers to resistance of material to scratching or abrasion. Hardness may be measured from a small sample of material without destroying it. Principle of hardness test method is forcing an indenter into the sample surface followed by measuring dimensions of the indentation (depth or actual surface area of the indentation). Hardness is not fundamental property and its value depends on the combination of yield strength, tensile strength and modulus of elasticity.

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Brinell Hardness Test 70

Brinell hardness number(Kg/mm )

Sp.1. Al-3Ti Sp.2. Al-5Ti Sp.3. Al-7Ti

60 55 50 45 40 35 30 25 20 15 10 5 0 0

Specimen No

Effect of Ti on hardness: From the fig. 4.4 initially with increase in the volume fraction of the Ti hardness value is increased. With further increase in the Ti, hardness value is decreased. Ti is a grain refiner. Initially with increase in the grain refines hardness values is increased. With further increase in more refiner hardness value is decreased because, it may tends towards brittleness. It is observed that Specimen 2 that is Al-5Ti is having high hardness value compared to the other Specimen and Specimen 1 having lowest hardness value. Tensile Test: Tensile strength is defined as a stress, which is measured as force per unit area. For some non-homogeneous materials (or for assembled components) it can be reported just as a force per unit width. Tensile strengths are rarely used in the design of ductile members, but they are important in brittle members. Tensile Test

Ultimate Tensile stress(KN/mm )

0.120

Sp.1. Al-3Ti Sp.2. Al-5Ti Sp.3. Al-7Ti

0.115

0.110

0.105

0.100

0.095

0.090 0

Specimen No

Effect of Ti on tensile test: From the fig. 4.5 with increase in the Ti ductility will decrease. Therefore the ultimate tensile strength is decreased with increase in the Ti percentage. It is observed that with decrease in the percentage of Titanium the tensile strength is increased and further increase in the Ti% the tensile strength is decreased. Wear Test All the composites developed were tested on the pin on disc machine (TR-20, DUCOM). The effect of various tribological parameters Normal Pressure, Sliding speed and sliding distance was tested on each composite and compared with the wear behavior.

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Wear Test 0.1248 MPa 0.3747 MPa 1.20E-010

1.00E-010

Volumetric wear rate (m /m)

1.20E-010

8.00E-011

6.00E-011

4.00E-011

8.00E-011

6.00E-011

4.00E-011

2.00E-011

0.00E+000

0.00E+000 1

Specimen Nos.

Load - 1 KG

Speed (1m/s) Speed (3m/s)

Load - 3 KG

1.20E-010

1.00E-010

1.00E-010 3

Volumetric wear rate (m /m)

0.1248 MPa 0.3747 MPa

Sliding speed - 3 m/s

Volumetric wear rate (m /m)

Sliding speed - 1 m/s

8.00E-011

6.00E-011

4.00E-011

2.00E-011

8.00E-011

6.00E-011

4.00E-011

2.00E-011

0.00E+000

0.00E+000 1

Specimen Nos.

Effect of normal pressure on volumetric wear rate for the sliding speeds and loads From fig. 4.6 it is observed that with increase in volume fraction of Ti volumetric wear rate is decreased. Hence more percentage of Ti is preferable. Hence specimen Al-3Ti is more volumetric rate as compared to other 2 specimens. W ear Test

Sp.1. Al-3Ti Sp.2. Al-5Ti Sp.3. Al-7Ti

Sliding Speed -1m/s

Volumetric wear rate(m /m)

1.00E-010

Sp.No.1. Al-3Ti Sp.No.2. Al-5Ti Sp.No.3. Al-7Ti

1.00E-010

Volumetric wear rate (m /m)

Load - 1 KG

0.00E+000 0

0.00E+000 0.0000

Sliding Speed(m/s)

0.1248

0.2496

0.3744

Normal Pressure (MPa)

Sp.1. Al-3Ti Sp.2. Al-5Ti Sp.3. Al-7Ti

Load - 3 KG

Sp.No.1. Al-3Ti Sp.No.2. Al-5Ti Sp.No.3. Al-7Ti

1.50E-010 1.40E-010

Speed - 3 m/s 1.30E-010 1.20E-010

Volumetric wear rate(m /m)

