22 SEM Scanning Electron Microscopy JEFFREY B, BINDELL Contents * Introduction * Physical Basis and Primary Modes of Operation + Instrumentation * Sample Requirements * Applications * Conclusions {instrument that would come to mind for small scale materi- be the optical microscope. The optical microscope look at most samples and could be used to routinely doc- ‘an investigation. As the sophistication of investigations cope often has been replaced by instrumentation hav- lution or depth of focus. However, its use has continued availability of the tool. materials characterization, the optical microscope more potent instruments: the Transmission Electron Scanning Electron Microscope (SEM). Because of its range of information that it provides in a timely man- the optical microscope as the preferred starting tool for or with a highly magnified image of the surface to what one would expect if one could actually “see” to simplify image interpretations considerably, but IMAGING TECHNIQUES Chapter 2ELECTRON SOURCE DEFLECTION ‘AMPLIFIER —Hill @- BEAM CAT DEFLECTION | 2 COIL | DETECTOR 5 | A SCREEN SIGNAL SAMPLE Figure 1 ‘Schematic describing the operation of an SEM. reliance on intuitive reactions to SEM images can, on occasion, lead to erroneous results. The resolution of the SEM can approach a few nm and it can operate at magnifications that are easily adjusted from about 10x-300,000x. Nor only is topographical information produced in the SEM, but information i ition near surface regions of the material is provided as well. important instruments closely related to the SEM, nota- (EMP) and the scanning Auger microprobe (SAM). well as the TEM, are described in detail elsewhere in trons is focused (in vacuum) into a fine probe that is specimen, Figure 1. As the electrons penetrate the Ms occur that can result in the emission of electrons the surface. A reasonable fraction of the electrons propriate detectors, and the output can be used to thode ray tube (CRT) whose x and inputs are x-yvoltages rastering the electron beam, In this way T; every point that the beam strikes on the sample ponding point on the screen. If the amplitude of the x and deflection amplifiers in the SEM is CRT saw-tooth voltage is kept fixed at the level nnecessary to produce a full screen display, the magnification, as viewed on the screen, will be increased by the same factor. f images produced in the SEM are of three types: secondary electron ‘tered electron images, and clemental X-ray maps. Secondary and ns are conventionally separated according to their energies. They are produced by different mechanisms, When a high-energy primary electron intemets with an atom, itundergoes either inelastic scattering with avomic electro} or elastic scattering with the atomic nucleus. In an inelastic collision with an cle tron, some amount of energy is transferred to the other electron. Ifthe energy trans~ feris very small, the emitted electron will probably not have enough energy to exit the surface. Ifthe energy transferred exceeds the work function of the material, the emitted electron can exit the solid. When the energy of the emitted electron is less than about 50 eV, by convention it is referred to as a secondary electron (SE), or simply a secondary. Most of the emitted secondaries are produced within the first few nm of the surface. Secondaries produced much deeper in the material suffer additional inelastic collisions, which lower their energy and trap them in the inte- rior of the solid. Higher energy electrons are primary electrons that have been scattered without Joss of kinetic energy (i.e., elastically) by the nucleus of an atom, although these col- lisions may occur after the primary electron has already lost some of its energy to inelastic scattering. Backscattered electrons (BSEs) are considered to be the clec- i cimen with an energy greater then 50 cV, including Auger BSEs have energies comparable to the energy of the pri- atomic number of a material, che more likely it is that Thus as a beam passes from a low-Z (atomic number) to fue to backscattering, and consequently the image bright- fa built in contrast caused by elemental differences. wn the secondary electron contributions into three AI. SEIs result from the interaction of the incident beam of entry. SEIIs are produced by BSE s on exiting the ed by BSEs which have exited the surface of the sample ‘components on the interior of the SEM usually not and SEIIIs come from regions far outside that defined ‘can cause serious degradation of the resolution of the rimary beam current ig, the BSE current igsp, the SE current transmitted through the specimen to ground nt law holds: (1) IMAGING TECHNIQUES — Chapter 2nt is “These signals can be used co form complementary images. As the beam curfent see sod, each of these currents will also increase. The backscattered electron yi r hand the secondary electron yield 8, which refer to the number of backscattere 11d secondary