ABSTRACT. Being the raw materials, fibers have the biggest importance in textiles industry. With the

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1 ABSTRACT HATIBOGLU, BILGE. Mechanical Properties of Individual Polymeric Micro and Nano Fibers using Atomic force Microscopy (AFM). (Under the direction of Dr. Behnam Pourdeyhimi and Dr. Juan P. Hinestroza.) Being the raw materials, fibers have the biggest importance in textiles industry. With the invention of the first man-made fiber, nylon, in 1930s, fiber industry gained a new aspect. During the recent years, fibers gained another aspect with the term nanotechnology. Now, today s science is focused on the nano materials. Analyzing and finding new applications for them are some of the concerns. Textile industry is affected from the fiber part of the nanomaterials. The introduction of the nanofibers added a lot of interesting applications to textiles. Drug delivery, tissue engineering, reinforcement for composite materials, filtration are some of the interesting applications of nanofibers. Having a lot of exciting applications, nanofibers require to be examined well. However, since they are fairly small materials, it is not very easy to analyze them. In this thesis, we aimed to develop a method to analyze mechanical properties of individual micro and nanofibers using a technique called Atomic Force Microscopy (AFM). After finding a useful approach to prepare individual islands-in-the-sea form fibers for the further analysis, we also set up AFM and developed an experimental approach to examine individual PET and Nylon-6 micro and nanofibers mechanical properties.

2 MECHANICAL PROPERTIES OF INDIVIDUAL POLYMERIC MICRO AND NANO FIBERS USING ATOMIC FORCE MICROSCOPY (AFM) by Bilge Hatiboglu A thesis submitted to the Graduate Faculty of North Carolina State University in partial fulfillment of the requirements for the Degree of Master of Science Textile Engineering Raleigh, North Carolina 2006 Approved By: Dr. Behnam Pourdeyhimi Chair of Advisory Committee Dr. Juan P. Hinestroza Co-chair of Advisory Committee Dr. Orlando Rojas Member of Advisory Committee Dr. Phillip Russell Member of Advisory Committee

3 BIOGRAPHY Bilge Hatiboglu was born on July 20th, 1981 in Merzifon, Turkey. On completing her elementary and high school study in Merzifon, Bilge entered college at Istanbul Technical University, Istanbul, Turkey, in the year 1999 to proceed towards her Bachelor s degree in textile engineering. She graduated with distinction in 2004 and, upon graduation she entered the Master of Science program in Textile Engineering, at North Carolina State University in While she was working on her masters program, she worked as a research assistant under Dr. Behnam Pourdeyhimi and Dr. Juan P. Hinestroza on a project funded by Nonwovens Corporative Research Center. ii

4 ACKNOWLEDGEMENTS I would like to express my gratitude to my advisors Dr. Behnam Pourdeyhimi and Dr. Juan P. Hinestroza for giving me the opportunity to work with them and for their continuous patience and guidance. This work would not have been possible without their knowledge and support. I also appreciate the support given by the other members of my advisory committee, Dr. Phillip Russell and Dr. Orlando Rojas. I also appreciate the financial support provided by Nonwovens Cooperative Research Center. I would like to thank Chuck Mooney, Mike Salmon, David Nackashi, Roberto Garcia and Dale Batchelor for their help and support with the experimental work. I extented my great appreciation to Jeffrey Krauss. My special thanks go to Umut Kivanc Sahin and Erkmen Ercan for their support and encouragement throughout this work. My last but not least gratitude goes to my parents and my sister for being with me, supporting me and trusting me at every moment of my life Without all of you, this degree would not be possible. Thank you all once more iii

5 TABLE OF CONTENTS LIST OF TABLES.....vii LIST OF FIGURES viii 1. INTRODUCTION LITERATURE REVIEW Fibers Natural Fibers Man-Made Fibers General Fiber Properties Geometric Characteristics Physical Properties Chemical Properties Mechanical Properties Properties of Polyamide-6 (Nylon-6) and Polyester (PET) Nylon-6 Fibers PET Fibers Microfibers Nanofibers Fabrication of Nanofibers Drawing Template Synthesis Phase Separation Bicomponent Extrusion iv