1.00E-010

Volumetric wear rate (m /m)

1.10E-010 1.00E-010

9.00E-011 8.00E-011 7.00E-011 6.00E-011 5.00E-011 4.00E-011 3.00E-011 2.00E-011 1.00E-011

0.00E+000 0

Sliding Speed(m/s)

0.00E+000 0.0000

0.1248 0.2496 Normal pressure (MPa)

0.3744

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Effect of Specimens on Volumetric Wear Rate From the fig. 4.7 it is observed that, 3Ti values are higher than the other two materials. Ti is ductile material so with decrease in the volume fraction of the Ti softness is decreased hence the plastic deformation will also decrease. With decrease in the plastic deformation work hardening does not takes place hence, values of the volumetric wear rate is higher for Al-3Ti than the other two materials. Wear Test

Specimen .2. Al-3Ti

Data 2

g din Sli

re ( MP a)

s) m/ d( ee sp

1.40E-010 1.20E-010 1.00E-010 8.00E-011 6.00E-011 4.00E-011 2.00E-011 3 0.00E+000 0.0000 2 s) 0.1248 No 1 ed (m/ rma 0.2496 l pr pe ess 0.3744 0 ur gS e (M Pa )

Data 3

din Sli

Specimen .2. Al-7Ti

1.40E-010 1.20E-010 1.00E-010 8.00E-011 6.00E-011 4.00E-011 2.00E-011 3 0.00E+000 0.0000 2 s) 0.1248 No 1 ed (m/ rma 0.2496 l Pr pe ess 0.3744 0 gS ur

rate Volumetric wear

3 (m /m)

Specimen .2. Al-5Ti

rate Volumetric wear

3 (m /m)

rate (m3/m) Volumetric wear

Data 1

1.40E-010 1.20E-010 1.00E-010 8.00E-011 6.00E-011 4.00E-011 2.00E-011 0.00E+000 0.0000 0.1248 No rma 0.2496 l pr ess 0.3744 u

e (M Pa )

din Sli

Effect of normal pressure and sliding speed on volumetric wear rate From Fig.4.8 Under high sliding speed with increase in the normal pressure volumetric wear rate is decreased. Under high sliding speed effect of frictional temperature is high. Therefore volumetric wear rate is high under high sliding speed at low normal pressure. Whereas for the same under high normal pressure volumetric wear rate is decreased. This may be due to high frictional temperature, at this high frictional temperature a layer of wearing surface may be melted and this molten layer may be behaved as lubricated film so volumetric wear rate is decreased. Generally for all specimens under low speed of 1m/s, volumetric wear rate is increased with the normal pressure. For under high sliding speed of 3m/s the same is decreased with the normal pressure .Under low normal pressure the volumetric wear rate is increased with the sliding speed as the same is almost decreased with sliding speed under high normal pressure. Under low normal pressure with increase in the sliding speed volumetric wear rate is increased. Under low normal pressure very few asperities are get contact with disc so local stress on the asperities is high. Due to this high local stress, during wearing high temperature generates. Due to this high temperature softening effect takes place hence volumetric wear rate is increased, where as under high normal pressure more number of asperities get contact with the disc. Due to more number of asperities local stress generates on the asperities hence low temperature generates and this temperature may not be sufficient to soften the material also due to more number of asperities contact more percentage of metal deform plastically so some asperities of work hardening takes place, therefore volumetric wear rate is decreased. Under low sliding speed with increase in the normal pressure volumetric wear rate is increased as per the Archard equation, load is directly proportional the volume loss. Hence with increase in normal pressure volumetric wear rate is increased. Finally there is no much deviation between Specimens Al-3Ti and Al-7Ti in volumetric wear rate. Due to low volumetric wear rate in specimen Al-5Ti.Hence Al-5Ti is Preferable.

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Wear Test 0.1248 MPa 0.3747 MPa 14

Sliding Speed - 1 m/s

Sliding Speed - 3 m/s

Frictional Force (N)

Wear Test

0.1248 MPa 0.3747 Mpa

9 8 7 6 5 4

0 0

Specimen Nos.