electrons emitted per incident electron, respectively, are defined by the relacionships ‘BSE Q) (3) In most currency available SEMs, the energy of the primary electron beam can range from a few hundred eV up to 30 keV. The values of 6 and 7 will change over this range, however, yielding micrographs chat may vary in appearance and infor- mation content as the energy of the primary beamt is changed. ‘The value of the BSE yield increases with atomic number Z, but its value for a fixed Z remains constant forall bam energies above 5 keV. The SE yield 8 decreases slowly with increasing beam energy after reaching a peak at some low voltage, usually around 1 keV. Foe any fixed voltage, however, 8 shows very little variation over the full range of Z Both the secondary and backscattered electron yields increase with decreasing glancing angle of incidence because more scattering occurs closer to the surfsce jor reasons why the SEM provides excellent topographical as the surface changes its slope, the number of secondary as well. With the BSEs this effect is not as prominent, BSE detector would have to be repositioned to measure interaction of major importance in the SEM occurs when fides with and ejects a core electron from an atom in the I decay to its ground state by emitting either a character- electron (see the article on AES). The X-ray emis- energy in an energy dispersive X-ray detector (see the igth with a wavelength spectrometer (see the article on are characteristic of the elements that produced them ignals to produce elemental images that show the spa- elements in the field of view. The primary electrons ces into a solid before losing enough energy through to excite X-ray emission. This means that large vol- X-ray emission for any position of the smaller pri- the spatial resolution of this type of image will rarely 3e f the same region of a specimen in various imaging modes on a ‘SEM: (a) and (b) SE micrographs taken at 25 and 5 keV. (c) backscattered image taken at 25 keV; (d) EDS spectrum taken sh phase of the Pb-Sn solder; (e) and (f) elemental maps of the taken by accepting only signals from the appropriate spectral \s. uussion can be seen in Figure 2, which is a collection of fe surface of a Pb-Sn solder sample contaminated with a igure 1a, a secondary eléctron image (SE) taken with a distinguishes the two Pb-Sn eutectic phases as brighter arated by darker bands corresponding to the Sn-rich finally was taken at a magnification of 4000x but care ing published examples because of the likelihood of reduction by the printer. Most SEMs produce a graph chat defines the actual magnification. In the dors at the bottom of the micrograph span a physical used as an internally consistent ruler for measure- IMAGING TECHNIQUES — Chapter 2The mi the eee nlcrograph also shows the presence of a scratch that goes diagonally across ent i aces ee of er ee the appearance of depth to this scratch as a result of k secondary clectron yield with the local slope of th - tial resolution of the SEM due to SEs usually ih ae s proves with increasing energy of the primary beam because the beam can be focusec acess 1 into a smaller spot. C p » a smaller spot. Conversely, at higher energies the increased penetration of the electron beam into the sample ha oe the interaction volume, which may cause some degradation of the image resolution due to SE ls and SEIIIs. This is shown in Figure 2b, which is a SE image taken at only 5 keV. In this case the reduced electron penetration brings out more surface detail in the micrograph There are two ways to produce a backscattered electron image. One is to put a grid between the sample and the SE detector with a -50-V bias applied to it. This will repel the SEs since only the BSEs will have sufficient energy to penetrate the clectric field of the grid. This type of detector is not very effective for the detection of BSEs because of its small solid angle of collection. A much larger solid angle of collection is obtained by placing the detector immediately above the sample to col- lect the BSE. Two types of detectors are commonly used here. One type uses par- tially depleted n-type silicon diodes coated with a layer of gold, which convert the incident BSEs into electron-hole pairs at the rate of 1 pair per 3.8 eV. Using a pair of Si detectors makes it possible to separate atomic number contrast from topo- graphical contrast. The other detector type, the so-called scintillator photo muli- plier detector, uses a material that will fluoresce under the bombardment of the ce a light signal that can be further amplified. The pho- tused to produce the BSE micrograph in Figure 2c. Since present, the surface topography of the scratch is no fic number contrast appears. ‘can be used to estimate concentrations in binary alloys ‘increases somewhat predictably with the concentra- ‘of the pair. 1d wavelength-dispersiv e X-ray detectors can be used SEM, The detectors produce an ourput signal that is