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Methods of inspecting Materials

Microscopes
Prepared by : Karim Sami Mohamed Mahmoud

Supervisor: Professor Dr. Osama Mounir Date : October 2012

Helwan University Faculty of Engineering class 2012-2013 Master Degree preparation year

Contents 1. 2. 3. 4. Objective scope Introduction Types of microscopes: 4.1 Light microscopy A. Single lens (simple) microscope B. Compound microscope 4.2 X-ray diffraction analysis 4.3 Electron Microscopy A. Transmission Electron Microscopes B. Scanning Electron Microscopes

1.Objective The objective of this report is to provide some information on the types of microscopes used to investigate the structure of material. The types used will be of the same order of magnitude of the structure to be studied. Not all types of microscopes will be discussed but the most popular ones. This report does not discuss in complex details of design of the types used but gives a brief over view of the theory of operation.

2. Scope This report will describe briefly few of the microscopes used in the field of metallurgy engineering and will describe only the limitation of use or the working range giving quick description of the theory ofoperation. The report will discuss the light microscope, X-ray diffraction microscope, and the electron microscope.

3. Introduction As the microstructure of material is very important in determining the properties of a material and studying the behavior of material during processes and working , then it is required to find a method to enable researcher and students to see and analyze the material structure in a clear resolution and magnification . The method to be used should be suitable to the order of magnitude of the required view or display. It will be of no great use to use unsuitable microscope , not providing clear image of the required part. From here it is essential to start by the size of the crystal structure, which depends on the atom size. The start will be determining the order of magnitude of the atom, the atom size is determined by its radius.

Definition : The atomic radius of a chemical element is a measure of the size of its atoms, usually the mean or typical distance from the nucleus to the boundary of the surrounding cloud of electrons The arrangement of the materials in the periodic table shows us the variation in atomic size of element, see fig 1-1, it can be seen that as we move to the left atomic radius increases, also as we move down the table the atomic radius increases.

Fig 1-1 periodic table showing how atom size change

Fig 1-2 shows a schematic drawing showing the size variation among the different element in the periodic table.

Fig 1-2 atom size variation in periodic table

The atomic radius of some elements are shown in table 1-1 Table 1-1 atomic radius for some elements in picometre Element Helium (He) Calcium (Ca) Silver (Ag) Sodium (Na) 1 m = 1,000,000,000,000 picometre (pm) 1m = 1,000,000,000 nanometer (nm) Atomic radius (picometre) 31 pm 197 pm 144 pm 190 pm

Grains The microstructure of metals and many other solids consists of grains. A molten metal is poured into a sand mold and allowed to air cool slowly will result in the production of coarse grains. Pouring a molten metal into a metal mold with enhanced cooling produces finer grains. Introducing forced circulation of water /oil in the metal mold produces even finer grain

structures. Fig 1-3 schematic drawing showing atoms arranged in a crystal lattice inside the grain boundaries

Fig 1-3 schematic drawing of grains

The order of magnitude of atoms in a single grain is in the order of 1018 atoms, which can indicate that the method used to examine the atomic structure is different from that examining the grains .

Is it more important the resolution or the magnification? The microscope, in its various forms, is the principal tool of the materials scientist. The magnification of the image produced by an electron microscope can be extremely high; however, on occasion, the modest magnification produced by a light stereomicroscope can be sufficient to solve a problem. In practical terms, the microscopist attaches more importance to resolution than magnification that is, the ability of the microscope to distinguish fine detail. In a given microscope, increasing the magnification beyond a certain limit will fail to reveal further structural detail; such magnification is said to be empty. Unaided, the human eye has a resolution of about 0.1 mm: resolution of light microscopes and electron microscopes are, respectively, about 200 and 0.5 nm. The resolution is a function of wave length.

4.Types of microscopes: 4.1 Light microscopy The light microscope provides two-dimensional representation of structure over a total magnification range of roughly 40 to 1250 Examination will reveal structural features such as shrinkage or gas porosity, cracks and inclusions of foreign matter

Fig 1-4 light microscope

There are two basic configurations of the conventional optical microscope: the simple (single lens) and the compound (many lenses). The vast majority of modern research microscopes are compound microscopes while some cheaper commercial digital microscopes are simple single lens microscopes. A magnifying glass is, in essence, a basic single lens microscope. In general, microscope optics are static; to focus at different focal depths the lens to sample distance is adjusted, and to get a wider or narrower field of view a different magnification objective lens must be used. Most modern research microscopes also have a separate set of optics for illuminating the sample.

A. Single lens (simple) microscope A simple microscope is a microscope that uses only one lens for magnification, and is the original design of light microscope. Van Leeuwenhoek's microscopes consisted of a small, single converging lens mounted on a brass plate, with a screw mechanism to hold the sample or specimen to be examined. Demonstrations by British microscopist have images from such basic instruments. Though now considered primitive, the use of a single, convex lens for viewing is still found in simple magnification devices, such as the magnifying glass and the loupe.