6 Self-Assembly Electrospinning Other Techniques Applications of Nanofibers Filters Biomedical Applications Protective Clothing Reinforcement for Composite Materials Sensors Analytical Techniques Scanning Electron Microscopy (SEM) Transmission Electron Microscopy (TEM) Atomic Force Microscopy (AFM) EXPERIMENTAL APPROACH Materials Instruments Focused Ion Beam (FIB) Scanning Electron Microscopy (SEM) Dynamic Mechanic Analyzer (DMA) Atomic Force Microscopy (AFM) Experimental Procedures First Approach Second Approach 61 v

7 Third Approach Final Approach RESULTS AND DISCUSSION Cross-sectioning and imaging islands-in-the-sea form fibers Method Validation AFM Imaging and Indentations Determination of the tip radius Determination of the cantilevers size Determination of the cantilevers spring constant Data processing and obtaining Force vs. Displacement curves Calculation of elastic modulus values Results for PET micro and nanofibers Results for Nylon-6 micro and nanofibers Results for Nylon-6 hollow micro and nanofibers SUMMARY AND CONCLUSIONS REFERENCES APPENDIX.115 vi

8 LIST OF TABLES Page Table 2.1 Effect of drawing on Elastic modulus of Nylon-6 fibers [3]...8 Table 2.2 Typical Properties of nylon fibers [3] 10 Table 2.3 Typical properties of Polyester fibers [3]..11 Table 4.1 Elastic modulus values [GPa] of the PET film, obtained under different testing conditions..71 Table 4.2 An example of the variation on the same cantilevers spring constants because of the size, RF and QF..81 vii

9 LIST OF FIGURES Page Figure 2.1 Cross-sections of bicomponent fibers..16 Figure 2.2 Classical bilateral bicomponent spinning (A, B: Polymers) [12].17 Figure 2.3 Pipe-in-pipe mixers [12]...17 Figure 2.4 Schematic figure of Elecrtospinnig process [13]..19 Figure 2.5 Fractional efficiency (Filtration Efficiency vs. particle size) for a standard cellulose media and nanofiber filter media [22]..22 Figure 2.6 SEM images of nickel titanate fibers: a)as-prepared composite fibers, b) fibers calcinated at 1273 K [28].27 Figure 2.7 SEM images of the V 2 O 5 fibers [29] 27 Figure 2.8 SEM images of elastomeric nanofiber membranes under two different levels of biaxial strain a) 100%, b) 0 % [24]...28 Figure 2.9 SEM photograph of PVA/lithium chloride/manganese acetate composite fiber samples [30].29 Figure 2.10 SEM images of a) polyaniline nanofibers b) polyaniline nanofibers and polyaniline/ceo2 composite microspheres [32].30 Figure 2.11 TEM image of polyaniline nanofibers [32] 31 Figure 2.12 TEM images of a) Twisted nantubes; b) and c) Aligned, nanotubes in PEO nanofibers [35]..32 Figure 2.13 TEM image of an individual Collagen-r-PCL composite nanofiber a) collagen as the shell material, and PCL the support b) is the TEM image of a pure PCL nanofiber [34]..33 Figure 2.14 Transmission electron micrographs of a) PA6 fiber, a segment almost constant in diameter b) PLA nanofiber fibers with modulations [37]...34 Figure 2.15 AFM images of PA6 nanofibres a) regular fiber b) plasma treated fiber (for 60 seconds) [40].35 viii