fof X-ray photons in the area under electron bombard put is displayed as a histogram of counts versus X39 ven in Figure 2d. This spectrum was producsd 1 Me lon one of the Pb-ich areas ofthe sample. The ike corresponding to Pb and a small amous t ved with Cu, the small Cu peak 2 nly a range of pulses cor reritic of 2Figure 3 Photograph of a modern field emissi M. rt RA ield emission SEM. (Courtesy of Ine. oowiany (Courtesy of AMRAY Ine. tify portions of the SE or BSE image having specific local compositions. The data usually can be quantified through the use of appropriate elemental standards and well-established computational algorithms. faph of a recent model SEM. The main features of ¢ column containing the electron source (i.e., the gi , the sample vacuum chamber and stage region (at the the electronics console containing the control panel, jes and the scanning modules. A solid stare EDS X-ray to the column and protrudes into the area immediately ics for the detector are in separate modules, but there integration into the SEM system architecture. fe electron gun is to produce a source of electrons ema- as possible, The lenses act to demagnify this spot and in itself produces clectron emission from a small area ly before presenting it to the lens stack. The actual jum in diameter and will be focused eventually into a A) he specimen. ‘of electron sources: thermionic tungsten, LaBg, and the first case, a tungsten filament is heated ro allow IMAGING TECHNIQUES — Chapter 2electrons to be emitted via thermionic emission. Temperacures as high as 3000° C are required to produce a sufficiently bright source. These planeta easy "i work with but have tobe replaced frequently because of evaporation. ‘The materi LaBg has a lower work function chan tungsten and thus can be epecutel 3 act temperatures, and it yields a higher source brightness. However, pars ‘to require a much better vacuum then tungsten to achieve good stability and a ee lifetime. The brighter the source, the higher the current density in the spot, whic! consequently permits more electrons to be focused onto the same area of a speci- men. Recently, field emission electron sources have been produced. These tips are very sharp; the strong electric field created at the tip extracts clectrons from the source even at low temperatures. Emission can be increased by thermal assistance but the energy width of the emitted electrons may increase somewhat. The sharper the energy profile, the less the effect of chromatic aberrations of the magnetic defo- cusing lenses. Although they are more difficult to work with, require very high vac- uum and occasional cleaning and sharpening via thermal flashing, the enhanced resolution and low voltage applications of field emission tips are making them the source of choice in newer instruments that have the high-vacuum capability neces- sary to support them. The beam is defocused by a series of magnetic lenses as shown in Figure 4. Each lens has an associated defining aperture that limits the divergence of the electron beam. The top lenses are called condenser lenses, and often are operated as if they were a single lens. By increasing the current through the condenser lens, the focal length is decreased and the divergence increases. The lens therefore passes less beam in the chain. Increasing the current through the first lens Produced (thus the term spot size for this control). It ting in beam current control as well. Smaller spot inumbers to correspond with the higher lens currents are attained with less current (signal) and a smaller igh magnification images therefore are inherently final lens—aperture combination. The final lens je beam onto the surface of the sample. The sample Ethat provides x- and motion, as well as tile with on about an axis normal to the specimen’s sur- adjustment of the distance between the final lens Ce is called the working distance. Timiting aperture size determine the convergence the convergence angle is a few mrad and it can aperture or by increasing the working distance. the more variation in the zdirection topogra- remaining in focus to some prescribed degree. res to the case of observation of topographical n———— SOURCE IMAGE azz =< — APERTURE —— CONDENSER LENS — APERTURE —+— CONDENSER LENS STIGMATOR AND DEFLECTION COILS ee FINAL LEI (azz io NS ®% — FINAL APERTURE SIGNAL =—° CONVERGENCE ANGLE —+——— SAMPLE STAGE Figure 4 Schematic of the electron optics constituting the SEM. the SEM is compared in Figure 5 with that of an opti- fication for viewing the top of a com: ie same magn ry little in regard co sample preparation, provided fompatible. If the sample is conducting, the major into the stage or, for that matter, into the specimen very large stage-vacuum chamber combinations Targe forensic samples (such as boots or weapons) wafers can be placed. For the latter case, special hhave been developed to allow for observation of ‘small working distances. re are still methods