Chapter 1: Introduction and literature review

1.1 Introduction: Use of rubber in modern world is so important; its application is from simple rubber insulator in electrical supplies to washers used in sealing of high pressure containers. Rubber can be either natural or artificial. Natural rubber is a simple agricultural product produced form tree called Para rubber tree or Hevea brasiliensis. Natural rubber on its raw state does not have much desired property for most application, the desired properties of natural rubber what we use is achieved by many chemical processes. During the time of Second World War the supply of natural rubber in Europe from Far East and South America was cut out and led to invention and commercial production of artificial rubber. (John S. Dick, 2003) Indentation test is important to materials like rubber because normal hardness test methods like Rockwells hardness tests are difficult to carry out on materials like this. Instrumented indentation can be used to test ceramics, polymeric and biological materials. In instrumented indentation test a controlled force or displacement is applied and is measured continuously and simultaneously over the whole loading - unloading cycle. Instrumented indentation or nano indentation test uses very small force and displacement and from the force displacement data it is possible to obtain many other properties of materials like modulus, stress strain relations etc. Indentation test can be done with different indentor tips, like spherical, diamond or conical, flat and so on. Spherical and flat indentors are used for testing thin rubber and the behaviour of both flat and spherical indentors are almost similar except flat indentors needs a slight more force than spherical indentors. Thin rubber is now widely used in many engineering and medical applications because of the advance in manufacturing to make it possible to manufacture as thin as in 0.001mm thickness rubber sheets. These thin rubbers are used in various applications like MEMS devices which include pressure sensors, valves and actuators in these devices. In medical application for the reconstruction of

tissues, cell seeded polymeric scaffold thin biomaterial are used. All this the performance depends on the mechanical properties of thin rubber used. Hence the characterization of mechanical properties likes youngs modulus, residual stress and the effects of force on deformation of thin rubber experimentally will help very much in improving the performance and will be able to predict the performance and service life. [17]

1.2 Aim and objective: 1) Study of the effect of indentor shape, size and loading rate on rubber of different thickness. 2) Find the Youngs modulus using a formula and the stimulation of indentation test on solid works with different youngs modulus and compare with the experimental results. 3) Find viscoelasticity of rubber with thickness of 0.2mm, 0.5mm and 1.0mm with indentor of different shape and radius. 4) Carry out indentation test on three different medical gloves from three manufactures with different properties.

1.3 Brief history of rubber Early days before synthetic rubbers are produced the only source of rubber was from trees. Even though many species of trees which can yield rubber are native to parts of Asia, Africa, Far East, the first noticeable mention about rubber was in fifteenth century in equatorial regions of South America. According to an article published by Massachusetts Institute of Technology in an article by Tech Talk rubber was used by Mayan people in ancient Mesoamerica for making rubber balls, hollow human figures, and used as bindings to secure axe heads to their handles as early as in 1600 BC. In early 16th century when first Europeans reached South America they observed the local population playing with a crude bouncing ball made out a white milk like fluid collected when bark of certain trees are cut. The elastic, high deformability, water resistant properties attracted Scientists in Europe. (Jim R. White, 2001) The scientific name of this species that produces natural rubber is Hevea brasiliensis. The first notable use of rubber was in the production of water proof garments. The disadvantages of this rubber garments was in original conditions this will become soft and sticky in summer and brittle in winters. In 1823 Charles Macintosh found a new way to minimise this defects and was by placing rubber between two textile fabrics and was called double texture waterproof garments or Macintoshes. In 1839 Charles Goodyear of Woburn, Mass, USA found another was to overcome the major disadvantage of rubber-susceptibility to temperature change. The method was combining rubber chemically with sulphur because of the trade depression Charles Goodyear made a little commercial progress. In the early stages of rubber history, rubber grades were not so important even though tests are conducted to distinguish between good and bad rubber. This test had a little commercial importance because these tests used to assist product development internally by large companies and had only visual standards. In late 1960s Malaysia introduced a new grade called technically

specified rubber (TSR) which changed commercial aspect of natural rubber. In early 1970s ASTM test become much important and by that time there was almost 22 official grades of natural rubber. (John S. Dick). Six grades technically specified rubber (TSR) by International Standard Organisation (ISO) are shown in table below. Parameters Grade: TSRCV 0.05 0.60 0.60 0.80

TSRL 0.05 0.60 0.60 0.80

TSRS 0.05 0.50 0.50 0.80

TSR10 0.10 0.75 0.60 0.80

TSR - 20 0.20 1.00 0.60 0.80

TSR50 0.50 1.50 0.60 0.80

Dirt content Ash content Nitrogen content Volatile matter

Table 1.1: TSR's Specified by ISO under ISO-2000, in percentage weight of the maximum weight

From 19th century applications of rubber is increasing constantly. Even though rubber is used in many applications like in automobiles the locations are not easily visible. Many applications and devices like automobile tires, medical gloves, footwear, belts, wires and cables in machineries, many sport utilities, waterproof fabrics wont be exist in the present form if rubber was not discovered. A modern passenger car will have as many as 600 rubber parts. Any problem with this rubber parts because of its quality or manufacturing defects could lead to problems from its performance to a complete failure of the whole vehicle. Even though the history of rubber industry started about more than two hundred years still research and development works are continuing. To suite new application the rubber is constantly modified, new improved manufacturing methods, adoption of new additives, new techniques used for recycling are changing rubber day by day. (Jim R. White, 2001)

1.4 Literature review: Natural rubber Natural rubber is collected from trees called Para rubber of family called Euphorbiaceae and the species is Hevea brasiliensis. There are a number of other species like Parthenium argentatum also known as Guayule rubber, Manihot glaziovii also called Ceara rubber, Ficus elastic also called India rubber but rubber from these species have several disadvantages like extraction process is difficult, low rubber content or high resin. The rubber latex will be present in latex vessels on in the bark of Para rubber trees which will be under a pressure called turgor pressure at 1MPa to 1.9 MPa. Latex is extracted by making a small shave of bark of about 1 mm deep, this process is called tapping. Latex which flows down through the cut is collected in a small vessel. (Jim R. White, 2001) There are different ways of collecting rubber from latex. The most widely used method includes coagulation in which latex obtained is mixed with half of water and with acids like acetic acid (CH3COOH) or formic acid (HCOOH) to make latex coagulate in 12 hours. After about 12 hours coagulum of rubber in the form of solid slabs is formed. These solid slabs are squeezed to take out most of its water contents and other residuals and make it thin to about 3 mm. This are the passed through another set of rollers have a criss-cross pattern on them which are formed on the coagulum. These sheets are kept in a closed room called smoke house on wooden frames where it is dried. In smoke room hot smoke contains creosote is produced by burning lump of dry wood. This prevents rubber from oxidation, fungus, mildew etc. The rubber thus produced is called ribbed smoked sheet. This rubber is shipped to industries and different additives and manufacturing process are selected according to the applications and product to be produced. (Mikell P. Groover, 2010)

1.5 Synthetic Rubber The scared uses and applications of rubber due to it indiscipline behaviour changed in early 1900 when the first motor vehicle rolled out. The wide use of rubber tires in motor vehicles caused an explosion in rubber prices. As the plantations were unable to support the huge demand of natural rubber researches to manufacture rubber artificially was started by many countries and industries. In 1930s Germany started the commercial production of first artificial rubber called Buna-S (styrene butadiene co polymer). Later United States modified styrene butadiene and manufactured on a large scale under the name Government Rubber Styrene widely known as SBR and is still widely used in rubber industry. (Andrew Ciesielski, 2000) 1.6 Common vulcanized rubber compounds Natural rubber: Natural rubber which is one of the most common forms of rubber is widely used for automobile tyres, anti vibration and other similar mountings. Some of the qualities of natural rubber are it got a better fatigue resistance, good strength, a wide range of hardness can be obtained by varying the compounding process and compounds. Styrene- butadiene rubber: Styrene- butadiene rubber also known as SBR resembles some of the properties natural when is compounded with reinforcing fillets rubber but certain properties are better than the natural rubber like abrasion resistance, fatigue resistance. SBR is commonly used for

manufacturing of tyres of heavy vehicles. Chloroprene rubber: Chloroprene rubber is also known as poly chloroprene is used in harsh environments. Chloroprene rubber is much resistant to most chemicals, ozone, oil and even resistant to high temperatures. Ethylene propylene rubber: Ethylene propylene rubbers also known as EPM have similar properties that of SBR but EPR have a better resistance to atmospheric aging, oxidation and weather resistance. EPM is crossed liked with

sulphur can be used in sealing strips of automobile windows, seals in washing machines and radiator hoses in automobiles. (Peter C Powell, 1983) 1.7 Chemical structure Chemically rubber is a polymer with a continuous chain of isoprene whose chemical formula is (C5H8) n. Rubber can be either natural or artificial. Rubber is considered as an elastomeric and hence rubber materials usually have low Youngs modulus and high yield strain. Natural rubber is usually very soft, can be deformed into different shape by applying small heat and becomes brittle under low temperature. Rubber is a polymeric material which has a long molecular chain arrangement which is flexible and deform elastically. In order to make rubber into hard more durable a chemical process called vulcanization or vulcanisation is carried out which will have has superior mechanical properties than natural rubber. Vulcanization is a curing process in which sulphur is added at a high temperature. In this chemical process the polymer molecules are linked with other polymer molecules with sulphur atoms as bridges. This makes natural rubber a bulky material with much hardness and also much resistant to chemical attack and this was the first way used to improve the properties natural rubber. The bridging of sulphur also makes the surface smooth and less sticky. In 19th and 20th century addition of several solid particulates found to improve the mechanical properties of natural rubber. Composition of typical rubber used in industries is Para rubber Zinc Oxide Magnesia Java rubber China Clay Red Lead 83.3 53.3 20.0 16.7 10.0 6.7

Sulphur 6.2 (Rubber processing: technology, materials, principles by James Lindsay White)

The most important property of rubber that makes it so widely used is the high degree of deformation under a small force. It is been considered that steel is more elastic than rubber and it is true. The fact is that steel can be stretched not more than 2%, after steel wont be elastic. Rubber sometimes can be stretched to about few hundred percent and when the stress causing deformation is removed it can regain its original dimension without much stress remaining. The graph of tensile force vs. extension of rubber will be as shown below.