Speed (1 m/s) Speed (3 m/s) Wear Test Load - 1 KG

Frictional Force (N)

Wear Test

Speed (1 m/s) Speed (3 m/s)

9 8 7 6 5 4

Load - 3 KG

0 0

Specimen Nos.

Effect of normal pressure on fictional force on sliding speeds and loads From Fig. 4.9 it observed that with increase in Titanium, the ductility will increase hence the frictional force is increased. In figure the maximum frictional force is high in specimen Al-5Ti compared to other 2 specimens due ductile property of Titanium. Wear Test Sp.1. Al-3Ti Sp.2. Al-5Ti Sp.3. Al-7Ti 18 17

Sliding speed - 1 m/s

Frictional Force (N)

Sp.1. Al-3Ti Sp.2. Al-5Ti Sp.3. Al-7Ti

11 10 9 8 7 6

Sliding speed - 3 m/s

0 0.00

0.05

0.10

0.15

0.20

0.25

0.30

0.35

0 0.00

0.40

0.05

0.10

0.15

0.20

0.25

0.30

0.35

0.40

Normal Pressure (MPa) Normal Pressure (MPa)

Sp.1. Al-3Ti Sp.2. Al-5Ti Sp.3. Al-7Ti

18 17

Sp.1. Al-3Ti Sp.2. Al-5Ti Sp.3. Al-7Ti

Load - 1 KG

Load - 3KG

15 14

13 12

Frictional Force (N)

12 11 10 9 8 7 6

5 4

3 2

1 0

0 0

Sliding speed (m/s)

Effect of specimens on frictional force From fig.4.10 it is observed that, 5Ti values are higher than the other two materials. Ti is ductile material so with increase in the volume fraction of the Ti softness is increased hence the plastic deformation will also increase. With increase in the plastic deformation work hardening takes place hence, values of the frictional force is higher for Al-5ti than the other two materials.

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Tribological Investigations on Al-Al3Ti In-situ Metal Matrix Composite (IJIRST/ Volume 3 / Issue 01 / 020)

Wear Test

Specimen.1. Al-3Ti

Data 2

e (M Pa)

Frictional Force (N

17 16 15 14 13 12 11 10 9 8 7 6 5 4 3 2 1 3.0 /s) 0 0.00 2.5 0.05 2.0 m 0.15 No 0.10 1.5 d( rma 0.20 0.25 1.0 0.5 Spee l Pr 0.30 0.35 0.0 0.40 es g sur

Specimen.2. Al-5Ti

)

) Frictional Force (N

Data 1

17 16 15 14 13 12 11 10 9 8 7 6 5 4 3 2 /s) 3 0.00 1 0.05 0 0.10 2 ed (m No rma 0.15 0.20 1 pe 0.30 l Pr 0.25 ess 0.35 0.40 0 ing S u

din Sli

re (

d Sli

Specimen.3. Al-7Ti

) Frictional Force (N

Data 3

MP a)

17 16 15 14 13 12 11 10 9 8 7 6 5 4 3 2 1 3 0 s) 0.00 0.05 0.10 m/ 2 0.15 No 0.20 d( rma 0.25 1 e 0.30 e l Pr 0.35 sp 0.40 0 ess ing u re (

MP a)

d Sli

Under high sliding speed with increase in the normal pressure frictional force is decreased. Under high sliding speed effect of frictional temperature is high. Therefore frictional force is high under high sliding speed at low normal pressure. Whereas for the same under high normal pressure frictional force is decreased. With increase in contact pressure the percentage at contact area will increase with increase in percentage at contact area frictional force is increased. With increase in the sliding speed the residential time between the wearing surface at the pin with the disc is reduced, with reduction in residential time the growth of micro weld reduces, with reduction in micro weld friction force is reduced. Hence with increase in sliding speed frictional force is reduced. With increase in sliding speed the frictional temperature also increases. Hence again the intimate contact between wearing surfaces increase. So some times with increase in sliding speed frictional force will increase due to more percentage at intimate contactness due to more plastic deformation of the wearing pin. Surface Roughness (Perpendicular) Test: Roughness is a measure of the texture of a surface. It is quantified by the vertical deviations of a real surface from its ideal form. If these deviations are large, the surface is rough; if they are small, the surface is smooth.