10 Figure 2.16 a) NCAFM image (25 ím _ 25 ím) of dendrimer 1 nanofibers prepared by drop-casting a 2.0 _ 10-6 M dendrimer 1 solution in THF on a silicon surface in a saturated environment of THF, b) NCAFM image (25 ím _ 25 ím) of dendrimer 1 nanofibers repared by drop-casting a 2.0 _ 10-6 M dendrimer 1 solution in THF in a saturated environment of THF:H2O ) 90:10 (v/v) on a silicon surface, c) NCAFM image (50 ím _ 50 ím) of dendrimer 1 nanofibers prepared by drop-casting a 2.0 _ 10-6 M dendrimer 1 solution in THF in a saturated environment of THF:H2O ) 80:20 (v/v) on a silicon surface [31] 37 Figure 2.17 a) Schematic diagram of three-point bending test and b) actual AFM scanning data on fiber (i) and pore (ii) [41].38 Figure 2.18 Young s modulus (E) vs. diameter of TiO 2 PVP and TiO 2 nanofibers [41]..39 Figure 2.19 (a and b) AFM images of indents on a silver nanowire c) height profile of an indent on the wire, and d) a representative nanoindentation load-displacement curve for a silver nanowire [42] 40 Figure 2.20 (a) Indentation load-displacement curves made on a solid Cu 2 O nanocube and (b) a hollow Cu 2 O nanocube [43].41 Figure 2.21 Schematic of AFM tip depressing suspended nanofiber [44] 42 Figure 2.22 a) Average Young s modulus versus diameter for several PEO nanofibres produced by electrospinning b)average Young s modulus versus diameter for several polysiloxane and glass nanofibres produced by electrospinning [44].. 42 Figure 2.23 Nanofibers suspended over etched grooves of silicon wafer: a)electron micrograph of PLLA nanofibers deposited onto the silicon wafer; b) AFM contact mode image of a single nanofiber (300 nm diameter) suspended over an etched groove; c) schematic diagram of a nanofiber withmid-span deflected by an AFM tip [45].43 Figure 2.24 Variation of elastic modulus with fiber diameter for nanoindentation of PLLA nanofiber [46].44 Figure 2.25 (a) AFM image of a SWNT rope adhered to the polished alumina ultrafiltration membrane, with a portion bridging a pore of the membrane. (b) Schematic of the measurement [49] 45 ix

11 Figure 2.26 Measured reduced modulus, E r, for ten different SWNT ropes with diameters between 3 and 20 nm (circles) [49]...46 Figure 3.1 Custom-made TEM grids.48 Figure 3.2 SEM image of the calibration grating used for tip radius determination...49 Figure 3.3 Schematic figure of FIB [60] 49 Figure 3.4 Schematic Diagram of an SEM [49] 52 Figure 3.5 Schematic of how DMA works [49] 53 Figure 3.6 Essential elements of AFM [59]..56 Figure 3.7 a) Force calibration Z waveform, b) a typical force-distance curve for a tip in contact with a sample [49]. 58 Figure 3.8 A microscope image of an epoxy coated PET/PE islands in the se form fiber.60 Figure 3.9 AFM images of PET nanofibers coated with adhesive 62 Figure 3.10 SEM images of the PET nanofibers on perforated aluminum plates.63 Figure Schematic of the sample preparation method; a) threading the I/S fiber through the windows of the grids, b) Submerging and keeping the grid in the appropriate solution, c) Obtaining the PET and Nylon6 nanofibers and Nylon6 hollow fibers on the grid 65 Figure 4.1 SEM images of a) PET/PE islands-in-the-sea fibers and b) Nylon6/Evoh islands-in-the-sea hollow fiber 67 Figure 4.2 FIB images of a) PET/PE and b) Nylon6/Evoh islands-in-the-sea fibers 68 Figure 4.3 AFM images of a) PET/PE b) Nylon-6/Evoh islands-in-the-sea fibers...70 Figure 4.4 AFM images of quartz sample a) before and b) after indentation 72 Figure 4.5 A typical Piezo Movement vs. Tip Deflection Curve for Quartz. 73 Figure 4.6 Schematic of AFM tip imaging the nanofiber..74 Figure 4.7 3D images of a) PET and b) Nylon6 nanofibers..75 x

12 Figure 4.8 Examples of Tip Displacement vs. Piezo Movement curves of a a)pet and a b)nylon6 nanofiber...77 Figure 4.9 Size relations between some of the AFM tips and the fibers...77 Figure 4.10 a) An AFM image of the tip obtained imaging calibration gratings and b) Cross-section of the AFM tip.78 Figure 4.11 SEM images of some of the cantilevers.79 Figure 4.12 Some examples of F vs. d curves retracting parts of PET micro and nanofibers 87 Figure 4.13 Some examples of F vs. d curves retracting parts of Nylon6 micro and nanofibers..93 Figure 4.14 Some examples of F vs. d curves retracting parts of Nylon6 hollow micro and nanofibers..98 Figure 4.15 Cross-section of two solids a) before and b) after deformation Figure 4.16 Elastic modulus vs. Fiber diameter relation for PET micro and Nanofibers Figure 4.17 Elastic modulus vs. Fiber diameter relation for Nylon-6 micro and nanotubes 105 Figure 4.18 Elastic modulus vs. Fiber diameter relation for Nylon-6 hollow micro and nanofibers Figure 7.1 3D image of PET nanofiber 116 Figure 7.2 3D image of Nylon-6 nanofiber.116 Figure 7.3 Raw indentation Curve of PET microfiber ( φ = 2.5 ± 0. 18μm ) Figure 7.4 Raw indentation Curve of PET microfiber ( φ = 1.8 ± 0. 11μm ).117 Figure 7.5 Raw indentation Curve of PET microfiber ( φ = 700 ± 50nm ) Figure 7.6 Raw indentation Curve of PET microfiber ( φ = 400 ± 30nm ) Figure 7.7 Raw indentation Curve of PET microfiber ( φ = 300 ± 20nm ) Figure 7.8 Raw indentation Curve of PET microfiber ( φ = 100 ± 7nm ).119 xi