by which it can be studied in ach is to coat it with a thin (10-nm) conducting metal, In following this approach, care must be ‘tions that could be produced by nonuniform ig macerial. If an X-ray analysis is r0 \e coatin; IMAGING TECHNIQUES Chapter 2Figure 5 Micrographs of a machine screw illustrating the great depth of field of the SEM: (a) optical micrograph of the very tip of the screw; (b) and (c) the same area in the SEM and a second image taken at an angle (the latter shows the field quite clearly); (d) lower magnification image. Surface, care must be taken to exclude or correct for any the deposited material ples also can be studied by using low primary beam sne is willing to compromise image resolution to some tal electron yield as o = 8 + n, then when G < 1 we either trons from the specimen to avoid charge build-up. Con- ically takes care of this problem for conducting samples, ‘not occur, Consequently, one might expect it to be g samples in the SEM. The way around this difficulty ich plots as a function of energy of the incident elec- from 0 to some amount greater than 1 and then to energy increases. The «wo energy crossovers E and Ey, ging occurs, are often quite low, typically less than 9Figures _Total olectron yield as a function of the primary electron’s energy whan it arrives at the surface of the specimen. The energy scale in the figure is actually meant to depict the energy of the elec- tron as it arrives at the surface. Because of charging, the electron’s energy may be preater or less than the accelerating voltage would suggest. Consider electrons strik- nergy near E> as identified by point B in the figure. If the that of the crossover point, the total electron yield will be ce will be positively charged, thereby attracting incom- the effective energy of the primary beam. The elec- increase until E, is reached. Ifit overshoots, the yield charging will begin until, again, a balance is reached at a stable operating point for the insulator in question, point will allow excellent micrographs to be produced. at a stable operating condition. that has been coated with a thin oxide layer, a higher ually improve the image. The reason for this is that as rough the oxide, it can create electron-hole pairs in ish local conduction. This effect is often noted while vices that have been passivated with thin deposited icatil ials char- umber of applications of the SEM to materi ) imaging, Energy-Dispesive X-Ray analysis (EDS) measurements to determine the composition of briefly discuss applications that are, in part, spe- IMAGING TECHNIQUES Chapter 2cific to certain industries or technologies. Although there is significanc literature on applications of the SEM to the biological sciences, such applications will not be covered in this article. At magnifications above a few thousand, the raster scanning of the beam is very linear, resulting in a constant magnification over the entire image. This is not the case at low magnifications, where significant nonlinearity may be present. Uniform magnification allows the image to be used for very precise size measurements, The SEM therefore can be a very accurate and precise metrology tool. This requires careful calibration using special SEM metrology standards available from the National Institute of Standards and Technology. The fact that the SE coefficient varies in a known way with the angle that the pri- mary beam makes with the surface allows the approximate determination of the depth (2) variation of the surface morphology from the information collected in « single image. By tilting the specimen slightly (58°), sterco pairs can be produced that provide excellent quality three-dimensional images via stereoscopic viewers Software developments now allow these images to be calculated and displayed in three-dimension-like patterns on a computer scteen. Contour maps can be gener- ated in this way. The computer~SEM combination has been very valuable for the analysis of fracture surfaces and in studies of the topography of in-process inte- grated circuits and devices, Computers can be used both for image analysis and image processing, In the izedistributions of particles or features, and their associated measure- i circumference, maximum or minimum diameters, etc,) can luse the image information is collected via digital scanning in apacible with the architecture of image analysis computers. isa stored array of 500 x 500 signal values. Larger arrays sr memory capacity computers. fs to the manipulation of the images themselves. This smoothing, differentiation, and even image subtraction. mess in an image can be adjusted in a linear or nonlinear exist to highlight edges of features or to completely sup- dons. These methods allow the microscopist to extract the rmation from a single micrograph. As high-speed PCs to decrease in price while increasing in capacity, these re commonplace. a been a very fertile area for SEM application. The cney luced by a