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A fiber is defined as a unit matter characterized by flexiblity, fineness, and a high ratio of length sufficient high temperature stability and a certain minimum strength and extension are also required. Fine structure relates to the physical arrangements of molecules constituting the fiber from general consideration and also chemical analysis it is known that the molecules constituting the fiber are considerably long as compared to their width. Further these molecules are made a large number of smaller units called monomers repeating them several times. For this reason these fiber forming molecule are called as polymers (derived from Latin word poly-many and mer-unit).the unit of the polymer is the monomer, it is also derived from the Latin word mono-one. At the molecular level the polymer is extremely long and linear, whereas the monomer is very small. Monomers are usually chemically reactive where as the polymers are unreactive. “The chemical reaction which causes the monomers to join end to end to form a polymer is called polymerization.” Polymer are chemically unreactive this does not prevent its being subsequently attacked by chemicals and other degrading agents. The length of the polymer is important .all fibbers both of man-made or natural have to extremely long polymers. For measuring the length of the polymer is a complicated task and can be determined by its DEGREE OF POLYMERISATION. Degree of polymerization = average molecular weight of the polymer Molecular weight in repeating unit in the polymer
METHODS OF INVESTIGATION OF FINE STRUCTURE
The optical methods are not suitable for this purpose, since the smallest object which cannot be seen with the help of visible light is equal to its wavelength which is in the range of 0.5µ where as the molecules have dimensions of the order of few Ao . So we have to use the waves or rays which have a very fine wave length ( prefferably high frequency). Infrared rays,X-rays,and electron beam are used for investigation of fine structure of fiber.
Infrared red rays
The infrared radiation gives the idea about the atoms constituting the moleculrs and the type of bonds between them. Where as the X-ray gives the idea about the physical arrangement of the molecules,and the electron beam gives the idea very much enlarged images of fine stucture as agains the indiret information given by X-rays and infrared rays. The infrared radiation are composed of electromagnetic waves whose wave length varies between 1 µ -15 µ. When these rays are passed through the material , it is mostly absorbed at certain characterstic frequency. With the help of the sprectometer the variation in the absorption can found and plotted against wave length of more commonly called wave number. The wave number on which the absorption takes place depend upon the nature of two atoms and the bond between them. The absorption frequency of such group are as ≥C-H,>C=O, C-O-,-O-H-,>N-H, ,>C=C and so on. To a smaller extent it also depends upon the group of its neighborhoods. For example the absorption frequency for a carbon hydrogen bond in a terminant group is different from that for the same bond in(-CH2 -) therefore infrared spectroscopy can help in deducting the chemical structure of fiber. This method can also be used for estimating quantity of substance like water and other chemical present in the fiber.
Further if infrared rays are polarized than they give maximum absorption for orientation and minimum absorption at an orientation at right angles. This is also known as infrared diachroism. This can be used in investigate the degree of orientation of molecule in the fiber. An advantage of the infrared absorption meted is that it is influenced by all the molecule in the fiber in both the crystalline and non-crystalline regions. Whereas X-ray diffraction method gives detailed information only about crystalline region. One of the major techniques involves exposure of a material to the vapour of the heavy water (D2O) there by replacement of hydrogen atoms by deuterium atoms. In case of the fibers only non crystalline region are assessable to heavy water. Hydrogen atom of this entire region will be replaced by deuterium. Whereas as those in crystalline region will remain unaffected. From this difference in infrared absorption the percentage of two regions can be estimated.
X-RAY DIFFRACTION METHOD
If a beam of X-ray is directed at a crystalline region it is strongly reflected whenever it strikes the layer of atoms at an angle θ such that nλ=2dsinθ Where, n=integer, λ=wavelength of X-ray, d= distance between atomic layer. Under this condition the reflection from individual layer rain force each other since they are in phase with each other whereas at other angle they interface with one another.
There may be many layers of atoms of varying density in different direction. There will be a series of characteristics angle for each case. From these angles and from the variation in the intensity of reflection, the general crystal structure can be work out. In fibers we are not dealing with single crystal there will be a lot of small crystal and they are oriented parallel to the fiber axis. But it is simpler to consider first the diffraction pattern which is found where there is no preferred orientation. This is what we get, the process of passing an X-ray beam through powdered crystals is called powder photograph. For a strong reflection to occur the layer of atoms should make the required angle with X-ray beam. This will happen for a series of orientation of crystals distributed around a cone. The X-rays will be reflected around a cone of twice this angle. Due to this all the orientation present and all the other reflection will occur with the appropriate layers of the atoms distributed around the cones given in a characteristic angle of incidence.
Thus, the powdered photograph, therefore series of circles subtending angle can be determined by the distance between the layers of the atoms.
When there is a preferred orientation such that the layers are distributed round a cone making an angle of Ф as shown in fig below….
Now if an X-ray beam is passed at an right angle to the fiber axis, the reflection will occur at the four point of intersection of two cone as shown in fig. above and below…….each
Each of the layers of atoms will contribute different sets of four spots distributed symmetrically in the four quadrants and these will be repeated at different value of ‘n’. There are two special cases:1. If Ф =∏/2 then the cone of fig-2 become a plane cutting the other one in only two places& the reflection occur at two spots on the equator of the photograph. 2. If Ф = (∏/2—θ) than the two cones just touch and again we obtain two spots but this time at the poles. If Ф < (∏/2—θ) than no reflection occurs. If the orientation is not perfect we get reflection over a wide range of angle & the spots can be converted into arcs. Due to imperfect or varying crystal structure, the arcs become thicker in the radial direction. Apart from the strong reflection from the crystalline region , there is a scattering of X-rays from the non-crystalline region which gives the diffuse back ground from the relative intensities of the two, the proportion of crystalline and amorphous region can be obtained.