Figure 1.1: Typical tensile versus extension curve for rubber (L. R. G. Treloar)

For rubber the stress strain graph will not be linear as shown in the above graph so Hooks law are invalid for rubber material. Youngs modulus is almost inapplicable for rubber material. For materials like steel which follows Hooks law will satisfy Hooks law only up to an elastic limit which is usually 2%. In rubber up to 2% or more than 2% the stress strain curve is linear. From figure 1, it can be seen that for an extinction of less than 50% the curve can be considered as linear and as the strain increases strain abruptly increases shows its deviation from its linear path. However rubber is a material which is elastic up to several hundred percentage and hence it cannot be considered as a material which follows Hooks law. For an extinction of more than 100% rubber becomes softer. The other factors affecting youngs modulus are temperature and loading rate. If temperature increases youngs modulus will decrease. For small change in loading rate will not affect too much on youngs modulus but a large change have some effect on youngs modulus (Andrew Ciesielski, 2000) Some other properties are: Elasticity Good electric insulation Resistance to tear Resistant to many chemicals, oil etc

1.8 Thermo elastic properties Thermo elastic property is a mechanical property of rubber. The study on thermo elastic properties started in early 19th century when John Gough an English scientist observed two things about rubber. When rubber is stretched by a constant load and was held for a long time it changes its dimension like length, area etc but in most of the cases rubber contract reversibly under heating. When rubber is stretched quickly it gives out some heat. Even Gough observed thermo elastic properties of rubber in 1805, his findings where conformed after some 50 years by Joule in 1859. Joules experiments where contacted on vulcanized rubber which was unavailable when Goughs experiments were carried out. These two thermal effects of rubber are now known as Gough Joule effects. Figure 2 shows the second effect of thermo elastic property of rubber when rubber is stretched to 100 percent to produce a temperature of 0.20K.

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Figure 1.2: shows heat produced when a rubber strip is stretched up to 100% (L. R. G. Treloar, Page 38, 2005) Thermo elastic properties are not only observed for natural rubber but for a wide range of materials in rubber like state, like most variety of synthetic rubber polymers. (L. R. G. Treloar, 2005) 1.9 Viscoelasticity: Viscoelasticity in simple words can be defined as the property of certain materials which can be viscous but exhibits elastic properties. Even rubber can be considered as elastic material but rubber exhibits certain properties of viscous materials. In indentation test of rubber of thickness 0.2 mm, 0.5mm and 1.0mm, thicker rubber stores more energy than thin rubber i.e. thicker rubber shows more division from elastic characteristics. Viscoelasticity in rubber can be considered as a combination of two different mechanisms which will be exhibited at same time. The mechanism can be considered as spring and dashpot where spring represents elastic behaviour of

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rubber and dashpot represents viscous part. As we know the behaviour of spring and dashpot is different. When a force is applied causing a deformation on a spring dashpot combination system the behaviour of system will be different than spring and dashpot considered individually. When a force is applied to a spring, the deformation on the spring is stored as energy and this energy is released when the spring returns to its original state. Where as in dashpot when the piston moves the piston has kinetic energy and this energy is converted into heat and it is irreversible. The piston will not have energy to return to its original state.

Figure 1.3: The figure represents rubber with viscous and elastic components by using Maxwell and Voights models. (Andrew Ciesielski, 2001, page 128)

The above figure (figure 3) represents the concept of Maxwell and Voight model. In Maxwells model spring and dashpot are arranged in series and in Voight model spring and dashpot are arranged in parallel. In applications Maxwells model is widely used for stress relations experiments and Voight models is used in experiments with creep. Both Maxwell and Voight can describe dynamic and mechanical experiments but Voight model is widely used. Viscosity component can explain some of the engineering properties like creep, stress relaxation. (Andrew Ciesielski, 2000)

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1.10 Creep: Creep can be defined as the change in strain with time when the stress is constant. From an example when a load is kept over a rubber block the thickness of rubber block will decreases with time even the load is kept constant. As the time progresses the thickness will continues to decrease but the rate will be decreased as time advances. In a couple of weeks this rate will becomes extremely small and this phenomenon is called creep. For a very short time creep is very difficult to predict accurately but for a long time period it can be predicted with much accuracy. Creep at room temperature is proportional to the logarithm of time but as temperature increases creep also increases. Creep is occurring in rubber because of viscous component in rubber hence more viscous the rubber is the more the creep level. 1.11 Stress relaxation Stress relaxation can be considered as the inverses of creep. Stress relaxation can be defined as change in stress as time changes while the strain is constant. In some applications of rubber as in seal or gasket will fail due to stress relaxation. Seal or gaskets are used to prevent leak, leak could be of pressure leak or fluid or air under pressure. Rubber kept as seals will be kept under compression inside the housing. Rubber sealing will exert a force against the housing and this force will keep it from leakage. The force is due to both viscous and elastic components. As time passes the force acting against housing will reduce and finally the seal will become unable to hold the pressure of fluid without leak. This is due to the phenomenon called stress relaxation. Stress relaxation will increases as viscous component increases in rubber. (Andrew Ciesielski, 2000)

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1.12 Elastic behaviour of rubber There is a number of theorys suggesting the elastic behaviour of rubber. One of the theories was by Ostwald in 1926. According to his theory elasticity is because of a serious of networks of electrically charged molecules of proteins or resins from the outer parts of latex globule suspended in a semi liquid medium of hydrocarbons. This rubber hydro carbons usually have a lower density than and molecular weight than latex globules. Another theory was by Fikentscher and Mark in 1930 known as helical spring theory. In helical spring theory the retraction force occurs because the force between two adjacent turns of helix. All this theories are able to explain the retraction force of rubber and some of its elastic properties but was unable to explain thermo elastic properties and was unconvincing about the interpretation of mechanical properties. Generally accepted theories of elasticity of rubber are Meyer, Valko and Kerrer and von Susich. According to Meyer larger amplitudes of vibration is produced by atoms thermal energy in long chain molecules. Atoms thermal energy is created because of the external force which pulls rubber strip. The vibrations will be greater in the direction perpendicular to the chain rather than the vibration in the direction of chain. The uneven vibration along the chain will cause a repulsive force along the parallel and extended chains. This repulsive force between parallel and extended chains will cause rubber to retract. This theory is now widely accepted as the theory of elasticity of rubber. (L. R. G. Treloar, 2005)

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1.13 Load Displacement curve Indentations tests are carried out to obtain a force displacement diagram and thus to obtain elastic modulus, hardness of the test material. In a load displacement diagram load will be plotted along the X axis and load will be along Y axis. In a typical indentation test load is applied from zero on the test specimen to a certain maximum force and then the load is decreased from the maximum value back to zero load. (Figure A4, figure A5) Since rubber beaver is as of an elastic material indentation tests will not make any impression on the rubber test specimen. As in materials like forms the indentation is more likely to plastic deformation rather than to elastic deformation. In plastic deformation more energy stored rather than elastic material and also some residual impression is left on such materials. When the indentor (load) is removed the material will try to regain its original shape back and to some extended it will regain its shape because of the relaxation of elastic strain in the material but full recovery is prevented due to its plastic deformation. In nano indentation tests the depth of penetration due to plastic deformation will be so small and can be found accurately by modern optical measurement techniques and can be used in measurement of hardness. 1.14 Tests on rubber The important purpose of testing are to predicting service performance: It should be possible to predict service. To get more satisfactory results the test conditions should relates to service condition. It is better if the test is not extensively complex and extreme speed and inexpensive. There could be one or more reasons for testing. The most common reasons for testing could be for quality control purpose or for design data or to predict service performance or for investigate failure. There are some attributes related to each tests. (R. P. Brown, 2001) For a good design, production and quality control of goods the material properties should be known and is much important. There are many testing methods for different materials.