13 Figure 7.9 Raw indentation curve of Nylon 6 Nanofiber ( φ = 1.3 ± 0. 09μm ) Figure 7.10 Raw indentation curve of Nylon 6 Nanofiber ( φ = 1.2 ± 0. 08μm )..120 Figure 7.11 Raw indentation curve of Nylon 6 Nanofiber ( φ = 1± 0. 07μm ).121 Figure 7.12 Raw indentation curve of Nylon 6 Nanofiber ( φ = 900 ± 60nm ) 121 Figure 7.13 Raw indentation curve of Nylon 6 Nanofiber ( φ = 800 ± 55nm ).122 Figure 7.14 Raw indentation curve of Nylon 6 Nanofiber ( φ = 700 ± 50nm ) 122 Figure 7.15 Raw indentation curve of Nylon 6 Nanofiber ( φ = 600 ± 40nm ) 123 Figure 7.16 Raw indentation curve of Nylon 6 Nanofiber ( φ = 500 ± 35nm ).123 Figure 7.17 Raw indentation curve of Nylon 6 Nanofiber ( φ = 300 ± 20nm ) Figure 7.18 Raw indentation curve of Nylon 6 Nanofiber ( φ = 200 ±15nm ).124 Figure 7.19 Raw indentation curve of Nylon 6 hollow Microfiber ( φ = 1.3 ± 0. 09μm ).125 Figure 7.20 Raw indentation curve of Nylon 6 hollow Microfiber ( φ = 1.1± 0. 07μm ).125 Figure 7.21 Raw indentation curve of Nylon 6 hollow Microfiber ( φ = 1± 0. 07μm ) 126 Figure 7.22 Raw indentation curve of Nylon 6 hollow Microfiber ( φ = 500 ± 35nm ) Figure 7.23 Raw indentation curve of Nylon 6 hollow Microfiber ( φ = 400 ± 30nm )..127 Figure 7.24 Raw indentation curve of Nylon 6 hollow Microfiber ( φ = 300 ± 20nm )..127 Figure 7.25 Raw indentation curve of Nylon 6 hollow Microfiber ( φ = 100 ± 7nm ). 128 xii

14 1. INTRODUCTION The objective of this work was to develop a method capable of analyzing the mechanical properties of individual micro and nanofibers using Atomic Force Microscopy. An optimized protocol for sample preparation was developed and the properties of polyester and nylon-6 islands-in-the-sea fibers were probed by applying Hertzian Contact Theory to the experimental data obtained via AFM. The introduction of polymeric nanofibers has spurred a great number of new and interesting applications to the field of textiles. Some of these applications include drug delivery, tissue engineering, reinforcement for composite materials, and filtration. During the last ten years, due to advances in instrumentation and the nanotechnology revolution, it has been established that some material properties may be size dependent. However, most of current manufacturing and testing techniques for micro/nano scale devices are still based on bulk material properties that do not consider size dependent phenomenon. Some improved microscopy techniques, including Atomic Force Microscopy (AFM), Transmission Electron Microscopy (TEM) and Scanning Electron Microscopy (SEM) are currently used to analyze micro and nano-sized materials. Atomic Force Microscopy (AFM) has been chosen for this study because this technique provides a topographic contrast as well as direct height measurements. AFM images are obtained without expensive sample preparation and yield more information than those 1

15 obtained by cross sectioning samples and analyzing the sections via TEM. AFM can be used not only as an imaging technique, but it shows an increasing potential for direct measurements of mechanical properties of micro/nano-sized materials. 2