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Tribological Investigations on Al-Al3Ti In-situ Metal Matrix Composite (IJIRST/ Volume 3 / Issue 01 / 020)

Surface Roughness Test

0.1248MPa 0.3747MPa

Speed (1 m/s) Speed (3 m/s)

Sliding speed - 3 m/s

Load - 1 KG 4

Surface Roughness(m)

0 0

Specimen Nos.

Speed (1 m/s) Speed (3 m/s)

0.1248 0.3747 Sliding Speed - 1 m/s

Load - 3 KG 4

Surface Rougness(m)

Surface Roughness(m)

0 0

Specimen Nos.

Effect of normal pressure on surface roughness on sliding speeds and loads From fig. 4.12 with increase in hardness value surface roughness decreases due to shearing action. Shearing action is due to the ductile property of Titanium. Under high sliding speed the surface roughness is high, under low normal pressure surface roughness is high. Surface Roughness Test

Sp.1. Al-3Ti Sp.2. Al-5Ti Sp.3. Al-7Ti

4.0

Load - 1 KG

4.0

3.5

3.0

Surface Roughness(m)

Sliding Speed - 3 m/s 3.5

2.5

2.0

1.5

2.5

2.0

1.5

1.0

0.5

0.0 0.00

0.0 0.05

0.10

0.15

0.20

0.25

0.30

0.35

0.40

Normal Pressure (MPa)

Sp.1. Al-3Ti Sp.2. Al-5Ti Sp.3. Al-7Ti

Load -3 KG 4.0

4.0

3.5

Surface Roughness Test(m)

Surface Roughness(m)

Sliding speed (m/s)

3.0

2.5

2.0

1.5

1.0

0.5

Sliding Speed - 1 m/s

3.0

2.5

2.0

1.5

1.0

0.5

0.0 0

Sliding speed (m/s)

0.0 0.00

0.05

0.10

0.15

0.20

0.25

0.30

0.35

0.40

Normal Pressure (MPa)

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Tribological Investigations on Al-Al3Ti In-situ Metal Matrix Composite (IJIRST/ Volume 3 / Issue 01 / 020)

Effect of specimens on surface roughness From fig. 4.13 it is observed that, 3 Ti values are higher than the other two materials. Ti is ductile material so with decrease in the volume fraction of the Ti softness is decreased hence the plastic deformation will also decrease. With decrease in the plastic deformation work hardening does not takes place hence, with decrease in Ti values of the surface roughness is higher than the other two materials. Wear Test

Specimen.1. Al-3Ti

Data 2

)

Specimen.2. Al-5Ti

Frictional Force (N

Data 1

17 16 15 14 13 12 11 10 9 8 7 6 5 4 3 2 3 (m/s) 0.00 1 0.05 0 0.10 2 No d rma 0.15 0.20 ee 1 0.30 l Pr 0.25 Sp ess 0.35 0 0.40 g in u

sur

e (M Pa)

Frictional Force (N

17 16 15 14 13 12 11 10 9 8 7 6 5 4 3 2 1 3.0 /s) 0 0.00 2.5 0.05 0.10 2.0 m 0.15 No 1.5 d( rma 0.20 0.25 1.0 0.30 ee 0.5 l Pr p 0.35 0.40 0.0 g S es din Sli

re (

d Sli

Specimen.3. Al-7Ti

Frictional Force (N

)

Data 3

MP a)

17 16 15 14 13 12 11 10 9 8 7 6 5 4 3 2 1 3 0 s) 0.00 0.05 0.10 m/ 2 0.15 No 0.20 d( rma 0.25 1 e 0.30 e l Pr 0.35 sp 0.40 0 ess ing u re (

