Electron Microscopy Lab - PowerPoint Presentation

Electron Microscopy Lab Introduction to scanning electron microscopy The aims of this course are:● to introduce the principles of scanning electron microscopy● to describe the components of the microscope and explain how they work● to highlight some of the problems which can arise during imaging Click on the buttons to move between slides.(Make sure you are in “Slide Show” mode) Tutor: Peter Harris

Scanning electron microscopy is a technique for achieving high resolution images of surfaces. It involves scanning a fine beam of electrons over a specimen and detecting the signals which are emitted. The resolution of modern SEMs is of the order of 2 nm. This compares with a resolution of about 1 m for a conventional optical microscope. The transmission electron microscope, in which electrons pass through a very thin sample, has a higher resolution than the SEM (~ 0.1 nm). Imaging in the SEM must be carried out under vacuum, as electrons cannot travel through air. The basic components of the SEM are illustrated on the next slide.Units: 1 nm = 10-9 m; 1 m = 10-6 m Overview

Electrons emitted by the gun are accelerated, typically by 20 kV. They pass through condenser and objective lenses, and then through a set of scan coils and an aperture. A scan is simultaneously generated on a computer monitor. Electrons emitted by the specimen are detected, amplified and the signal is then used to produce an image.Components of the SEM

Schottky Field Emission Source High brightness Energy spread < 0.5 eVElectron sources A number of different kinds of electron source are used in SEM. The microscopes in CfAM use the following sources: Tungsten thermionic source This is simply a very fine tungsten wire, through which a current is passed. Characteristics This is a crystal to which a very high voltage is applied. Low brightness Energy spread ~ 1-2eV Characteristics

Electromagnetic lenses All modern SEMs use electromagnetic lenses. These consist of a coil of copper wires inside iron pole pieces. solenoid of wire together with a magnetic pole piece that creates and concentrates a magnetic field. A current through the coils creates a magnetic field, symbolized by red lines in the diagram on the left. Electrons close to the centre are less strongly deflected than those passing through the lens far from the axis.

Interaction of electrons with specimen When high energy electrons impinge on the specimen, a number of signals are generated: ● Backscattered electrons – these are high energy electrons which are scattered out of the specimen, losing only a small amount of energy.● Secondary electrons – these originate in the specimen itself, and have a much lower energy than the backscattered electrons (typically < 50 V).● X-rays - These give information about the elemental composition of the sample.

Information given by secondary and backscattered electrons Secondary electrons originate from within a few nm from the surface. They are therefore very sensitive to surface structure, and provide topographic information. Backscattered electrons originate from much deeper within the sample (a few m below the surface), and interact much more strongly with the sample. They therefore provide compositional information, but give lower resolution images.

Detectors: secondary electrons The detector for secondary electrons is the Everhart Thornley Detector (ETD).This consists of a scintillator that emits photons when hit by high-energy electrons. The emitted photons are collected by a lightguide and transported to a photomultiplier for detection.A metal grid known as a Faraday cage surrounds the scintillator, and is usually held at a positive potential to attract the secondary electrons.

Origin of topographic contrast in secondary electron images In order to obtain an image in the SEM, we must have some variation in the signal from different parts of the specimen. The yield of secondary electrons is at a minimum when the surface of the specimen is perpendicular to the electron beam. This is because of the shape of the interaction volume and its relationship to the surface of the specimen, as shown here. At regions of the specimen which are not exactly perpendicular to the beam, electrons are more likely to be scattered out of the specimen, rather than further into the specimen. Hence, such regions appear bright in the secondary electron image. Fewer 2ndaryelectrons escapeMany 2ndaryelectrons escape Sample

Detectors: backscattered electrons Backscattered electrons can be detected using an Everhart Thornley detector, by applying a negative potential to repel the secondaries. However, the collection efficiency of such an arrangement is low. As the name suggests, backscattered electrons are strongly scattered back in the direction of the incident beam. Therefore, the detector for these electrons is generally placed around the final lens, as shown. Backscattered electron detectors are usually solid state devices. The electrons which impinge on the detector produce electron-hole pairs which produce a current which can be amplified.

Resolution in the SEM The resolution of the SEM is determined by the size of the incident beam. This can be reduced by introducing an aperture unto the beam path and by reducing the probe size using the condenser lens. Note that reducing the probe size using the condenser lens also reduces the beam current (for an explanation, see Goodhew et al., p. 131). Therefore, as you reduce the probe size you eventually reach a point where imaging is impossible. For a typical SEM operating at 20 kV, the minimum usable probe size is of the order of 1 – 3 nm. Resolution also depends on accelerating voltage. This is because higher energy electrons experience less spherical aberration when they pass through the lenses. Resolution is also improved by reducing the working distance, up to a certain point. Beyond that point the lenses may not be able to focus the beam on the sample. As already noted, images obtained with backscattered electrons have a lower resolution than these obtained with secondary electrons, because they originate from deeper within the specimen.

Depth of field 1 Depth of field is the distance above and below the plane of optimum focus within which the image is in focus. In the diagram on the right, d represents the diameter of the electron beam at the specimen. The depth of field is h, since it makes no difference to the sharpness of the image if the object is anywhere within the range h.Reducing the angle α increases the depth of field. This can be achieved by using a smaller aperture or by increasing the working distance.

Depth of field 2 These diagrams illustrate the effect of the convergence angle α on the depth of field. Because of the geometry of the imaging system, scanning electron microscopes have a much greater depth of field than optical microscopes .

Astigmatism 1 Astigmatism is a problem that is commonly encountered in SEM (and TEM). It is an aberration of lenses that causes rays in a plane parallel to the optical axis to be focused at a different focal point from rays in a plane at 90° to it . The effect of astigmatism is that objects in the image generally appear “stretched” in one direction, and then in the other direction as you go through focus.All electron microscopes are equipped with stigmators, which allow the user to correct the astigmatism, as shown in the next slide. Properly corrected astigmatism is essential in achieving high resolution images.

Astigmatism 2 The SEM images shown below left illustrate how astigmatism affects the image as you go through focus. On the right is shown the image following correction with the stigmators. Astigmatic Corrected

Spherical aberration Spherical aberration is less important in the actual operation of the SEM than astigmatism, but it is important to understand what it is. A lens suffers from spherical aberration if it focuses rays more tightly if they enter it far from the optic axis than if they enter closer to the axis. It therefore does not produce a perfect focal point. This is illustrated in diagram A on the right.

Chromatic aberration Like spherical aberration, this is not usually a major problem in SEM, except in high resolution or low voltage operation. It is caused by a lens having a different refractive index for different electron energies. Chromatic aberration is present in all electron lenses, but can be reduced by minimising the energy spread of the electron source. Field emission sources have the lowest energy spread.

Charging In order to avoid this problem, specimens can be covered with a conducting coating of gold or carbon. An alternative to coating is to use a “low vacuum” SEM. This kind of microscope operates with a small pressure of water vapour in the chamber. The water molecules become positively charged and neutralize the negatively charged regions on the surface.When a poorly conducting specimen is imaged in a conventional SEM, the surface rapidly accumulates charge. This can result in a severely distorted image, as the incident electrons are repelled by the charged areas of the surface. A typical feature of charging is that some regions appear extremely bright, as can be seen here.

The recommended book for this course is "Electron microscopy and analysis", by Goodhew, Humphreys and Beanland. Further informationPeter Harris and other members of EMLab staff will be happy to answer your questions. Links to some useful websites can be found on the “SEM course” page.