16 2. LITERATURE REVIEW 2.1. Fibers In early history only natural fibers such as cotton, linen and jute from plants as well as wool and mohair from the fleece of sheep and goats, and silk from the cocoon of the silkworm, were available. During the twentieth century some derivative fibers were created from existing natural fibers and more importantly new synthetic fibers were developed using by using by-products of the coal and petroleum industries. Today, it is possible to synthesize polymeric fibers with almost any desired property by manipulating their chemistry[1]. Fibers can be seen everywhere. Even the fundamental blocks of living systems are formed by fibrous materials in nanometer scale such as DNA molecules, cytoskeleton filaments, rod cells of the eyes etc. [2]. Fibers are also raw material for all kinds of textiles. Having a combination of high specific surface area, flexibility and superior directional strength, fibers are preferred materials for applications ranging from clothing to reinforcements in aerospace applications [3] Natural Fibers Natural fibers are mostly derived directly from animals, vegetables or minerals. With the exception of silk, which is extruded by silkworms as a continuous filament, natural fibers are of finite length and are used directly in textile manufacturing after preliminary cleaning. These fibers are commonly referred to as staple fibers. The utility of natural 3

17 fibers for textile purposes is also affected by their fineness, presence of impurities, color, absorption of water and dyestuffs, thermal and environmental stability, resistance to chemical degradation [3] Man-Made Fibers As it is apparent from their name, all fibers manufactured by man are called man-made fibers; distinct from those which occur naturally. Man-made fibers are grouped into two major categories: natural organic polymer fibers and synthetic organic polymer fibers [4]. Natural organic polymer fibers can be either regenerated or derivative fibers. Regenerated fibers are formed by dissolving and extruding a natural polymer or a derivative thereof retaining the chemical nature of the originating natural polymer Since their commercialization in 1940, synthetic organic polymers have revolutionized the textile industry. There are many synthetic polymers that have fiber forming ability. However the most widely used synthetic polymers are based on polyamides, polyesters, polyolefins... etc. [3] 2.2. General Fiber Properties After years of research and experience, the relationship between fiber properties and enduse performance has been roughly established for several families of synthetic fibers facilitating the selection of the best fiber for a particular application. Fiber properties can be classified as geometrical, physical, chemical and mechanical [1]. 4

18 Geometric characteristics These properties include fiber properties such as length, cross-sectional area, shape and crimp. Fiber length uniformity, cross-sectional area of the fiber (fiber diameter) and fiber fineness affects processing efficiency and the quality of the final product. As the fibers become finer, the number of fibers in the cross section of a yarn will increase creating more regularity. Crimp describes the waviness or longitudinal shape of the fiber. Conventional textile manufacturing equipments require some degree of fiber crimp. All natural fibers are crimped; however synthetic fibers must be crimped artificially to be processed into spun yarns. It is very difficult to control the length; fineness and crimp of natural fibers and the economic value of these fibers are mostly dependent on the uniformity of these properties. In terms of synthetic fibers, the length can be set to almost any desired value and their uniformity can be easily controlled. [3] Physical properties Subjected to elevated temperatures, textile fibers must have high melting or degradation points while other fibers properties must be relatively constant over a useful temperature range. Usually textile fibers are opaque and they have significantly different refractive indexes than those of their surrounding environment. 5

19 In terms of electric properties, textile fibers are classified as insulators which cause static electrification. This problem is common in fibers with low water absorption preventing them from forming an electrically conducting system able to dissipate the static charges. Furthermore, inter-fiber friction and geometric roughness also affect the process ability and final product performance of synthetic fibers [3] Chemical Properties Textile fibers are required to be resistant to the effects of acids, alkalies, reducing agents, oxidizing agents, besides electromagnetic and particulate irradiation. Due to their chemical structure, some textile fibers are generally capable of absorbing large amounts of moisture from atmosphere. The amount of moisture uptake has a great effect on their electrical and mechanical properties [3] Mechanical Properties The mechanical properties of fibers can be described as the responses of a fiber to deforming loads under conditions that induce tension, compression, torsion or bending. The mechanical properties of fibers are usually evaluated under standard conditions of temperature and humidity (65% rh, 21ºC). Mechanical properties can be described in terms of strength, extensibility, stiffness, elasticity and toughness. Fiber strength is the stress required to produce rupture in units of mass per unit cross section. In common fiber terminology, strength is expressed as the tenacity at break or ultimate tenacity in units of N/tex or gram-force per denier. Extensibility describes the 6