MP a)

d Sli

Effect of normal pressure and sliding speed on surface roughness of specimens From Fig.4.14 Under high sliding speed with increase in the normal pressure surface roughness is decreased. Under high sliding speed effect of frictional temperature is high. Therefore volumetric wear rate is high under high sliding speed as low normal pressure. Whereas for the same under high normal pressure surface roughness is decreased. Under high normal pressure the surface roughness is almost reduced with the sliding speed. Under high normal pressure the intimate contact between wearing pin surface with the disc is increased. Due to this increase in more contact area the smoothness is increased hence with under high normal pressure with increase in sliding speed roughness values is decreased. Under high sliding speed with increase in the normal pressure the roughness is decreased. Under high sliding speed the micro growth of weld is reduced due to reduction the residential time between the wearing pin with the disc. Hence under high sliding speed with increase in normal pressure the roughness values are decreased. VPN Test: The VPN test was carried out in the micro Vickers hardness tester after the wear test. Hardness is resistance of material to plastic deformation caused by indentation. Sometimes hardness refers to resistance of material to scratching or abrasion. Hardness may be measured from a small sample of material without destroying it. Principle of hardness test method is forcing an indenter into the sample surface followed by measuring dimensions of the indentation (depth or actual surface area of the indentation).

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Tribological Investigations on Al-Al3Ti In-situ Metal Matrix Composite (IJIRST/ Volume 3 / Issue 01 / 020)

Hardness Test 0.1248 MPa 0.3747 MPa 1.4

1.2

1.0

Hardness Value (Kg/mm )

Hardness Value(Kg/mm )

0.1248 MPa 0.3747 MPa

Sliding speed - 3 m/s

Sliding Speed - 1m/s

1.4

0.8

0.6

0.4

0.2

0.8

0.6

0.4

0.2

0.0

0.0 0

Specimen Nos.

Speed (1 m/s) Speed (2 m/s)

Speed (1m/s) Speed (3m/s)

Load - 1 KG 1.4

Load - 3 KG

1.4 1.3

1.2

Hardness Value (Kg/mm )

1.1 1.0

0.8

0.6

0.4

1.0 0.9 0.8 0.7 0.6 0.5 0.4 0.3

0.2

0.2 0.1

0.0

0.0 0

Specimen Nos.

Effect of normal pressure on Hardness value for sliding speeds and loads From fig. 4.15 with increase in hardness fraction of Ti hardness value is increased. Ti is ductile material so with increase in the volume fraction of the Ti softness is increased hence the plastic deformation will also increase. With increase in the plastic deformation work hardening takes place hence, values of the hardness for Al-7Ti is higher than the other two materials. VPN Test Sp.1. Al-3Ti Sp.2. Al-5Ti Sp.3. Al-7Ti

Sliding Speed - 3 m/s

1.4

Sp.No.1 Al-3Ti Sp.No.2 Al-5Ti Sp.No.3 Al-7Ti

1.4

1.0

Hardness Value(Kg/mm )

1.2

Hardness Value (Kg/mm )

Sliding Speed - 1 m/s 1.2

0.8

0.6

0.4

0.2

0.8

0.6

0.4

0.2

0.0 0.00

0.05

0.10

0.15

0.20

0.25

0.30

0.35

0.0 0.00

0.40

Normal Pressure (MPa)

0.10

0.15

0.20

0.25

0.30

0.35

0.40

Normal Pressure (MPa)

Sp.No.1. Al-3Ti Sp.No.2. Al-5Ti Sp.No.3. Al-7Ti

1.4

0.05

1.4

Sp.No.1 Al-3Ti Sp.No.2. Al-5Ti Sp.No.3. Al-7Ti

Load - 1KG

1.0

Hardness Value (Kg/mm )

1.2

1.0

Hardness Value(Kg/mm )

Load -3 KG 1.2

0.8

0.6

0.4

0.2

0.8

0.6

0.4

0.2

0.0

0.0 0

Sliding Speed (m/s)

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Tribological Investigations on Al-Al3Ti In-situ Metal Matrix Composite (IJIRST/ Volume 3 / Issue 01 / 020)

Effect of specimens on Hardness From fig.4.16 it is observed that, 7 Ti values are higher than the other two materials. Ti is ductile material so with increase in the volume fraction of the Ti softness is increased hence the plastic deformation will also increase. With increase in the plastic deformation work hardening takes place hence, values of the hardness is higher than the other two materials.