material in the SEM has been shown to ati tial of the surface. This phenomenon allows a way to measure voltages on the surfaces of Ge Tee lished using energy analysis of the SEs and by dirty ‘The measurements can be made very rapidly so a i ‘c nodes can be determined accurately. lar internal ci 81ic Very high frequency operation of circuits can be observed by eee ee techniques, blanking the primary beam at very high frequencies and by cov/ecting information only during small portions of the operating cycle. By sliding the view- ing window over the entire cycle, a waveform can be extracted with surprising sen- sicivicy and temporal resolution. Recently, special § instruments have been designed that can observe high-speed devices under nominal operating conditions. ‘The cost of these complex electron beam test systems can exceed $1,000,000. Actually, any physical process that can be induced by the presence of an electron beam and thac can generate a measurable signal can be used to produce an image in the SEM. For example, when a metal film is deposited on a clean semiconductor surface, a region of the semiconductor next to the metal can be depleted of mobile charge. This depletion region can develop a strong electric field. Imagine the metal to be connected through a current meter to the back side of the semiconductor sur- face. No current will flow, of course, but we can turn on an el etrates the metal and allows the impinging electrons to create electron-hole pairs. The electric field will separate these carriers and sweep them out of the depletion region, thereby generating a current, Among other things, the current will be deter- mined by the perfection or the chemistry of the spot where the beam strikes, By scanning the beam in the SEM mode, an image of the perfection (or chemistry) of the surface can be generated. This is referred to as electron beam-induced conduc- tivity, and it has been used extensively to identify the kinds of defects that can affect i tor device operation. used to provide crystallographic information, Surfaces that (fracture surfaces, etched, or decorated surfaces) can obvi- to grain size and shape. Electrons also can be channeled when channeling occurs, fewer backscattered electrons ineling patterns so generated can be used to determine lectron beam that pen- an electron beam strikes a crystal also can be dif- ich they are produced. Ifa photograph is made of this pattern) using a special camera, localized crystallo- fields affect the trajectories of the the SEM a useful tool for observing the magnetic terials, magnetic tapes, and disk surfaces. Pulsed elec- and acoustic signals which can be imaged to pro- ips of materials. Some semiconductors and oxides iolet, visible, or infrared regions, and these cathod- valuable information about the electronic properties ion of this method to semiconductor lasers or LED 1. Even deep-level transient spectroscopy, a method erpret and that provides information about impu- IMAGING TECHNIQUES — Chapter 2i od ti tities having energy levels within the band gap of semiconductors, has been uscd’ £0 produce images in the SEM. Conclusions Every month a new application for the SEM appears in the lirerature, no reason ro assume that this growth will cease. The SEM is one of the more versa- tile of analytical instruments and it is often the first expensive instrument that 2 characterization laboratory will purchase. As time goes on, the ultimate resolution of the SEM operated in these modes will probably level our near 1 nm. The major growth of SEMs now seems to be in the development of specialized instruments. An environmental SEM has been devel- oped that uses differential pumping to permit the observation of specimens at higher pressures, Photographs of the formation of ice crystals have been taken and the instrument has particular application to samples that are not vacuum compati- ble, such as biological samples. Other instruments have been described that have application in the electronics field. Special metallurgical hot and cold stages are being produced, and stages capa- ble of large motions with sub-um accuracy and reproducibility will become com- mon. Computers will be integrated more and more into commercial SEMs and there isan enormous potential for the growth of computer supported applications. At the i instruments will be developed and extended, such as the scan- ich uses liquid-metal ion sources to produce finely focused ‘SEs and secondary ions for image generation. The con- exhibited in these instruments can provide new insights and there is the Encyclopedia » Surface Roughness, AES, and CL lewbury, P. Echlin, D. C. Joy, C. Fiori, and E, Lif ‘and X-Ray Microanalysis, Plenum Press, New and widely ranging introductory textbook on related rechniques. Some biological applications Echlin, C. E. Fiori, and J. I. Goldstein. Microscopy and X-Ray Microanalysis. Plenum tinuation and expansion of Reference 1, level of difficulty.