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TRIBOLOGY LAB- REPORT

Optical Microscope & SEM


Ajay Kumar Verma( P2008 me1104)

OPTICAL MICROSCOPY
The use of "Optical Microscopes" in "Materials Evaluation" is very popular since it enables the researcher to observe the "internal structure" of materials. This information can then be used to improve material processing and properties which form the foundation of materials science and engineering (MSE). The microstructure generally ranges from the atomic scale (0.1nm) to 1mm(1000m) with the most widely used scale of 1-1000 m. Practically the optical microscopes can be used up to 2000x at which the resolution becomes so poor that objects smaller than 1 m cannot be distinguished. But since most materials have grain sizes in the range 1-100m optical microscope (OM) is a perfect low cost tool. Typical microstructural features are grains(single crystal), precipitates, inclusions, pores, whiskers, defects, twin boundaries, etc. Most of the manufacturers use OMs for process control and R&D. There are mainly two types of optical microscopes (OM): Reflected Light (RL) Transmitted Light (TL). In the former the light is reflected from the surface of the specimen while in the latter the sample is so thin (20-50m) that light passes through it. A third but less important type may be the stereo microscopes that do not require any sample prep and are generally used to observe fracture surfaces, electronic curcuit boards, etc.

Reflected Light Optical Microscopes are the most widely used machines in materials science. Because they involve light reflection the specimen surface must be very well polished to a "mirror finish". In order to have a mirror finish the sample goes through a number of "sample preparation treatments"

1) Cutting: Specimen should be cut to <1.25 inch with a hacksaw or a disc saw. Care must be taken not to heat the sample during cutting. (2) Mounting: Hot mounting in a press w/phenolic resin or cold mount in polyester. The former is faster and more generally used for metals while the latter is favored for ceramic samples. (3) Grinding: Successively sized SiC grinding papers (180-320-600-1200 Grit) are rotated on a wheel (~50-250 rpm) and the sample is pushed face down while watercooling. Small SiC particles are glued to the grinding paper so these are also sometimes called fixed abrasives. These particles slowly remove chips from specimen surface. (4) Polishing: Same as grinding except the abrasive particles are loose and no watercooling is performed. Diamond or alumina suspension having particles 0.05 30m diameter are used. (5) Etching: Selective removal of certain microstructural features to reveal the internal structure. Use a hood and do not inhale acid vapor. Wash the specimen thoroughly to avoid damage on objective lenses. Because OM examination of any material is actually a sampling operation from a larger material, care must be taken not to change the microstructure during sample preparation. It is important that the sample must be representative. The sample is examined in OM in two main modes: (1) Bright Field (BF): The polished surface appears bright and the surface irregularities such as grain boundaries appear dark. The reason why grain boundaries appear dark can be clearly seen in the figure. Light reflected from the grain boundaries do not go back to the objective. The same thing is true for precipitates that also appear dark. BF mode is more commonly used than DF.

Light from an incandescent source is aimed toward a lens beneath the stage called the condenser, through the specimen, through an objective lens, and to the eye through a second magnifying lens, the ocular or eyepiece. The condenser is used to focus light on the specimen through an opening in the stage. After passing through the specimen, the light is displayed to the eye with an apparent field that is much larger than the area illuminated. Typically used on thinly sectioned materials.

(2) Dark Field (DF): The incident light is fed from an angle therefore polished smooth surface appears dark and surface irregularities appear bright. DF is less commonly used. Applications are generally in grain size measurements and in judging the quality of polishing. To view a specimen in dark field, an opaque disc is placed underneath the condenser lens, so that only light that is scattered by objects on the slide can reach the eye. Instead of coming up through the specimen, the light is reflected by particles on the slide. Everything is visible regardless of color, usually bright white against a dark background.

Limitations of light-optical microscopy The amount of information a micrograph can provide is dependent on resolution. The maximum resolution that can be achieved using a microscope means the smallest interval distinguishable between two adjacent points. Any magnification exceeding such maximum would not make sense since further information cannot be provided.

SCANNING ELECTRON MICROSCOPE


The scanning electron microscope (SEM) uses a focused beam of high-energy electrons to generate a variety of signals at the surface of solid specimens. The signals that derive fromelectron-sample interactions reveal information about the sample including external morphology (texture), chemical composition, and crystalline structure and orientation of materials making up the sample. In most applications, data are collected over a selected area of the surface of the sample, and a 2-dimensional image is enerated that displays spatial variations in these properties. Areas ranging from approximately 1 cm to 5 microns in width can be imaged in a scanning mode using conventional SEM techniques (magnification ranging from 20X to approximately 30,000X, spatial resolution of 50 to 100 nm). The SEM is also capable of performing analyses of selected point locations on the sample; this approach is especially useful in qualitatively or semiquantitatively determining chemical compositions (using EDS), crystalline structure, and crystal orientations (using EBSD). The design and function of the SEM is very similar to the EPMA and considerable overlap in capabilities exists between the two instruments.

Fundamental Principles of Scanning Electron Microscopy (SEM)


Accelerated electrons in an SEM carry significant amounts of kinetic energy, and this energy is dissipated as a variety of signals produced by electron when the incident electrons are decelerated in the solid sample. These signals include secondary electrons (that produce SEM images), backscattered electrons (BSE), diffracted backscattered electrons (EBSD that are used to determine crystal structures and orientations of minerals), photons (characteristic X-rays that are used for elemental analysis and continuum X-rays), visible light (cathodoluminescence--CL), and heat. Secondary electrons and backscattered electrons are commonly used for imaging samples: secondary electrons are most valuable for showing morphology and topography on samples and backscattered electrons are most valuable for illustrating contrasts in composition in multiphase samples (i.e. for rapid phase discrimination). X-ray generation is produced by inelastic collisions of the incident electrons with electrons in discrete ortitals (shells) of atoms in the sample. As the excited electrons return to lower energy states, they yield X-rays that are of a fixed wavelength (that is related to the difference in energy levels of electrons in different shells for a given element). Thus, characteristic X-rays are produced for each element in a mineral that is "excited" by the electron beam. SEM analysis is considered to be "non-destructive"; that is, x-rays

generated by electron interactions do not lead to volume loss of the sample, so it is possible to analyze the same materials repeatedly. Essential components of all SEMs include the following: Electron Source ("Gun") Electron Lenses Sample Stage Detectors for all signals of interest Display / Data output devices Infrastructure Requirements: o Power Supply o Vacuum System o Cooling system o Vibration-free floor o Room free of ambient magnetic and electric fields SEMs always have at least one detector (usually a secondary electron detector), and most have additional detectors. The specific capabilities of a particular instrument are critically dependent on which detectors it accommodates.

Applications
The SEM is routinely used to generate high-resolution images of shapes of objects (SEI) and to show spatial variations in chemical compositions: 1) acquiring elemental maps or spot chemical analyses using EDS, 2)discrimination of phases based on mean atomic number (commonly related to relative density) using BSE, and 3) compositional maps based on differences in trace element "activitors" (typically transition metal and Rare Earth elements) using CL. The SEM is also widely used to identify phases based on qualitative chemical analysis and/or crystalline structure. Precise measurement of very small features and objects down to 50 nm in size is also accomplished using the SEM. Backescattered electron images (BSE) can be used for rapid discrimination of phases in multiphase samples. SEMs equipped with diffracted backscattered electron detectors (EBSD) can be used to examine microfabric and crystallographic orientation in many materials.