20 deformation of the fiber that is produced by a given stress. Quantitatively it is defined by the ultimate strain. The units for extensibility or strain are length-per-unit-length expressed as percentage. Stiffness describes the resistance of the fiber to deformation. The elastic stiffness is equivalent to the elastic modulus or Young s modulus of elasticity and has the units of stress-per unit-strain [3] Properties of Polyamide-6 (Nylon-6) and Polyester (PET) Being the main materials used this research work, Poly(ethyleneterephthalate) (PET, Polyester) and Polyamide-6 (Nylon-6) fibers are explained in detail Nylon 6 Fibers Nylon was the first of the synthetic fibers. Nylon s story begins in 1928 at DuPont Company with the hiring of Dr. Wallace H. Carothers. By 1935 the first nylon 6,6 polymers had been prepared and pilot plant production started in In 1939, the first nylon fiber plant went into production and the first stockings went on sale in the same year. Most production during World War II was focused on military uses, especially on parachute fabrics. Nylon was available for domestic uses in During that time, in 1931, in Germany, a parallel development was occurred leading nylon 6. Some coarse monofilaments were produced in 1939 with small scale production of continuous filament in 1940 and a larger scale production a year later [1, 5, 6]. 7

21 Nylon fibers have monomer units joined by amide groups [ CONHRNHCOR' and are usually prepared from diamines and dicarboxylic acids, or, in the case of [ RCONH, from lactams. If R and R are aliphatic, alicylic, or mixtures containing less than 85 wt % aromatic moieties, the polyamides usually are referred to as Nylon. If more than 85 wt % of the repeating units is aromatic structure, the fibers are called Aramids [6]. ] n ] n (CH 2 ) 5 O nhn C O H NH (CH 2 ) 5 C Nylon-6 n OH Nylon filaments are usually manufactured via melt spinning. The melting point of nylon- 6 is about 215 ºC [3]. Basically the molten polymer is extruded through a spinneret into a chamber where the melt solidifies in filament form. However, in order to achieve desirable properties in terms of molecular orientation and crystallinity, the newly formed filaments must be drawn. Since the glass transition temperature, T g, of nylon is below the room temperature, nylon can be cold drawn. Nylon filaments can be drawn up to several times their initial length. With the drawing promoting molecular orientation and hence increase in the elastic modulus of the Nylon fibers [3]. Table 2.1 Effect of drawing on Elastic modulus of Nylon-6 fibers [3] Draw Ratio Elastic Modulus [GPa]

22 Instead of having extrusion and drawing as two separate processes, a one step high-speed spinning can also being used. In this process, the filament windup speed is significantly higher than the extrusion speed that orientation and crystallinity in the fibers develop in the spin line [3]. Nylon-6 is a semi-crystalline polymer with several possible crystalline polymorphs. Nylon-6, being a linear aliphatic polyamide, is able to crystallize because of strong intermolecular hydrogen bonds through the amide groups and van der Waals forces between the methylene chains [3]. The mechanical properties of nylon-6 depend on processing, drawing and the nature of heat setting. Typical drawn nylon filaments are strong, highly resilient and sensitive to moisture. Even though it is often thought to be a hydrophobic fiber, in practice it is significantly hydrophilic and can absorb water within the structure. Water is able to penetrate the amorphous regions and hydrogen bond to the amide groups. Being a good plasticizer for nylon-6, water increases the mobility of the molecular chains and reduces the tenacity, modulus and the T g. [3, 5] Polyamide fibers are resistant to chemical and microbial degradation. They are also electrical insulators. The fibers can be heat and moisture set and they return to their set shape after deformation if the setting conditions have not been exceeded [3]. 9