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1.15 Indentation Test Indentation test is a type of hardness test. In indentation test for rubber a hard indenter, can be of shapes like spherical, flat, berkovich which are commonly used indentors. This indentor is pressed against rubber which is under a certain tension. Indentation test or instrumented indentation or nano indentation is been used to test some of the mechanical properties of materials like metals, ceramics, polymers, biological materials and so on. (Mark R. VanLandingham, 2003) Indentation test also known as micro indentation, ultramicro indentation, nano indentation etc. In nano indentation, test is carried for load and displacement on nano level, less than 100nN or 100nm respectively. For thin rubber sheets of thickness less than 1mm the ideal experiment method is instrumented indentation to understand mechanical properties like elastic modulus, onset of nonlinear elasticity, loss tangent, creep compliance, energy dissipation etc. In indentation test it is possible to obtain good accurate force displacement results and also a small material volume is required for the quantitative analysis. Indentation test can be conducted by changing either load or displacement and in both cases is noted against time. In most of the indentation test are carried out by changing the load and can be considered as load controlled test equipment. According to ISO 14577, part 1 which specifies the indentation tests for finding different material parameters and hardness are defined in three ranges as shown in table below. Where F is force in Newtons and h is the depth of indentation. (Anthony C. Fischer-Cripps, 2004) Macro indentation range 2 N F 30000 N Micro indentation range 2 N > F, h> 0.02 micro meter Nano indentation range h 0.02 micro meter

Table 1.2: Different ranges in indentation tests

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Indentation tests are used for several applications. Indentation tests can be used for the analysis of different properties of materials like hardness of material, creep of material, viscoelasticity, cracking point, toughness, and stress and strain graphs and so on. Indentation can be used for materials of various thickness according to the force used for indentation. For example since the force used in nano indentation is less than one Newton and the deformation is so small, nano indentation can be used for materials of very small thickness such as thin surface films. 1.16 Working of indentation test equipment: Another name for indentation test is depth-sensing indentation. In this experiment a load is applied on an indenter and the displacement of indentor is measured simultaneously. By knowing the material properties and geometry of indentor tip and with the load displacement results mechanical properties of rubber can be find. The indentation depth can be varied from few nanometres to several millimetres.

Figure 1.4: Figure shows the common arrangements in indentation testing instrument. (Journal of Research of the National Institute of Standards and Technology Volume 108, Number 4, July-August 2003)

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In indentation test a device used for producing displacement is usually an electric motor or electromagnetic actuators that can produce very accurate displacement. Once the signal for motion reached the actuator from controller it will produce the same displacement as per the signal. There will be one or more sensors are used to measure the displacement produced by the actuator. The commonly used sensors are load cells. The controller can either produce the required force or displacement. The force from actuator is transferred to the tip of indentor which will cause the effect on the sample. The load cell measures the displacement continuously and can produce it against time or force. Indentation test have several advantages over conventional hardness tests like Rockwell hardness tests. In indentation systems a specific force or displacement can be applied and can be simultaneously controlled and measured over whole load cycle. Indentation test also have very high resolution of force and displacement. This resolution can be as low as 1 N of force and 0.2 nm displacement. The hardness of rubber is determined by the size of indentor and shape of indentor.

Commonly used indentors in testing of rubber are flat indentor and spherical indentor. Flat indentor will have a flat surface and spherical will have spherical tip. Flat indentor has certain advantages and disadvantages over spherical indentor. In flat for low loads the force is distributed all along the flat surface but as load increases more load will be acting on the circumference or corners of the flat surface sometimes will causes errors or even can damage the rubber. In spherical indentor as the load increases the area of contact between rubber and spheres increases will cause slight error as load increases.

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1.17 Difference between Indentation tests and other hardness tests Indentation testing can be also called as hardness testing because both are used for finding the quality, character and for quality control of different materials. The difference is only on the methods carried out. In conventional hardness tests like in Rockwells hardness tests a constant force is applied on the material and will do for a particular span of time. The tip used for such tests will have a specific geometry and specific material. This tip will be pressed with a constant force against the materials to be tested which will makes a hardness impression on the testing material. This impression could be so small; the dimensions of the impression could be in the order of millimetres. The value of hardness depends on the depth of penetration made by tip. In Rockwells tests and the other conventional tests the result of hardness will be a dimensionless single value. (Mark R. VanLandingham, 2003) For example Rockwell hardness has different scales according to different tips used. Table below shows some of the scales and material and geometry of tips used. Scale A B Indentor tip Diamond cone (120o) Steel sphere(1/16 inch diameter sphere) C D E Diamond cone (120o) Diamond cone (120o) Steel sphere(1/8 inch diameter sphere) F Steel sphere(1/16 inch diameter sphere) Table 1.3: Table showing the different types of indentors used, the total load and youngs modulus in Rockwells hardness test. 60 kgf 130 150 kgf 100 kgf 100 kgf 100 100 130 Total load 60 kgf 100 kgf Youngs modulus(E) 100 130

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There are different scales after F but all the tips after are steed balls with different dimension, load and youngs modulus. The most commonly used scales are B and C. Scale A is commonly used for hardest materials like tungsten carbide, titanium alloys etc. Scale B is used for common materials like brass, aluminium soft steel and other soft materials and scale C is used for hard steel. Whereas instrumented indentation can not only used for testing metals but can also be used to test ceramics, polymeric and biological materials. In

instrumented indentation test a controlled force or displacement is applied and is measured continuously and simultaneously over the whole loading unloading cycle. Instrumented indentation or nano indentation test uses very small force and displacement. Rockwells test and instrumented indentation tests are been used for a long time but Rockwells test havent changed much in recent times but instrumented indentation have changed due to the development in control of force and displacement by user more precisely, new powerful software and hardware, high response time in measurement instruments, sensitivity made instrumented indentation more popular.

Indentation technique is now widely used for research propose for the analysis of dimensions and finite element analysis and to study the behaviour from force displacement curve from actual instrumented indentation test and can even predict stress strain curves behaviour. (Mark R. VanLandingham, 2003) 1.18 Applications of rubber Common applications of rubber are in medical applications like medical gloves, catheters tubes, surgical and veterinary apparatus, condoms, swimming caps, balloons, rubber bands, automobile tyres, O rings, hoses, buffer and bearing springs for carriages, piston and washers, air pump valves, inking rollers of printers, flexible joints for pipes, insulations for electrical wires. According to an article published by Massachusetts Institute of Technology in an article by Tech Talk rubber the first rubber was ever used was in 1600 BC by Mayan people of ancient Mesoamerica. They used rubber for making rubber

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balls, hollow human figures, and used as bindings to secure axe heads to their handles. Thin rubber is now widely used in many engineering and medical applications because of the advance in manufacturing to make it possible to manufacture as thin as in 0.001mm thickness rubber sheets. These thin rubbers are used in various applications like MEMS devices which include pressure sensors, valves and actuators in these devices. In medical application for the reconstruction of tissues, cell seeded polymeric scaffold thin biomaterial are used. All this the performance depends on the mechanical properties of thin rubber used. Hence the characterization of mechanical properties likes youngs modulus; residual stress and the effects of force on deformation of thin rubber experimentally will help very much in improving the performance and will be able to predict the performance and service life. [17] 1.18a Medical gloves Medical gloves are usually made from latex. Medical gloves are used as safety accessory to limit patients exposure to infectious matters and to ensure sanitary hospital conditions and also to protect health of professionals from diseases. The two common types of medical gloves are exam, and surgical gloves, of which surgical gloves should be more reliable, should not rip or tear and should be more precise. Gloves are also used by emergency medical technicians, police persons, and fire persons. In the manufacturing of gloves starts with mould which have the shape of hand or sometimes with a forearm. This mould is dipped in a bath of natural rubber latex, forming thin polymer latex coating on the mould. This set is heated to a slight more temperature and then is removed from the mould. Thus gloves are formed.

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1.18b Catheter tube Catheter tube is used to insert into body, duct, vessel etc for injection of fluids or drainage of body fluids or for access to surgical instruments into body. Catheter tube is flexible tube made from rubber latex. Certain properties of latex which makes it most suitable for catheter tube are latex can be made into thin, can be very flexible, can be made soft and long. Catheter can be sometimes left inside the body, temporarily or permanently. So rubbers without aging or resistant to body fluid are widely used for catheter tubes. 1.18cTyres Most of the rubber produced in world is used for the production of rubber tyres. In the manufacturing of tyres natural rubber is thickened by drying, during this process additive like carbon black is added. Carbon black will give rubber its black colour. Tyre is not made with just rubber it is a product made up of polymers, rubber, fabric and thin steel reinforcements. In rubber tyres different proportions of natural rubber and artificial rubber is mixed with different fillers like carbon black, silica and some more chemicals to make rubber tougher. Next phase is the assembly of various rubber parts and the finishing operations. Another important use of rubber in automobile industry is the coolant hoses. In recent years as a way to improve fuel efficiency new ways like turbo charging, power assist devices, emission control etc the under hood temperature also increases resulting in reduced life of coolant hoses. In 1988 the goal of coolant tubes was 100,000 miles but now the improved manufacturing process and advanced method of testing and predicting the life of coolant tubes, a life time of 10 years or 150,000 mile have achieved.