B. Compound microscope A compound microscope is a microscope which uses multiple lenses to collect light from the sample and then a separate set of lenses to focus the light into the eye or camera. Compound microscopes are heavier, larger and more expensive than simple microscopes due to the increased number of lenses used in construction. The main advantages of multiple lenses are improved numerical aperture, reduced chromatic aberration and exchangeable objective lenses to adjust the magnification. A compound microscope also makes more advanced illumination setups, such as phase contrast

Fig 1-5 Optical path in a typical microscope

4.2 X-ray diffraction analysis

X-ray crystallography is a method of determining the arrangement of atoms within a crystal, in which a beam of X-rays strikes a crystal and causes the beam of light to spread into many specific directions. From the angles and intensities of these diffracted beams, a crystallographer can produce a three-dimensional picture of the density of electrons within the crystal. From this electron density, the mean positions of the atoms in the crystal can be determined, as well as their chemical bonds, their disorder and various other information. X-ray crystallography has been fundamental in the development of many scientific fields. This method determined the size of atoms, the lengths and types of chemical bonds, and the atomic-scale differences among various materials, especially minerals and alloys. The use of diffraction methods is of great importance in the analysis of crystalline solids. Not only can they reveal the main features of the structure, i.e. the lattice parameter and type of structure, but also other details such as the arrangement of different kinds of atoms in crystals, the presence of imperfections, the orientation, sub-grain and grain size, the size and density of precipitates. X-rays are a form of electromagnetic radiation differing from light waves (=400800 nm) in that they have a shorter wavelength (0.1 nm). These rays are produced when a metal target is bombarded with fast electrons in a vacuum tube. The radiation emitted can be separated into two components, a continuous spectrum which is spread over a wide range of wavelengths and a superimposed line spectrum characteristic of the metal being bombarded. The energy of the white radiation, as the continuous spectrum is called, increases as the atomic number of the target and approximately as the square of the applied voltage, while the characteristic radiation is excited only when a certain critical voltage is exceeded. The characteristic radiation is produced

when the accelerated electrons have sufficient energy to eject one of the inner electrons (1s-level, for example) from its shell. The vacant 1s-level is then occupied by one of the other electrons from a higher energy level, and during the transition an emission of X-radiation takes place.

Fig 1-6 Workflow for solving the structure of a molecule by X-ray crystallography.

4.3 Electron Microscopy An EM is a microscope that focuses beams of energetic electrons to examine objects up to nano-scales. They utilize the same principles behind an optical microscope, but rather than photons or particles of light, concentrate electrons, charged particles located on the outside of atoms, onto an object. Additional differences include preparation of specimens before being placed in the vacuum chamber, the use of coiled electromagnets instead of glass lenses, the use of a thermionic gun as an electron source and the image or electron micrograph is viewed on a screen rather than an eyepiece. All EMs use electromagnetic and/or electrostatic lenses, which consist of a coil of wire wrapped around the outside of a tube, commonly referred to as a solenoid.

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In addition, EMs use digital displays, computer interfaces, software for image analysis and a low vacuum or variable pressure chamber, which upholds the pressure differential between the high vacuum levels essential to the gun and column area and the low pressure required in the chamber. In this microscope, images are produced from the interaction between the prepared samples in the vacuum chamber and energetic electrons. The electron beam passes through one or more solenoids and, with the aid of the thermionic electron gun, is directed down the column and onto the sample. Equivalent to the magnification that occurs from light refraction in an optical microscope, the coils in an EM bend the electron beams to create an image. The following gives you a description of two types of EMs,the Transmission (TEM) and Scanning Electron Microscope(SEM). A. Transmission Electron Microscopes The transmission electron microscope (TEM), the first type of EM, has many commonalities with the optical microscope and is a powerful microscope, capable of producing images 1 nanometer in size. They require high voltages to increase the acceleration speed of electrons, which, once they pass through the sample (transmission), increase the image resolution. The 2-d, black and white images produced by TEMs can be seen on a screen or printed onto a photographic plate. TEM technique : a beam of electrons is transmitted through an ultra thin specimen, interacting with the specimen as it passes through. An image is formed from the interaction of the electrons transmitted through the specimen; the image is magnified and focused onto an imaging device, such as a fluorescent screen, on a layer of photographic film, or to be detected by a sensor such as a CCD camera.

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TEMs are capable of imaging at a significantly higher resolution than light microscopes, owing to the small de Broglie wavelength of electrons. This enables the instrument's user to examine fine detaileven as small as a single column of atoms, which is tens of thousands times smaller than the smallest resolvable object in a light microscope. TEM forms a major analysis method in a range of scientific fields, in both physical and biological sciences. TEMs find application in cancer research, virology, materials science as well as pollution, nanotechnology, and semiconductor research.

Fig 1-7 Cross sectional diagram of an electron gun assembly, illustrating electron extraction

B. Scanning Electron Microscopes Reflecting light microscopes are the optical counterpart to scanning electron microscopes (SEM) and produce similar data. SEMs are primarily used to obtain topographical information. In this type of EM, a series of solenoids pulls the beam back and forth across the sample, systematically scanning the surface; it detects secondary electrons emitted from the surface and produces an image. Although SEMs are approximately 10 times less powerful than TEMs, they produce high-resolution, sharp, black and white 3D images.

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The primary advantage of Electron Microscopy is its powerful magnification. SEM begins with an electron gun generating a beam of energetic electrons down the column and onto a series of electromagnetic lenses. These lenses are tubes, wrapped in coil and referred to as solenoids. The coils are adjusted to focus the incident electron beam onto the sample; these adjustments cause fluctuations in the voltage, increasing/decreasing the speed in which the electrons come in contact with the specimen surface. Controlled via computer, the SEM operator can adjust the beam to control magnification as well as determine the surface area to be scanned.

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