23 Table 2.2 Typical Properties of nylon fibers [3] Property Continuous Staple Filament Tenacity at break, N/Tex 65% rh, 21ºC Wet Extension at break, % 65% rh, 21ºC Wet Elastic Modulus, N/Tex 65% rh, 21ºC Moisture regain at 65% rh, % Specific Gravity 1.14 Approx. volumetric swelling in water, % PET Fibers Polyester fibers (poly(ethylene terephthalate) (PET)) fibers dominate the world synthetic fibers industry. A polyester fiber is composed of any long-chain synthetic polymer including at least 85 wt % of an ester of a dihydric alcohol (HOROH) and terephthalic acid (p-hoocc 6 H 4 COOH) [5, 6]. O O CH 2 CH 2 O C PET monomer O C n 10

24 The free terephthalic acid, or its methyl ester, is polymerized with ethylene glycol in vacuum by a condensation mechanism at elevated temperatures. The polymer may be isolated and formed into chips for subsequent handling, but the current trend is toward continuous processes where fiber formation immediately follows polymerization. Polyester fibers are usually produced via melt-spinning. The molted polymer jets solidify almost immediately after extrusion. Then, the filaments are drawn in order to improve their molecular orientation and crystallinity. As in the case of polyamide fibers, high speed spinning is beginning to replace the traditional two-step spinning and drawing process. Similar but fully equivalent, crystalline structures are developed in polyester by high speed spinning as well as by the two-step process. The properties of typical polyester fibers are summarized in Table 2.3. Table 2.3 Typical properties of Polyester fibers [3] Property Continuous Staple Filament Tenacity at break, N/Tex 65% rh, 21ºC Wet Extension at break, % 65% rh, 21ºC Wet Elastic Modulus, N/Tex 65% rh, 21ºC Moisture regain at 65% rh, % Specific gravity Approx. volumetric swelling in water, % none none 11

25 The tensile stiffness or elastic modulus at low strains is much higher for drawn polyester than for corresponding polyamides. Polyester exhibits high elastic recovery, especially for small deformations. A very important property of polyester is that its mechanical properties in the wet state and under standard conditions are practically the same. PET fibers have excellent resistance to acids, alkalies and microbial attack. They also have good resistance to light and actinic degradation. Polyester fibers have moisture regains about 0.4% under standard conditions which results with the fibers high electrical receptivity and creation of static electrification. The interactions between polyester and interactive chemical systems can lead to depression of T g, secondary crystallization and loss of orientation, which have an important affect on physical and mechanical properties [3] Microfibers For comparison, microfibers are half the diameter of a silk fiber, one-third the diameter of cotton fiber, one-quarter the diameter of fine wool fiber and one hundred times finer human hair. In order to be called a microfiber, a fiber must be less than one denier which is the weight in grams of a 9000m length of fiber or yarn. Many microfibers are 0.5 to 0.6 denier. Besides having a luxurious body and drape, microfiber fabrics are also lightweight resilient. They can retain their shape and resist pilling. Compared to other fabrics of similar weight, they are relatively strong and durable. Since fine yarns can be packed tightly together, microfiber fabrics have good wind resistance and water repellency. As the number of filaments in a yarn of given linear density increases, the surface area of all the fibers increases and the spaces between the fibers get smaller. 12

26 Liquid water is prevented by surface tension from penetrating the fabric, which will have a degree of water repellency. On the other hand, the spaces between the yarns are porous enough to breathe and wick body moisture way from the body [6, 7]. The production of microfibers depends on the fiber fineness. For the fibers up to 7µm in diameter, conventional melt extrusion can be used. For finer microfibers, the islands-inthe-sea (I/S) method can be used. In the I/S method, a number of bicomponent sheathcore polymer flows are combined into a single flow in the spinneret and extruded as a single fiber. A similar method involves the use of two polymers with poor adhesion to each other. After extrusion the polymer are separated and microfibers are obtained [6] Nanofibers In general, the definition of nano is one millionth (1/10 6 ) of a millimeter or 10-9 meter. When the term is applied to technology, nanotechnology, the common definition is the precise manipulation of individual atoms and molecules. For the polymeric nanofibers the smallest practical size is approximately 50 nm as a polyester crystallite has dimensions in the order of 40 nm so structures approaching this size would begin to become an ordered array of atoms and would not have typical fiber morphology [8]. Similar to the nature s design, polymeric nanofibers and their composites can provide fundamental building blocks for the construction of devices and structures. Drug delivery systems, scaffolds for tissue engineering; wires, capacitors, transistors and diodes for information technology; systems for energy transport; conversion and storage such as batteries and 13

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