1.18d Rubber adhesives Rubber latex is also used as bonding and sealants, most popular is building industries. Now most of the cases instead of natural rubber synthetic rubber

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latex are used, which are based on styrene and butadiene polyvinyl acetate and acrylic ester latex. The properties such as relatively stable cost, good weathering resistance, latex adhesives exhibits flexibility makes popular for non structural applications. Now latex adhesives are used in applications where mechanical properties of joints are more important. One way to predict deformations and stress distribution in rubber is by FMA or Finite Element Analysis using ABAQUS, SolidWorks or any similar numerical methods. 1.18e Vibration Isolation and shock absorbers Vibration isolators are used to provide a low resonant frequency for a suspended mass to make the amplitude of vibration small. Many machine will produce a high vibration during there working this could damage the structure on which the machine is kept and also the other equipments and machines attached. Rubber has a good vibration isolation property because of its elastic property. Depending on the kind and amount of vibration the rubber is selected for vibration isolation applications. Rubber used as vibration isolator will be under a constant load which will cause creep so rubber with slight high carbon content is used in vibration isolation applications. Shocks absorbs are used to stop moving object without transmitting the unwanted load to the unnecessary parts. Shock absorbs will reduce the speed of a moving part with a resistive force. Rubber shock absorbers are designed to have some degree of flexibility, a particular dynamic stiffness so rubber shock absorbs can undergo some large deflection before bringing the part to a total stop. One of the advantages of rubber is its non linear elastic response. One of the required characteristic of shock absorber is as deflection increases shock absorber should get softer so the resistive force could be constant for all the deflection range. This also helps the shock absorber to work with least deflection. Rubber used as shock absorber should also have a little internal damping to the reduce rebound. (Alan N. Gent, 2001)

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1.19 Finite element analysis

Finite element method which is also known as FEM is used to find the numerical solution of partial differential equations and integral equations. In strict mathematical view finite element method can be considered as an integral formulation. Finite element method can be used in mechanical industries for solving the design in aeronautical, automobile and so on. Most of the finite element software will have several ways of analysis like stress, thermal, fluid, electromagnetic and so on. For solving by using finite element method the model will be divided into a finite number of small elements all have the same properties as the whole part of that model. These small parts are connected together at different nodes. The nodes can be considered as pins or the gloved points that holds the whole elements together. For each node there will be an algebraic equation and the by solving these equations simultaneously will forms the solution. The accuracy of the finite element method improves as number of mesh increases or as the mesh size decreases. As the mesh size increases the nodes will also increases and the number of algebraic equation also increases. This makes the model to take more time for finding the solution and hence the mesh size is limited in most cases. The above figures (figure 1.8, 1.9) are the finite models developed for the experimental set up of the cylinder with 10 mm chamber size and the flat indentor of radius 2 mm. The figure 1.8 represents a finite element model with mesh size 1 mm generated in SolidWorks and the figure 1.9 represents the finite element model with mesh size 2 mm. It can be observed that the mesh number is much more in mesh 1 mm than mesh 2 mm and hence the time needed for solving mesh 1 mm will take a lot more time and memory than mesh size 2 mm.

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Figure 1.5: Mesh size 1 mm with cylinder with chamber size 10 mm, rubber and flat indentor

Figure 1.6: Mesh size 2 mm with cylinder with 10mm radius, rubber and flat indentor with radius 2 mm

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Finite element methods have several advantages and the important advantages are by finite element methods it is possible to solve the most complex geometry. Finite element method can solve the most complex shape once its mathematical model is generated and only for the modelling human assistance is needed. Finite element method can not only be used for solid mechanism like stress or displacement, it can also used for heat problems, electrostatic problems, fluid problems and so on. By finite element the load can be applied even on a point (nodal loading). The loading can be applied can includes pressure, thermal, viscous, inertia etc. The loading rate can also be varied by using finite element methods. Even though finite element methods have several advantages the solution is only approximated, it cannot be always the same in real cases. The advance in software and the robust in computer hardware make the finite element process more precise and accurate than ever before.

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CHAPTER 2:

EXPERIMENTAL WORKS

The experiment was carried out on the experimental set up as shown in figure 2.1. The figure 2.2 shows an iron flat table on to which the specimen to be tested are kept and also the frame which carries the screw mechanism to lift the actuator and sensor assembly is attached. The inputs are given through a computer having an interface called LinkMot, and its visual display called LinkMot Talk R1.3.12. Once the required displacement is given to the control unit it will produce the same force for 3 mm displacement. This displacement and force are continuously and simultaneously measured against time and is recorded on to the computer attached. These values of force and displacement are used for further calculations and different graphs.

Figure 2.1: Indentation testing equipments shows screen where output will be displayed and the frame to which the load cells are attached.

27

Figure 2.2: Rubber of thickness 1 mm attached on brass cylinder of chamber size 15mm during testing.

Figure 2.3: Output display showing the loading and unloading curves on testing 1 mm thick rubber on a chamber radius of 15 mm.

28

From the figure 2.3 the red curve is the reference line and the blue line is the experimental results. According to the displacement or force needed the reference line can be changed and hence the displacement can be set. 2.1 Different chamber size used

Figure 2.4: Brass cylinder with a chamber radius of 5 mm.

Figure 2.5: Brass cylinder with a chamber size of 10 mm.

29

Figure 2.6: Brass cylinder with a chamber radius of 15 mm. 2.2 Different rubber used in testing

Figure 2.7: Natural rubber with 0.2 mm thickness.

30

Figure 2.8: Natural Rubber with thickness of 0.5 mm.

Figure 2.9: Natural rubber with thickness of 1 mm

31

Figure 2.10: Chamber radius of 15 mm fitted with 1 mm thick rubber for experiment.

2.3 Different indenters used

Figure 2.11: Flat indentor with 4 mm radius.

32

Figure 2.12: Spherical indentor with 4 mm radius.

Figure 2.13: Flat indentor with 2 mm radius.

33

Figure 2.14: Spherical indentor with 2 mm radius.

2.4 Three kind of gloves used

Figure 2.15: Blue rubber gloves of 0.12 mm thickness.

34

Figure 2.16: White rubber gloves of 0.03 mm thickness.

Figure 2.17: Yellow rubber gloves of 0.14 mm thickness.

35

2.5 Four test on each rubber of thickness 0.2mm, 0.5mm, 1.0mm to show repeatability

Four tests on 0.2mm thickness with flat intentor of 2 mm radius

1.4 1.2 1

Force (N)

0.8 0.6 0.4 0.2 0 -0.2 0 0.5 1 1.5 2 2.5 3 3.5 4 Displacement (mm)

test 1 test 2 test 3 test 4 Poly. (test 4)

Figure 2.18: Tests with flat indentor of radius 2 mm on rubber sheet of thickness 0.2mm to show repeatability. In the test with flat indenter of radius 2 mm on rubber with thickness 0.2 mm the curve is not linear, (test 2, figure 2.17) until a displacement of 1 mm the slop is less than the slope after 2 mm displacement. This is because in rubber the rate of deflection increases as the force increases. The data obtained from four test overlap and hence we can conclude that the test with flat indenter of thickness 2 mm on 0.2 mm thin rubber is repeatable. The force varying is not more than 0.1 N at any point so the four tests can be considered as repeatable.

36

Four tests on 0.2mm thickness with sphrical intentor of 2 mm radius

1

0.8

0.6

Force (N)

test 1 0.4 test 2 test 3 0.2 test 4

0 0 -0.2 0.5 1 1.5 2 2.5 3 3.5

Displacement (mm)

Figure 2.19: Tests with spherical indentor of radius 2mm on rubber sheet of thickness of 0.2mm to show repeatability. In the test with spherical indentor of radius 2mm on rubber with thickness 0.2 mm (figure 2.19) all the four curves obtained from the four tests are one over the other and hence the tests can be considered as repeatable. As from the black curve (test 4) it can be see that the slope is not a constant. The slope is slightly less initially till 1 mm displacement and from there on the slope increases as the force and displacement increases almost similar as that of with flat indentor of radius 2 mm on 0.2 mm thick rubber (figure 2.18).

37

Four tests on 0.5mm thickness with flat intentor of 2 mm radius

3 2.5 2

Force (N)

1.5 1 0.5 0 0 -0.5 0.5 1 1.5 2 2.5 3 3.5 4

test 1 test 2 test 3 test 4

Displacement (mm)

Figure 2.20: Tests with flat indentor of radius 2mm on rubber sheet of thickness of 0.5 mm to show repeatability. For the tests with flat indentor of radius 2 mm on rubber with thickness 0.5 mm is plotted as per the data got from indentation test is shown is figure (figure 2.20). It can be seen that all the four tests results are comparable. In all the curves the slope slightly increasing as the force and displacement increases.

38

Four tests on 0.5mm thickness with spherical intentor of 2 mm radius

2.5 2 1.5

Force (N)

test 1 1 0.5 0 0 -0.5 0.5 1 1.5 2 2.5 3 3.5 test 2 test 3 test 4

Displacement (mm)

Figure 2.21: Tests with spherical indentor of radius 2mm on rubber sheet of thickness of 0.5mm to show repeatability. The figure 2.21 shows the force displacement curves of four tests. Curves of four tests are overlapping each other and hence the tests are repeatable. Slop of force-displacement curve is slightly increasing as force or displacement increases.

39

Four tests on 1.0mm thickness with flat intentor of 2 mm radius

4.5 4 3.5 3

Force (N)

2.5 2 1.5 1 0.5 0 -0.5 0 0.5 1 1.5 2 2.5 3 3.5 4 Displacement (mm)

test 4 test 1 test 2 test 3

Figure 2.22: Four tests with flat indentor of radius 2mm on rubber sheet of thickness of 1 mm showing repeatability. In the above figure 2.22 shows the repeatability with flat indentor of radius 2 mm on rubber of thickness 1 mm. Slope of the curve is relatively less for small force and displacement and increases as force and displacement increases.