Speciman.3.Al-7Ti Data 3

1.4 1.2 1.0 0.8 0.6 0.4 0.2 3.0 0.0 0.10 0.15 2.5 0.20 2.0 /s) 0.25 Nor 1.5 0.30 d(m ma 0.35 ee 1.0 l Pr 0.40 Sp ess g n ure (MP a)

di Sli

2 Hardness Value(Kg/mm )

Data 2

Data 1

2 Hardness Value(kg/mm )

Hardness Test

Specimen.1.Al-3Ti

1.4 1.2 1.0 0.8 0.6 0.4 0.2 3.0 /s) 0.0 0.10 0.15 2.5 0.20 2.0 (m 0.25 Nor ed 1.5 0.30 ma pe 0.35 l Pr S 1.0 g ess 0.40 n i ur lid e(M Pa)

Specimen.1. Al-5Ti

1.4 1.2 1.0 0.8 0.6 0.4 0.2 3.0 0.10 0.0 0.15 2.5 0.20 2.0 0.25 1.5 0.30 Nor /s) 0.35 ma (m 0.40 1.0 l Pr ed es pe sur eM Pa)

gS din Sli

Effect normal pressure and sliding speed on hardness for specimens From Fig.4.17 Under high sliding speed with increase in the normal pressure Hardness value is decreased. Under high sliding speed effect of frictional temperature is high. Therefore volumetric wear rate is high under high sliding speed as low normal pressure. Whereas for the same under high normal pressure Hardness value is decreased. This may be due to high frictional temperature, at this high frictional temperature a layer at wearing surface may be melted and this molten layer may be behaved as lubricated film so Hardness value is decreased. For the specimen – 1, under low normal pressure of .1248MPa with increase in the sliding speed hardness values are increased. Under low normal pressure the generation of frictional temperature is usually low hence, with increase in sliding speed deformation of the worn surface is more so work hardening effect is more. Due to this work hardening the hardness values are increased. Under high normal pressure with increase in the sliding speed hardness values are decreased. Under high normal pressure the amount of area of contact is more and generation of frictional temperature is more, due to this frictional temperature softening effect takes place. Due to this softening effect the worn surface hardness is deceased. V. CONCLUSION The present results suggest that the wear resistance of Al-Al3Ti composites increases with increase in percentage of Al3Ti particles compared to pure aluminum. In addition, the improvement in mechanical properties of the composite was observed in Al-5Ti specimen when compared to Al-3Ti and Al-7Ti and to the pure Al. Volumetric wear rate of Al-5Ti is less compare to Al3Ti and Brinell hardness value also more for Al-5Ti compare Al-3Ti, Al-7Ti. There is almost no variation at properties between 5Ti and 7Ti but there is much variation between 5Ti and 3Ti. Hence 5Ti is better material among 3Ti, 5Ti and 7Ti. REFERENCES [1] [2] [3] [4]

S.H.WANG and P.K.KAO, “The strengthening effect of Al3-Ti in high temperature deformation of Al-Al3Ti composites”, Institute of Material Science and Engineering, NationalSun Yat-sen University, Kaohsiung, 80424, Taiwan, R.O.C M. Nofar *, H.R. Madaah Hosseini, N. Kolagar-Daroonkolaie, “Fabrication of high wear resistant Al/Al3Ti metal matrix composite by in situ hot press method”, Department of Materials Science and Engineering, Sharif University of Technology, P.O. Box 11365-9466, Tehran, Iran A. K. Kuruvilla, K. S. Prasad, V.V. Bhanuprasad, Y.R. Mahajan, “Microstructural property correlation in AL/TiB2 (XD) composites” , Script Metal Mater,24, 1990. 873-878 G.J.C. Carpenter, S.H.J. Lo, F.E. Goodwin, “Characterization of a titanium di-boride particulate reinforced aluminium composite produced by an in-situ reaction technique”,J. Mater. Sci. Let.,13, 1994, 30-33.

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