TITLE: auxetic polymer formation TASK: production of auxetic polyester fiber including the characterization by videoextensometry CHEMICALS: Polyester

(tri methylene terphtahalate) in form of granules APPARATUS: y y y y y y y y Differential scanning calorimeter Partial vacuum oven Scanning electron microscope Cabline extruder Fudicial markers Cryogenic grinding Video extensometer icro tensile testing equipment

PROCEDURE: y Firstly check the thermal characterictics of the polyester granules using DSC, (a small amount of polyester sample (5.5 mg) is heated under flowing nitrogen at 10 degree per mint) y To obtain powdered particles from the supplied polyester granules before extrusion by in-house cryogenic grinding (using liquid nitrogen). y Dry the powder and granules before extrusion to prevent hydrolysis under partial vacuum oven at 108 degree for 2 days befor extrusion. y Then characterize the polyester powder derived from grinding by scanning electron microscope(at approximately 200 magnification)

y Study the micrograph of polyester powder in depth to analyze the size distributions and to understand the surface roughness and shape (by UTHSCSA image tool v3), y Using this micrograph calculate the Aspect Ratio. EXTRUSION PROCESS: y First apply the extrusion experiment on the granules sample to observe the behavior of polymer during extrusion. y Investigate processing temperature based on thermal analysis studies. y Extrusion carried out at high temperature (230 degree and gradually decrease to 210) y The polyester powder was fed through a hopper ionto the barrel. y Then transfer through the barrel zones to die zones. y Thereby undergo sintering due to maintained temp along the zones of the extruder. y Fiber extrude from the die head and called before winding SPECIFICATIONS OF EXTRUDER: y 25.4 mm screw diameter y Length/diameter 24:1 y Five temperature zones each having individual thermostatic controls y Die slot with 40-filament die having each hole size of 550 um CONDITIONS DURING EXTRUSION PROCESS: y Temperature investigation carried out at intervals of 5 degree,(in the range of 230 to 210) y Sscrew speed-------0.0525 rad/s y Take up speed-------0.075 m/s

y The minimum take up speed maintained in extrusion has direct impact on screw speed y The viscosity of the extrude fibers should be low to wind them with a take up speed of 0.03 m/sec and maintaining the screw speed of 1.05 rad/sec. y The draw ratio should be minimum. GRAPHS: y y y y TemperatureHeat flow graph Elongationforce graph Timewidth graph True axial strantrue lateral graph

CALCULATION: y y y y y y y y Calculate aspect ratio Aspect ratio = major axis/minor axis Calculate load extension data from microtensile apparatus process. Measure length and width from videoextensomete (marked length was divided into ten regions by the videoextensometer) Individual width of each part was recorded. The axial and lateral strains were calculated from the length-width data obtained from the videoextensometer Axial strain = ln(l/lo) Lateral strain = ln(W/Wo)

Where Lo, Wo are original length and width and L, W are deformed length and width

TESTS: y Loadelongation test to test the auxeticity of sample by deforming them to 1% strain. y Extruded fiber characterization carried out by using videoextensometer and microtensile testing equipment y One sample attached to microtensile unit process, the load extension data from from the micro tensile attached with 77 N load cell. y 2nd sample attached to the videoextensometer records the changes in length and width of the fiber during the test. y Polyester fibers cut to lengths approximately 10mm marked with two small markers at a distance of approximately 1mm apart along the strength of the fiber y Sample were mounted between the two clamps of the microtensile tester. y Each of test included mounting the sample between the jaws of the microtensile stage y Load is applied and removed cyclically (up to four cycles). SPECIAL PROPERTY TESTS: y y y y Energy absorption test Indentation resistance test Plain strain fracture toughness test Shear stiffness test

USE OF VIDEO EXTENSOMETER: y Videoextensometer operates directly as a strainmeter by tracking the displacement of the edge of the sample as defined by a contrast change in the video image at the edge of length or fiber width caused by strain y The marked length was divided into 10 regions by the videoextensometer and individual width of each was recorde. y Camera of the videoextensometer should mounted vertically above the microtensile stage to capture the image of the fiber. STRAIN RATE: 0.1mm/mint should applied until a maximum strain of 1 % was reached. PRECAUTIONS: y Viscosity of the powdered bulk should be too high to allow free flow through the die zone. y During load elongation test, not exceed the elastic limit of the fiber. y Size of powder particles should not small enough to be proceed in the extruder setup..