40

Four tests on 1.0mm thickness with spherical intentor of 2 mm radius

4.5 4 3.5 3

Force (N)

2.5 2 1.5 1 0.5 0 -0.5 0 0.5 1 1.5 2 displacement (mm) 2.5 3 3.5

test 1 test 2 test 3

Figure 2.23: Tests with spherical indentor of radius 2mm on rubber sheet of thickness of 1.0mm to show repeatability. In the figure 2.23 the curves from the three tests are overlapping each other so for spherical indentor with a radius of 2 mm on rubber of thickness 1 mm can be considered as repeatable. With flat and spherical indentor with radius 4 mm on rubber of thickness 0.2 mm, 0.5 mm and 1.0 mm shows a similar curves as in that of flat and spherical indentor with radius 2 mm on rubber of thickness 0.2 mm, 0.5 mm and 1.0 mm and are repeatable.

41

2.6 Test with different loading rate

Force Vs displacement
6 5 1 sec 4 2 sec 4 sec 10 sec 2 1 0 -0.5 -1 0 0.5 1 1.5 2 2.5 3 3.5 15 sec 20 sec 40 sec 100 sec

Force (N)

displacement (mm)

Figure 2.24: Force displacement curves showing different loading rate on 1 mm thick rubber. The above figure (figure 2.24) shows the force displacement data for rubber of 1 mm thickness under different loading rate, from 1 sec to 100 sec for 3 mm displacement.

42

2.7 Loading-unloading graph

Force Vs Displacement
1.4 1.2 1 0.8

Force (N)

0.6 0.4 0.2 0

loading unloading

-1

-0.2 -0.4

Displacement (mm)

Figure 2.25: Force displacement curve on 0.2 mm thick rubber with flat indentor of 2 mm radius showing the loading and unloading curves. The above figure is obtained when the whole cycle of both loading and unloading is considered during the experimental process. Unloading part is important to find viscoelasticty, creep, amount of plastic deformation and similar properties. In the above figure (figure 2.25) both the loading and unloading curves overlapping each other and is relatively high in higher loads or displacement. That means the rubber of thickness 0.2 mm behaves perfectly elastic at higher loads than at loads of less than 0.8 N. In appendix A1, A2 shows the loading and unloading curves of 0.5 mm and 1.0 mm thick rubber.

43

2.8 Test on three different gloves

3 different glove with flat indentor

6 5

Force (N)

4 3 2 1 0 0 2 4 6 displacement (mm) blue gloves (flat) yellow gloves (flat) white gloves (flat)

Figure 2.26: Force displacement figure with flat indentor of 2 mm radius on three different rubber gloves. Figure above (figure 2.26) represents the result of indentation test carried out on three different kinds of gloves. The thicknesses of gloves are 0.03 mm for white, 0.12 mm blue and 0.14 mm for yellow gloves.

44

Chapter 3: Results and discussions

3.1 Comparison of flat and spherical indentor

ForceVs dispalcement with spherical and flat indentors of 2mm for different thickness
4.5 4 3.5 3 Flat R2 at 0.2mm Flat R2 at 0.5mm Flat R2 at 1.0mm sphericalR2 at 0.2mm sphericalR2 at 0.5mm spherical R2 at 1.0mm 0.5 0 -1 -0.5 0 1 2 3 4 displacement (mm)

Force (N)

2.5 2 1.5 1

Figure 3.1: Tests with spherical and flat indentor with radius 2 mm on rubber sheet with thickness 1 mm, 0.5 mm and 0.2 mm shows not much difference.

By comparing the data obtained from flat and spherical indentor of 2 mm radius (figure 3.1) the force needed for same displacement is almost same for both flat and spherical indentors on rubber with diameter 0.2 mm, 0.5 mm and 1.0 mm but flat indentor needs a slight more force than spherical indentor. For rubber of thickness 0.2 mm for same displacement of less than 0.75, flat indentor needs slightly more force than spherical and from there after the force is almost equal for both flat and spherical indentors.

45

Force-displacement of 4mm indentor radius

7 6 5 Flat R4 for 0.2mm Flat R4 for 0.5mm Flat R4 for 1.0mm spherical R4 for 0.2mm spherical R4 for 0.5mm 1 0 -1 0 1 2 displacement (mm) 3 4 spherical R4 for 1.0mm

Force (N)

4 3 2

Figure 3.2: Tests with spherical and flat indentor with radius 4 mm on rubber sheet with thickness 1 mm, 0.5 mm, 0.2 mm shows flat indentor need slight more force than flat.

The above figure (figure 3.2) shows the graph plotted from data obtained by indentation test with flat and spherical indentors both with a radius of 4 mm. Form the graph for both spherical and flat indentors of 4 mm radius have same effect on rubber of thickness 1 mm, 0.5mm and 0.2 mm. In a careful examination of figure 3.2, curves for flat indentor can be found slightly high than spherical indentor. This is because of the penetration effect of spherical indentor. In flat indentor for a radius 4 mm the rubber under the indentor will not expand as the rubber under the spherical indentor so flat indentor needs a slight more force than spherical indentor.

46

3.2 Maximum force and slope on different thickness of rubber with 2mm indentor

Maximum force needed for 3 mm displacement with flat indentor of 2mm radius
4 3.5 3

Force (N)

2.5 2 1.5 1 0.5 0 0 0.2 0.4 0.6 0.8 1 1.2 Thickness of rubber (mm) maximum force needed for 3 mm displacement with flat indentor

Figure 3.3: Maximum force needed for a displacement of 3 mm on rubber sheet with thickness 0.2 mm, 0.5mm and 1.0 mm. The above figure (figure 3.3) represents maximum force needed for a displacement of 3mm on rubber with thickness from zero to maximum thickness of 1 mm. It can be seen that slope of the curve is in larger at small thickness and reduces gradually as thickness increases.

Slope Vs thickness
1.2 1 0.8

Slope

0.6 0.4 0.2 0 0 0.2 0.4 0.6 thickness (mm) 0.8 1 1.2

Figure 3.4: Shows the slope of force displacement curve against different thickness of rubber with flat indentor of radius 2 mm.

47

The above figure 3.4 shows the slope of force displacement curve along y axis at different thickness shown along x-axis. It can be seen from the graph that the slope rapidly increases till a thickness of 0.5 and the slope tents to decreases thereafter.

Flat indentor with 2 mm radius Thickness 0.2 mm 0.5 mm 1.0 mm

Maximum displacement 3 mm

Maximum force

Slope of force displacement curve

0.75

0.251

3 mm 3 mm

2.4 3.4

0.829 1.108

Table 3.1: Shows the maximum displacement, maximum force and slope of force displacement curve for different thickness using flat indentor with 2 mm radius

48

3.3 Maximum force and slope for indentor 4 mm on different thickness of rubber

Maximum force for 3mm displacement with flat indentor of 4mm radius
7 6 5
Force (N)

4 3 2 1 0 0 0.5 1 1.5
Thickness of rubber (mm)

Maximum force for 3mm displacement with flat indentor of 4mm radius

Figure 3.5: The figure shows the maximum force needed for a displacement of 3 mm with different thickness. The slope is slightly more for thin rubber but the curves slope is reducing as thickness increases.

49

Slope Vs thickness for flat indentor with 4mm radius

2.5 2 1.5 1 0.5 0 0 0.2 0.4 0.6 thickness (mm) 0.8 1 1.2

Figure 3.6: The figure shows thickness on X axis and slope of force displacement curve on Y axis for rubber with 1 mm thickness. In the figure 3.6 represents the slope of force displacement curve and the different thickness of rubber on X axis. The line is almost a linear than the flat indentor with radius 2 mm (figure 3.4) but the slope have a tent to decreases as the as the thickness increases. Flat indentor with 4 mm radius Thickness 0.2 mm Thickness 0.5 mm Thickness 1.0 mm Maximum displacement 3 mm 3 mm 3 mm 1.6 N 3.6 N 6.4 N Maximum force Slope of force displacement curve 0.504 1.260 2.179

Table 3.2: Shows the maximum displacement, maximum force and slope of force displacement curve for different thickness using flat indentor with 4 mm radius

Slope

50

Spherical indentor with 2 mm radius Thickness 0.2 mm Thickness 0.5 mm Thickness 1.0 mm

Maximum displacement 3 mm 3 mm 3 mm

Maximum force

Slope of force displacement curve

0.7 N 2.1 N 3.1 N

0.245 0.696 0.963

Table 3.3: Shows the maximum displacement, maximum force and slope of force displacement curve for different thickness using spherical indentor with 2 mm radius

Spherical indentor with 4 mm radius Thickness 0.2 mm Thickness 0.5 mm Thickness 1.0 mm

Maximum displacement 3 mm 3 mm 3 mm

Maximum force

Slope of force displacement curve

1.2 N 3.3 N 5.9 N

0.436 1.10 1.96

Table 3.4: Shows the maximum displacement, maximum force and slope of force displacement curve for different thickness using spherical indentor with 4 mm radius

51

Maximum force needed for Flat indentor with radius 2 and 4 mm for 3 mm displacement
7 6 5

Force (N)

4 3 2 1 0 0 0.2 0.4 0.6 0.8 1 1.2 Thickness of rubber (mm)

Maximum force for 3mm displacement with flat indentor of 4mm radius Maximum force needed for 3 mm displacement with flat indentor of 2mm radius

Figure 3.7: Graphs shows the maximum force needed for a displacement of 3 mm on rubber of thickness 1 mm with flat indentors of 2 mm and 4 mm.

