NDET ASSIGNMENT On

SCANNING ELECTRON MICROSCOPY

School of Mechanical and Building Sciences VIT University, Vellore 632 014

Submitted To PROF. DEVINDRAN S.

Submitted By

DEFINITION A scanning electron microscope (SEM) is a type of electron microscope that produces images of a sample by scanning it with a focused beam of electrons. The electrons interact with atoms in the sample, producing various signals that can be detected and that contain information about the sample's surface topography and composition. The electron beam is generally scanned in a raster scan pattern, and the beam's position is combined with the detected signal to produce an image. SEM can achieve resolution better than 1 nanometre. Specimens can be observed in high vacuum, in low vacuum, and in wet conditions. The most common mode of detection is by secondary electrons emitted by atoms excited by the electron beam. The number of secondary electrons is a function of the angle between the surface and the beam. On a flat surface, the plume of secondary electrons is mostly contained by the sample, but on a tilted surface, the plume is partially exposed and more electrons are emitted. By scanning the sample and detecting the secondary electrons, an image displaying the tilt of the surface is created.

SAMPLE PREPARATION All samples must also be of an appropriate size to fit in the specimen chamber and are generally mounted rigidly on a specimen holder called a specimen stub. Several models of SEM can examine any part of a 6-inch semiconductor wafer, and some can tilt an object of that size to 45. For conventional imaging in the SEM, specimens must be electrically conductive, at least at the surface, and electrically grounded to prevent the accumulation of electrostatic charge at the surface. Metal objects require little special preparation for SEM except for cleaning and mounting on a specimen stub. Nonconductive specimens tend to charge when scanned by the electron beam, and especially in secondary electron imaging mode, this causes scanning faults and other image artifacts. They are therefore usually coated with an ultrathin coating of electrically conducting material, deposited on the sample

either by low-vacuum sputter coating or by high-vacuum evaporation. Conductive materials in current use for specimen coating include gold, gold/palladium alloy, platinum, osmium. Additionally, coating may increase signal/noise ratio for samples of low atomic number (Z). The improvement arises because secondary electron emission for high-Z materials is enhanced. An alternative to coating for some biological samples is to increase the bulk conductivity of the material by impregnation with osmium using variants of the OTO staining method (O-osmium, T-thiocarbohydrazide, O-osmium). Non conducting specimens may be imaged uncoated using environmental SEM (ESEM) or low-voltage mode of SEM operation. Environmental SEM instruments place the specimen in a relatively high-pressure chamber where the working distance is short and the electron optical column is differentially pumped to keep vacuum adequately low at the electron gun. The high-pressure region around the sample in the ESEM neutralizes charge and provides an amplification of the secondary electron signal. Low-voltage SEM is typically conducted in an FEG-SEM because the field emission guns (FEG) is capable of producing high primary electron brightness and small spot size even at low accelerating potentials. Operating conditions to prevent charging of nonconductive specimens must be adjusted such that the incoming beam current was equal to sum of outcoming secondary and backscattered electrons currents. It usually occurs at accelerating voltages of 0.34 kV. Embedding in a resin with further polishing to a mirror-like finish can be used for both biological and materials specimens when imaging in backscattered electrons or when doing quantitative X-ray microanalysis.

IMAGE FORMATION IN SEM One of the most surprising aspects of scanning electron microscopy is the apparent ease with which SEM images of three-dimensional objects can be interpreted by any observer with no prior knowledge of the instrument. This is somewhat surprising in view of the unusual way in which image is formed, which seems to differ greatly from normal human experience with images formed by light and viewed by the eye.

The main components of a typical SEM are electron column, scanning system, detector(s), display, vacuum system and electronics controls. The electron column of the SEM consists of an electron gun and two or more electromagnetic lenses operating in vacuum. The electron gun generates free electrons and accelerates these electrons to energies in the range 1-40 keV in the SEM. The purpose of the electron lenses is to create a small, focused electron probe on the specimen. Most SEMs can generate an electron beam at the specimen surface with spot size less than 10 nm in diameter while still carrying sufficient current to form acceptable image. Typically the electron beam is defined by probe diameter (d) in the range of 1 nm to 1 m, probe current (ib)

pA to A; and probe convergence () 10-4 to 10-2 radians.In order to produce images the electron beam is focused into a fine probe, which is scanned across the surface of the specimen with the help of scanning coils. Each point on the specimen that is struck by the accelerated electrons emits signal in the form of electromagnetic radiation. Selected portions of this radiation, usually secondary (SE) and/or backscattered electrons (BSE), are collected by a detector and the resulting signal is amplified and displayed on a TV screen or computer monitor. The resulting image is generally straightforward to interpret, at least for topographic imaging of objects at low magnifications. The electron beam interacts with the specimen to a depth approximately 1 m. Complex interactions of the beam electrons with the atoms of the specimen produce wide variety of radiation. The need of understanding of the process of image formation for reliable interpretation of images arises in special situations and mostly in the case of high-magnification imaging. In such case knowledge of electron optics, beam-specimen interactions, detection, and visualization processes is necessary for successful utilization of the power of the SEM.

ADVANTAGES OF SEM The scanning electron microscope has many advantages over traditional microscopes. The SEM has a large depth of field, which allows more of a specimen to be in focus at one time. The SEM also has much higher resolution, so closely spaced specimens can be magnified at much higher levels. SEM uses electromagnets rather than lenses, the researcher has much more control in the degree of magnification. The actual strikingly clear images make the scanning electron microscope one of the most useful instruments in research.

DISADVANTAGES OF SEM Contamination The term contamination describes the collective phenomena by which the surface of a specimen undergoes deposition of a foreign substance, generally a carbonaceous material derived from the breakdown of hydrocarbon. The effect of this surface deposit is generally observed as a scan square when the magnification is reduced while centered on the previous field of view. Contrast arises in such image because of the change in the SE coefficient caused by the deposition of foreign material. This can be avoided by starting imaging at low magnifications and gradually increasing it. Contamination can affect the signal at high-resolution imaging. Hydrocarbon molecules are attracted to the beam location and form build-up, which obscures the fine detail features. Contamination can be reduced in first place by improving the vacuum in the specimen chamber. Also anti-contamination devices can be employed, which cool area in the close vicinity of the specimen so that hydrocarbon migration is reduced. This can be achieved also by cooling directly the sample. Charging When the beam interacts with the sample part of the incident electrons are emitted back, but larger fraction remains in the specimen as the beam electrons lose their initial energy and are captured by the specimen. This charge flows to ground if the specimen is conductor and a suitable connection exists to conduct away the charges. If the ground path is broken, even conducting specimen quickly accumulates charge and its surface potential rises. Charging is more often observed whenever a specimen or portion of it is an insulator. The charges injected by the beam cannot readily flow to ground. The resulting accumulation of charge is a complex, dynamic phenomenon. The specimen is in a continually changing state of surface potential due to the accumulation and discharge of electrons. Charging manifests itself in images in a variety of ways. When local charging alters the surface potential, the field lines of the detector potential, which exist around the sample, are disrupted, and collection of SE is greatly altered. A contrast mechanism develops known as voltage contrast in which the potential distribution across the surface is imaged. Some areas appear extremely bright because they are negative relative to the E-T detector and enhance SE

collection. Other areas appear black because they charge positively and suppress the collection of SE. The difficulty arises because the contrast due to surface potential becomes so large that it overwhelms the contrast from the true features of the sample.

These pollen grains taken on an SEM show the characteristic depth of field of SEM micrographs.