The observation of fine structure of fibers by optical microscope is restricted by the limit of resolution imposed by the wavelength of the light i.e., 0.5µ. The development of electron microscope enables picture to be obtained which shows much finer structure. The wavelength of electron used in electron microscope is of 0.05 A0 . In practice the best resolution so far obtained in the most favorable condition is about 5 A0 which almost enables to identify individual atoms of fiber or fine structure. There are mainly 3 types of electron microscope. They are as follows:1. Transmission electron microscope 2. Reflection electron microscope 3. scanning electron microscope
Transmission electron microscope
The ray from the electron source are condensed on the specimen and then focused by electric or magnetic fields acting as lenses to give a magnified image on a fluorescent screen or photographic plate. For the passage of electrons, it is necessary for the instrument to be evacuated. Only dry specimen can be examined. Contrast in the image depends on the variation on the scatterings of the electrons by the parts of the specimen of different density. The unscattered electrons are focused on the screen. The scattered electrons, which have lost their energy and slowed down, would come to focus at a different point. They form a diffuse background to a picture so reducing the contrast. In principle, the electron microscope is similar to the optical microscope. The electron beam is analogous to the ray of light where magnetic or electric fields are similar to optical lenses. On major advantage of electric lenses is that they can be continuously varied by varying the current but magnetic lenses are more preferable because there is no danger of high voltage as in case of electric lenses. One condition is provided in case of using the specimen in transmission electron microscope that the specimen should be very thin i.e. less than 0.1µ which allows the passage of electron.
Reflection electron microscope
This is useful for the direct examination of surface of materials against indirect method of replica technique used in the transmission electron microscope. The elements of this microscope are the same as that of the transmission type but the illuminating system (electron beam) is inclined at small angle ‘α’ (which generally lies between 80-150) to the axis of the instrument. The specimen which is not much thin is arranged with its surface at an angle ‘β’ such that α>β>α/2. The image is formed by objective and projector lenses system from electrons scattered or reflected from the specimen surface into the objective aperture. A thin layer or sliver is evaporated on to the specimen so as to make it conductive and prevent accumulate of charge. The magnification in the direction perpendicular to the plane of a incidence is much greater than that right angles to parallel, but because of great depth of focus of image a considerable length of fiber is in focus and it helps in evaluating the shape and surface characteristics. A serious drawback of this method is that the possibility of fiber damage by electron bombardment.
Scanning electron microscope
Scanning electron microscope uses a different approach to the direct examination of surface structure or fine structure. Electron lenses are used in illuminating source to form a generally reduced image of electron source (a very narrow and strong electron beam). The electron probe scans the specimen across by the electrostatic deflecting electrode as in a T.V. system. Secondary electrons leaving the specimen are collected directly into an electron amplifier and after amplification the signal is used to modulate the beam intensity of cathode ray tube. The beam starts scans the screen of the tube in synchronization with the scanning spot in the microscope. Thus an image is built on the screen of cathode ray tube. Although the intensity of the probe is high the average of electron intensity incident on the specimen is negligibly small so that chances of the fiber damage are less. The specimen is coated with a thin layer of film of evaporated metal to prevent the accumulation of charge on surface.
For getting proper contrast of image of the specimen or fine structure by electron microscope, we have to use the test specimen very thin. Since the fibers are mainly composed of lighter atoms they scattered the electrons to a lesser extent so that many of the scattered electrons reach the screen there by reducing the contrast. Improving contrast is one of the main problems in electron microscope.
As in the case of t5he optical microscope the specimen is held on a glass plate which is transparent to light. We need supporting films in electron microscope which do not scatter electrons but are strong enough to support the specimen. Generally colloidal or framework film are used. The films are prepared by dissolving this substance in a volatile solvents and spreading the solution either on a water surface or glass plate. The thickness is in the range of 100Ao. for the high resolution work carbon films are used which are prepared by evaporating a thin film of carbon on a substance which is subsequently dissolved away.
The contrast may be increased by evaporating on to the surface of the specimen or by thin coating of a suitable metal at a small angle. The metals used are paradium alloy of gold and palladium, chromium or platinum, since these metals have high atomic weight their scattering power is much more and hence they improve the contrast. The metal is evaporated in vacuum in such an angle that the shadow to object ratio is about 4:1. Knowledge of shadow angle and the length of shadow enable the height of the specimen above the supporting membranes to be determined.
Section for the examination in the electron microscope should be thinner than 0.1µ and some time they should be only a few hundred A0 thick. Special section
machine called “microtome” are available for this purpose. Since fibers are flexible a hard embedding medium is necessary during section cutting. The material is embedded in a mixture of butyl& methyl Meta crystal monomers which is than polymerized, epoxy resins are also used for this purpose. The forward movement of specimen on the microtome which is equal to the thickness read is obtained by the thermal expansions of a metal rod to ensure smooth and regulate movement. Steel glass and diamond knives are used for this section cutting. One of the limitations of this section is that some of the features observed may be a result of the section cutting.
This method overcomes the difficulties involved in the section cutting but they provide a different type of information. Fibers may be disintegrated into small fragments by mechanical action (grinding), irradiation with ultrasonic’s, dissolution by chemicals or enzymatic attack or by a combination of these techniques. The suspension of a disintegration product in a suitable liquid (generally water) is placed on a membrane coated grid and the liquid is allowed to evaporate. The particles from the suspension dry down on to the supporting film and are usually shadow cast to increase contrast. With this technique the fibril structure of cellulosic and fibers can be clearly visible and identified.
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