From the above figure (figure 3.7) the curves of flat indentor with radius of 4 mm have almost a constant slope than the indentor of 2 mm radius. The contact area is more for indentor of 4 mm radius and is more than four times for 4 mm radius flat indentor than the 2 mm radius flat indentor and hence the force is also more for 4 mm radius. The larger area of contact makes the curve more stable than the indentor of radius 2 mm. It can also seen that the difference of force between flat indentor radius 2 mm and 4 mm is have not much difference till 0.4 mm thick rubber but from 0.4 mm thickness the force difference between indentors of 2 mm radius and 4 mm radius increases dramatically.

52

3.4 Effect of rate of loading

As the times increases the force decreases slightly for flat indentor but it does not have much effect on spherical indentor.

Loading rate with flatR2 on 1mm

6 5 4 3 2 1 0 -0.5 -1 0 0.5 1 1.5 2 2.5 3 3.5 1 sec 2 sec

Force (N)

4 sec 10 sec 15 sec 20 sec 40 sec 100 sec

displacement (mm)

Figure 3.8: Force displacement data showing the effect of loading rate from 1 sec to 100sec with flat indentor with radius 2mm on 1mm thick rubber sheet. Figure 3.8 represents force displacement curve with flat indentor of radius 2 mm with rubber of thickness 1mm with different loading rates from 1 sec to 100 sec for a displacement of 3 mm. It can be seen that loading rate has not much effect on small changes of loading rates but for a large change in loading rates the slope changes, a small decrease in slope can be observed as loading rate increases.

53

Loading rate for flat R4

8 7 6 5 2 sec 4 sec 10 sec 15 sec 20 sec 2 1 0 -0.5 -1 0 0.5 1 1.5 2 2.5 3 3.5 displacement (mm) 40 sec 100 sec

Force (N)

4 3

Figure 3.9: Force displacement data showing the effect of loading rate from 2 sec to 100sec with flat indentor with radius 4 mm on 1mm thick rubber sheet. The figure above shows (figure 3.9) force displacement curve for flat indentor of radius 4 mm on rubber with thickness 1 mm. It can be seen that loading rate is not having as much effect it has on indentor with radius 2 mm. But still there is a slight effect on loading rate in indentor with radius 4mm. The slope of force displacement curve will reduces slightly as the loading rate increases so the force needed for a 3 mm displacement is less for a loading rate of 100 sec than 1 sec.

54

Force displacement curves for different loading rate

3.5 3 2.5 1 sec 2 sec 4 sec 1.5 1 0.5 0 0 0.5 1 1.5 2 2.5 3 3.5 displacement (mm) 10 sec 15 sec 20 sec 40 sec

Force (N)

Figure 3.10: Force displacement data showing the effect of loading rate from 1 sec to 40 sec with spherical indentor of radius 2 mm on 1 mm thick rubber sheet. The above figure (figure 3.10) shows force displacement diagram of 1 mm thick rubber on different loading rate from 1 sec to 40 sec with spherical indentor. The loading rate has some effect with indentor size of 2 mm similar to that of flat indentor with 2 mm. The slope tents to decrease as the loading time increases.

55

Loading rate spherical R4

6 5 1 sec 2 sec

Force (N)

4 sec 10 sec

15 sec 20 sec

40 sec 100 sec

0 -0.5 -1 0 0.5 1 1.5 2 2.5 3 3.5

displacement (mm)

Figure 3.11: Force displacement data showing the effect of loading rate from 1 sec to 100sec with spherical indentor of radius 4 mm on 1 mm thick rubber sheet. The above graph (figure 3.11) shows the force displacement curve of spherical indentor with a radius of 4 mm. It can be observed that loading rate have a slight influence on the slope of force displacement curves but the large indentors have slightly less influence on loading rate than smaller indentor.

56

3.5 Effect of indenter shape and size on force

7 6 5 Force (N) 4 3 2 1 0 flat R2 1mm flat R4 1mm spherical R2 1mm spherical R4 1 mm

Figure 3.12: Bar chart showing maximum force needed for a displacement of 2 mm on indenter shape with flat and spherical of radius 2mm and 4 mm shows force needed is slightly large for flat indentor. The above bar chart (figure 3.12) shows the maximum force needed for a displacement of 2 mm by flat and spherical indentors of radius 2 mm and 4 mm on rubber with thickness 1 mm. The maximum force needed for a displacement of 2 mm with flat indentors of radius 2 mm and 4 mm on rubber of thickness 1 mm is 4 N and 6 N respectively and for spherical indentors of radius 2 mm and 4 mm are also 3.9 N and 5.8 N respectively. It can be seen that the force needed for flat indentor is slightly more than spherical indentors it could be because the area of the tip of flat indentor is constant from the very starting of loading where as in spherical indentor the contact area with rubber will be slightly less in the initial stages of loading and as the loading increases the area of contact also increases. The spherical Indentor will also have a piercing effect and hence same displacement is obtained with less force.

57

3.6 Viscoelastic
Specimen calculation: Viscoelasticity for flat indentor with radius 2 mm on 0.2 mm thick indentor. Viscoelasticity can be found by the area between force displacement curves. By integral calculus to find the area between two curves can be found by subtracting the equation of curve with lower value from the curve with higher value and by integrating the resultant equation with limits with the two meeting points.

Calculation of viscoelasticity for 0.5 mm thick rubber on flat indentor with radius 2 mm

Equation for loading curve is y = 0.126x3 - 0.236x2 + 0.430x Equation for unloading curve is y = -0.016x3 + 0.123x2 + 0.056x Difference between loading and unloading curve (0.126+0.016) x3+ (-0.236-0.123) x2+ (0.430-0.056) x=0 0.142 x3 0.1466 x2 + 0.374 x =0 Integrating the above equation with limits (maximum and minimum force, 0 and 1.01 in this case) will give the area between loading and unloading curves and hence the viscoelasticity.
1.01

0.142 x3 0.1466 x2 + 0.374 x =0

58

0.142 (1.01)4 0.1466 (1.01)3 + 0.374 (1.01)2 - 0 4 3 2

= 0.0355 0.0488 + 0.187 - 0 = 0.271367

Loading unloading curve of flat indentor with radius 2mm on 1mm thickness
6 5 4 Force (N) 3 2 1 0 -1 0 1 2 displacement (mm) 3 4 y = -0.0192x3 + 0.102x2 + 1.3211x

y = -0.0082x4 + 0.0278x3 + 0.1909x2 + 0.7786x

unloading loading Poly. (unloading) Poly. (loading)

Figure 3.13: Above figure shows the loading (red) and unloading (blue) curve for flat indentor with radius 2mm on rubber sheet of thickness 1 mm.

59

Loading unloading curve of flat indentor radius 2mm on 0.5 mm thickness

3 2.5 2 y = 0.0091x4 - 0.0627x3 + 0.3119x2 + 0.107x unloading loading Poly. (unloading) Poly. (loading) 0 1 2 displacement (mm) 3 4 y = -0.011x3 + 0.1034x2 + 0.5832x

Force (N)

1.5 1 0.5 0 -0.5

Figure 3.14: loading (red) and unloading (blue) curve for flat indentor with radius 2 mm on rubber sheet of thickness 0.5 mm.

Loading unloading curve for flat indentor with 2 mm radius on 0.2 mm thickness
1.4 1.2 y = -0.0202x4 + 0.1269x3 - 0.2366x2 + 0.4304x 1 0.8 0.6 0.4 y = -0.0144x3 + 0.1238x2 + 0.0564x 0.2 0 -1 -0.2 0 1 2 3 4 -0.4 displacement (mm)

Force (N)

loading unloading Poly. (loading) Poly. (unloading)

Figure 3.15: loading (red) and unloading (blue) curve for flat indentor with radius 2 mm on rubber sheet of thickness 0.2 mm.

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viscoelasticity

Flat indentor radius: 2mm

4 mm

Spherical indentor radius: 2 mm

4 mm

Thickness: 0.2mm

0.271367

0.463914

0.175654

0.264753

0.5 mm 1.0 mm

4.071067 19.2056

5.833182 32.148

3.488667 14.18269

5.741422 24.33383

Table 3.5: Shows viscoelasticity of rubber with different thickness of rubber with flat and spherical indentors of radius 2 mm and 4mm Thicker the rubber viscoelasity will be more for thicker rubber and is more for large diameter indentor. Loading unloading curves for flat indentor radius is shown in appendix A-1, A-2, A-3.

3.7 Effect of chamber size

Chamber size is the radius of rubber where the effect of force affects. It is the radius of cylinder inside where the rubber is fixed. As the radius of cylinder or chamber size increases the force required will also decreases and is explained later in this part.

61

Load Vs displacement for 5 mm chamber size

8 7 6 5 0.2 mm thick flat 0.5 mm thick flat 1.0 mm thick flat 0.2 mm thick spherical 0.5 mm thick spherical 1.0 mm thick spherical

Force (N)

4 3 2 1 0 -1 0 0.5 1 1.5 2 2.5 3 3.5 Displacement (mm)

Figure 3.16: Load displacement curves for 1.0 mm, 0.5 mm and 0.2 mm with flat indentor of radius 2 mm with a chamber radius of 5 mm. The above figure shows the force displacement curve for a chamber size of 5 mm on rubber of thickness of 0.2 mm, 0.5 mm and 1.0 mm. For chamber size 5 mm the force needed is much larger than large chamber size. This is because the extinction is produced in an area of r2 i.e. * 52= = 3.14*25 = 78.5 mm2 For a chamber radius of 10 mm the area under goes extinction is * 102= 314, which is four times more than 5 mm chamber radius. Hence we can conclude that as the chamber size is more the force is also larger. Force displacement curves for a chamber size of 10 mm and 15 mm is shown in appendix A6 and A7.

62

Effect of chamber size

8 7 6 Force (N) 5 4 3 2 1 0 5 7 9 11 13 15 Chamber size (mm) 0.2 mm thickness 0.5 mm thickness 1.0 mm thickness

Figure 3.17: Force vs. Chamber size curves for rubber with thickness 0.2 mm, 0.5 mm and 1.0 mm for an extension of 5 mm. The above figure (figure 3.17) shows the effect of chamber radius and force for three different thickness of rubber. For a chamber size till 10 mm the slope of force chamber radius curve is more. The slope tents to reduce as the chamber size decreases. For a thickness of 0.5 mm and 0.2 the curves are much like a linear line. So it can be considered that the force is inversely proportional to chamber radius.

63

Slope- thickness for different chamber size

1.2 1 0.8

Slope

0.6 0.4 0.2 0 0 0.2 0.4 0.6 Thickness (mm) 0.8 1 1.2

10 mm radius 15 mm radius

Figure 3.18: Slope of force displacement curves of chamber radius 10 mm and 15 mm with various thickness of rubber. From the above figure (figure 3.18) for a very small thickness of rubber of less than 0.01 mm the chamber size of 10 mm and 15 mm does not have much difference than that of thickness from 0.1 mm. After the thickness of about 0.5 mm the 10 mm chamber radius line and 15 mm chamber radius line as almost parallel to each other so the difference of 10 mm could be a multiple of 15 mm radius chamber. The slope for chamber size 10 mm and 15 mm are showing same trend without much variation from 0.5 mm thickness of rubber. From the figures we can conclude that as the chamber size increases the force also increases.

64

Number

Chamber size

Thickness

Force for 3 mm displacement

Slope

0.2

1.8 3.8 7.5 0.8 2.4 3.6 0.6 1.3 3.2

0.5746 1.162 2.4935 0.2518 0.723 1.0726 0.1923 0.4055 1.0465

0.5 1.0 0.2

10

0.5 1.0 0.2

15

0.5 1.0

Table 3.6: Table with different chamber size and different thickness and the maximum force needed for 3mm displacement and slope of force displacement curve for each thickness. :

65

3.8 Youngs Modulus using formula

Deflection, w=

P [ 3 + a2 + c2 log c 16D 1+ a

7 + 3 c2 ]---- -----------(1)
4 (1 + )

(International Journal of Mechanical Science 47 (2005), page 326) Where P= force in Newtons P = c2 q c= radius of indentor q= intensity h= thickness of rubber a = chamber radius and D can be calculated by the formula D = Eh3/ (12 (1-2)) ----------------------------------------------------------------- (2) from which youngs modulus E can be found out. The comparison of experimental and calculated parameters of rubber published in the Journal called International Journal of Mechanical Science 47 (2005) and test conducted by myself is shown in the tables below. As per the journal the Youngs modulus is accurate and is around 1.6 MPa for rubber of thickness 120 m but when the same formula (1) is used in the experiment the youngs modulus found to be much inaccurate. In the journal the thickness of rubber used is 120 m and the radius of indentor is 250 m where as in the experiment the thickness used are of 0.2 mm, 0.4mm and 1.0 mm thick and the indentor radius is 2 mm and 4 mm. The difference between the journals calculated youngs modulus and experimental youngs modulus is because of the difference in value in the variable D. The value of variable D is

66

much higher than the Journals value. The variable D is calculated from the formula (2) and can be seen except the value of h, thickness all the other values is constant. Since the cube root of thickness is much different we can conclude that the above formula can be used for a small thickness.

By Journal

Number

P/w

E (MPa)

1.0 mm

120 m 120 m 120 m

7.40

0.325 X 10-6

1.693

2.5 mm

1.02

0.293 X 10-6

1.526

5.0 mm

0.270

0.313 X 10-6

1.631

Table 3.7: Shows the parameters used to find the Youngs modulus. (International Journal of Mechanical Science 47 (2005), page 327, table 1) [17] By experiment: Indentor radius 2 mm

Number

P/w

E (MPa)

1 2 3

10 mm 0.2 mm 10 mm 0.5 mm 10 mm 1.0 mm

0.251 0.829 1.108

2.05 X 106 3.71 X 106 4.96 X 106

1.26 0.26 0.044

Table 3.8: Experimental parameters used and the youngs modulus for each thickness with flat indentor of 2 mm radius

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By experiment: Indentor radius 4 mm Number 1 2 3 a 10 mm 0.2 mm 10 mm 0.5 mm 10 mm 1.0 mm h P/w 0.504 1.26 2.179 D 2.5 X 106 512 X 106 8.86 X 106 E (MPa) 1.31 0.367 0.079

Table 3.9: Experimental parameters used and the youngs modulus for each thickness with flat indentor of 4 mm radius

3.9 Test on three different gloves

3 different glove with flat indentor

6 5 4 Force (N) 3 2 1 0 0 1 2 3 4 5 displacement (mm) blue gloves (flat) yellow gloves (flat) white gloves (flat)

Figure 3.19: Load displacement curve for three different gloves. The above figure (figure 3.19) shows the force displacement curves for three different gloves of thickness 0.03 mm, 0.12 mm and 0.14 mm named white, blue and yellow respectively according to the colours of the gloves. It can be

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seen that for an elongation of 5 mm the largest force needed is for blue so it can be considered as the tightest gloves. From the loading unloading curve of three gloves (figure A4) it can be seen that the viscoelastic effect is maximum for blue gloves. Yellow gloves are the thickest as have the least viscoelastic and creep effect. Since the force needed for elongation of yellow rubber is between blue and white gloves it cannot be as tight as blue gloves are and white have most creep effect so it can get less fit after using a couple of times. The white gloves have a large amount of creep than the other gloves (figure A5). Since the creep effect is also least for yellow gloves it can be used again without any problem after wearing and removing for a number of times. The slopes of three gloves are 1.068, 0.542 and 0.286 respectively for blue, yellow and white gloves.

3.10 SolidWorks stimulation

Experiment and solidworks

2.5 2

SolidWorks E=1 SolidWorks E=2 SolidWorks E=3

Force (N)

1.5 1 0.5 0 0 0.5 1 displacement (mm) 1.5 2

SolidWorks E=4 SolidWorks E=5 SolidWorks E=6 experimental

Figure 3.20: The figure shows the SolidWork force displacement curves at different youngs modulus with the actual force displacement curve from experiment using 1 mm thick rubber and 2 mm radius indentor. Since the formula (1) used was unable to find the youngs modulus another approach is used to find the youngs modulus of rubber used in experiment. In this approach the rubber test is stimulated under the same properties except

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the youngs modulus. From the SolidWork stimulation different force displacement curves are plotted for different youngs modulus from 1 MPa and are compared with the force displacement curves obtained from the experiment as shown in figure 3.20. The above figure (figure 3.20) shows the experimental force displacement curve obtained from 1 mm thick rubber with an indentor radius of 2 mm on a chamber size of 10 mm. All the other curves are the SolidWorks results on the stimulation of the rubber of 1 mm under the same conditions as in the experiment with the youngs modulus 1 MPa to 6 MPa. It can be clear that the force displacement curve of rubber matches with the force displacement curve obtained from SolidWork stimulation of Youngs Modulus 6 MPa. Thus it can be concluded that the Youngs modulus of rubber of thickness 1 mm is 6 MPa. 3.11 Effect of mesh size As the element size decreases the number of elements increases and hence the accuracy of the stimulation will also increases. So the mesh size 0.5 mm can produce more accurate result than a model with a mesh size 1.0 mm. The table below shows the effect of different mesh size on a rubber of thickness 1 mm with a flat indentor of 2 mm radius. For a mesh size of 0.5 mm and a force 3N the displacement produced is 2.199 mm and for mesh size of 0.9 mm, for the same force 3N produces a displacement of 2.16 mm. That means a difference of 0.04 mm displacement is produced between a mesh size of 0.5 mm and 0.9 mm.

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Number

element size (mesh size)

Force (N)

Displacement (mm)

0.5 1 1.5

0.07643 1.211 1.526 1.778 1.994 2.199 0.07578 1.202 1.1515 1.766 1.98 2.182 0.075 1.194 1.508 1.759 1.975 2.178 0.7432 1.187 1.502 1.757 1.981 2.208 0.7367 1.181 1.495 1.746 1.963 2.16

0.5 mm

2 2.5 3 0.5 1 1.5

0.6 mm

2 2.5 3 0.5 1 1.5

0.7 mm

2 2.5 3 0.5 1 1.5

0.8 mm

2 2.5 3 0.5 1 1.5

0.9 mm

2 2.5 3

Table 3.10: Effect of mesh size at different force shows the deformation on 1 mm thick rubber

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3.12 Summary of project

Same tests under same conditions are carried out on rubber with thickness of 0.2 mm, 0.5 mm and 1.0 mm and the results found to be same so the tests are repeatable. Compared the flat and spherical indentor and from the force displacement graphs obtained shows the same characters except flat indentor needs a slight more force than spherical indentor to get the same displacement. For different loading rates both spherical and flat indentors have the same behaviour. For small radius indentors loading rate will affect more than indentors with a larger radius. Still loading rate of up to 0.03 mm/sec with 2 mm radius indentor shows not much influence on force displacements graphs. (figure 3.9-3.11) Visco elastic effect of natural rubber increases as the thickness of rubber increases. From table 3.5 as the thickness gets doubled from 0.5 mm to 1.0 mm viscoelasticity is getting square. As the chamber size increases the force needed for same extinction will decreases. The slope for chamber size 10 mm and 15 mm are showing same trend without much variation from 0.5 mm thickness of rubber. (figure 3.18) From figure 3.17 for rubber of thickness 0.5 mm and 0.2 mm the force varies almost linearly with force. So the force can be considered as inversely proportional to chamber radius. Compared the formula and parameters used by the Journal International Journal of Mechanical Science 47 (2005) and test conducted by myself and found that the same formulae used in that journal is valid for rubber of very small thickness of the order of less than 120 m and for small chamber size of less than 1 mm with small extension of 10 nm or small force of 0.1 N. [17] By comparing the test results of test carried out on three different gloves it can be found that Youngs modulus will be maximum for blue gloves then for yellow and least for white gloves. For white gloves the effect of creep and visco elastic is high than other two gloves. The blue glove needed much more force for

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same displacement than other two gloves so it can be considered to be too tight to wear. For different Youngs modulus values from 1MPa to 6MPa different force displacement graphs are plotted with SolidWorks. This force displacement data form SolidWorks are compared with the experimental force displacement data for 1 mm thick rubber and the Youngs modulus found to be 6MPa. Found the effect of mesh size, as the element size decreases the accuracy will also increases since for the mesh size of 0.5 mm and 0.9 mm the maximum difference in deflection for 3N is 0.039 N so we can be neglect the effect of mesh size for a difference of 0.4 mm. (table 3.10)

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CHAPTER 4: CONCLUSION
Rubber with different thickness of 0.2 mm, 0.5 mm and 1.0mm are test with flat and spherical indentors with two different radiuses of 2 mm and 4 mm. Both indentors of flat and spherical behave in a similar manner except for flat indentors the force is a little larger than flat indentor. As the size of indentor increases the force needed for extension will also increases. Thus for both spherical and flat indentor of 4mm radius needs more force than indentor of 2mm radius. The effect of loading rate can be neglected for indentor of 2 mm radius but as the indentor radius becomes larger the effect of loading rate becomes more predominant hence cannot be neglected for 4mm radius indentor. The viso elastic effects are less for less thickness of rubber than large thickness. Hence the effect is higher for 1 mm thick rubber than that of 0.5 mm and 0.2 mm. The force decreases as the chamber size chamber size increases. As chamber size increases the force can be found to be varying almost linearly for 0.5 mm and 0.2 mm thick rubber so force can be considered to be inversely proportional to chamber size. The formula used by the Journal International Journal of Mechanical Science 47 (2005) to find youngs modulus is valid only for very small parameters of thickness, chamber radius, displacement and force. By comparing the experimental works with the testing results of three different gloves found that white glove can be used only for a few times, blue glove is the hardest with the largest Youngs modulus and the white gloves is better than the other two gloves. By comparing solid works force displacement data with experimental force displacement data the youngs modulus of 1mm thick natural rubber found to be 6MPa. The mesh size of 0.5mm to 0.9mm does not have much difference. The largest difference in force for 3 mm displacement was for rubber of 1mm thickness and was only 0.039N so the effect of element size of a difference of up to 0.4 mm can be neglected. So the comparison of mash size of 0.5 mm and 0.9 mm wont affect much while comparing with the solid works and experimental works force displacement data.

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Reference: 1) Applications of Synthetic Resin Lattices: Lattices in diverse applications by Henry Warson, C. A. Finch 2) Alan N. Gent, Engineering with rubber: how to design rubber components, second edition, 2001, Hanser Gardner Publications Inc 3) Anthony C. Fischer-Cripps, Nanoindentation, Second edition, Springer Verlag New York, 2004 4) Andrew Ciesielski, An introduction to rubber technology, Rapra Technology Limited, First Edition, 2000 5) Basic rubber testing: selecting methods for rubber test program (Page 61-63) By John S. Dick, ASTM International Publisher, 2003 6) Bing Feng Ju, Yang Ju, Musumi Saka, Kuo Kang Liu, Kai Tak Wan, A systematic method for characterizing the elastic properties and adhesion of thin polymer membrane, 2005. 7) Challenges and Progress in High-Throughput Screening of Polymer Mechanical Properties by Indentation by Johannes M. Kranenburg, Catherine A. Tweedie, Krystyn J. van Vliet, and Ulrich S. Schuber 8) E. I. Rivin, Properties and prospective applications of ultra thin layered rubber-metal laminates for limited travel bearings. 9) Jim R. White and S. K De, Rubber technologist's handbook, Rupra Technology Limited, 2001, 1st edition. 10) L. R. G. Treloar, The physics of rubber elasticity, Oxford University Press, 2005. 11) Mikell P. Groover, Fundamentals of Modern Manufacturing: Materials, Processes, and Systems, John Wiley & Sons Publications, 4th edition 2010

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12) Mark R. VanLandingham, Review of Instrumented Indentation, Journal of Research of the National Institute of Standards and Technology, Volume 108, Number 4, July- August 2003 13) http://www.gordonengland.co.uk/hardness/rockwell.htm 14) http://slp.nist.gov/pic/NISTMV.pdf 15) www.advmat.de 16) http://silver.neep.wisc.edu/~lakes/VEnotes.html (Viscoelasticity) 17)http://www.adhesivestoolkit.com/DocuData/NPLDocuments/P%20A%20J/Ot hOt%20documents/Adh99%20rubber%20paper.pdf 18) Peter C. Powell, Engineering with polymers, Chapman and Hall Ltd, 1983 19) Rubber compounding: chemistry and applications by Brendan Rodgers 20) Roger P. Brown, Physical Testing of Rubber third edition, Champman and Hall, 1996 21) R. P Brown, Physical Testing of Rubber, Report 58 - Volume 5, Rupa Technology limited 2001. 22) The physics of rubber elasticity by L. R. G. Treloar 2005Oxford University Press.

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Appendix

Loading unloading curve of flat indentor radius 4mm on 1.0 mm thickness

7 6 5 y = 0.0493x3 + 0.2368x2 + 1.1243x 4 y = -0.0446x3 + 0.2544x2 + 1.8521x

Force(N)

loading unloading Poly. (loading) Poly. (unloading)

3 2 1 0

-1 -1

Displacement(mm)

Figure A1: loading (red) and unloading (blue) curve for flat indentor with radius 4 mm on rubber sheet of thickness 1 mm.

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Loading unloading curve of flat indentor radius 4mm on 0.5 mm thickness

3.5 3 2.5 2 1.5 1 0.5 0 -1 -0.5 0 1 2 displacement (mm) 3 4 y= -0.0347x4 + 0.2473x3 0.3123x2 + 0.6727x unloading loading Poly. (unloading) Poly. (loading) y = -0.0101x3 + 0.1572x2 + 0.6455x

Figure A2: loading (red) and unloading (blue) curve for flat indentor with radius 4 mm on rubber sheet of thickness 0.5 mm.

Force (N)

Loading unloading curve of flat indentor radius 4mm on 0.2 mm thickness

1.6 1.4 1.2 1 y = -0.0048x4 + 0.0591x3 - 0.079x2 + 0.3461x loading unloading Poly. (loading) Poly. (unloading) y = -0.0392x4 + 0.2334x3 - 0.4123x2 + 0.6776x

Force (N)

0.8 0.6 0.4 0.2 0 -0.2 0 0.5 1 1.5 2 2.5 displacement (mm) 3 3.5

Figure A3: loading (red) and unloading (blue) curve f or flat indentor with radius 4 mm on rubber sheet of thickness 0.2 mm.

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Force displacement curve for three gloves

6 5 4

Force (N)

3 2 1 0

Blue white Yellow

-1

-1

displacement (mm)

Figure A4: Force displacement curve showing loading and unloading curve of three different gloves.

Force displacement curve for three gloves

1.8 1.6 1.4 1.2 1 0.8 0.6 0.4 0.2 0 -1 -0.2 0

Force (N)

white

2 3 displacement (mm)

Figure A5: Force displacement curve for white rubber gloves.

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Force displacement curve chamber size of 10 mm

4.5 4 3.5 3 Flat R2 at 0.2mm Flat R2 at 0.5mm Flat R2 at 1.0mm sphericalR2 at 0.2mm sphericalR2 at 0.5mm spherical R2 at 1.0mm 0 1 2 displacement (mm) 3 4

Force (N)

2.5 2 1.5 1 0.5 0

Figure A6: Force displacement curve for 1 mm thick rubber on spherical and flat indentor with 2mm radius on a chamber size of 10 mm.

Force displacement curve for chamber size of 15 mm

3.5 3 2.5 FlatR2 for 0.2mm thick FlatR2 for 0.5mm thick FlatR2 for 1mm thick sphericalR2 for 0.2mm thick 0 1 2 Displacement (mm) 3 4 sphericalR2 for 0.5mm thick

Force (N)

2 1.5 1 0.5 0 -0.5

Figure A7: Force displacement curves for chamber size 15 mm with different thickness and with flat and spherical indentors.

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Figure A8: Solid work stimulation output for 1 mm thick rubber with mesh size 0.5mm

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