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Scanning electron microscopy for materials characterization
David C Joy

Current materials are usually complex in chemistry, for heating, cooling, tensile or other special devices and
three-dimensional in form, and of rapidly diminishing because such experiments provide uniquely valuable data.
microstructural scale. To characterize such materials the
scanning electron microscope (SEM) now uses a wide range Driven by the needs of the semiconductor industry,
of operating conditions to target the desired sample volume, however, the predominant use of the SEM is as an
sophisticated modeling techniques to interpret the data. analytical imaging tool for the metrology of integrated
It also uses novel imaging modes to derive new types of circuits. Here the requirement is to be able to extract from
information. These include depth-resolved three-dimensional an image precise and accurate measurements of selected
data, and spatially resolved crystallographic data. features for the control of the fabrication processes. This
has been made feasible as a result of the development
of detailed Monte Carlo models of the electron solid
Addresses interaction occurring in the SEM [6**,7,8”]. It is now
Electron Microscopy Facility, Department of Biochemistry,
routinely possible to take an experimental image and then
Cellular and Molecular Biology, University of Tennesse, Knoxville,
TN 37996-0810 and High Temperature Materials Laboratory,
to compare it with a computed simulation of the same
Oak Ridge National Laboratory, Oak Ridge, TN 37931, USA; image, and by refining this match to iteratively deduce the
e-mail: parameters which describe the three-dimensional structure
Current Opinion in Solid State & Materials Science 1997, of the surface [9,10*]. Although difficult to apply to
2465-466 poorly characterized situations [ 1l] the technique is quite
successful when applied to the well defined geometry
Electronic identifier: 1359-0266-002-00465
encountered in semiconductor devices, although problems
0 Current Chemistry Ltd ISSN 1359-0286 arising from sample charging are still a limit to the accuracy
Abbreviation that is possible.
SEM scanning electron microscope
While the SEM is usually considered to primarily be a tool
for the visualization of surfaces, the electron beam does
penetrate many micrometers into the sample. Because
the penetration increases rapidly with the incident energy
The scanning electron microscope (SEM) is the most
this effect can be exploited to add the missing depth
versatile and widely used electron beam instrument in
dimension to imaging. For example, by choosing the
the world. It owes its popularity to the easily interpreted
energy of the incident beam and of the collected
nature of the micrographs that it generates, to the
backscattered electrons, information specific to a particular
diversity of types of information that it can produce,
depth beneath the surface of a specimen can be retrieved
and to the fact that images and analytical information
[12*]. A sequence of images obtained by appropriately
can readily be combined. As this review demonstrates
varying the incident and exit energies then produces a
the use of the SEM for materials characterization is
sequence of optical sections of the sample which can
increasingly motivated by the desire to obtain not just
be reconstructed into a full three-dimensional image.
images but quantitative information in two, or even
Because of the multiple scattering events experienced
three dimensions, about the microstructure, the chemistry,
by every electron [13,14”] there is significant mixing of
the crystallography and the electronic properties of the
information between successive layers and so the vertical
material of interest.
resolution is limited, but the method is a further important
step in moving the SEM image from two into three
SEM for materials characterization dimensions and provides a non-destructive visualization
The basic mode of use of the SEM has always been in the tool of significantly higher lateral spatial resolution than
imaging of surface topography, and 90% of the literature is X-ray microtomography.
still devoted to one aspect or another of this application.
The increasingly high level of the performance of the In some parallel developments it has been shown that a
SEM, in particular, makes it an excellent complement to sequence of cathode-luminescence (emitted light) images
high resolution transmission electron microscope imaging produced from suitable samples, as the beam energy
[1*,2] (as it provides the surface detail lacking in the is varied, can also be processed to yield a stack of
TEM micrograph) or to scanning tunneling or atomic force depth resolved slices through the specimen [1.5*,16]. This
microscopies, where it can provide images for comparison cathode-luminescent (CL) signal is produced by the decay
that are readily interpretable [3*]. The SEM is increasingly of the electron-hole pairs generated by the incident beam
being used for in situ and dynamic experiments [4,5] in a semiconductor or insulating material and the intensity
because there is ample room in the specimen chamber of the CL signal, as well as the form of its spectrum,

microanalysis was based information from sub-micrometer areas. grain boundaries. a value typical An alternative route for improving spatial resolution is of the magnitude of the strains found in high quality the use of low beam energies which offer much reduced epitaxial films. permitting [29**]. Some novel display quantitatively. and that the surface was smooth. SEhsI) is therefore well suited for the study of polymers [30-323 and other fragile and exotic materials such as snow A significant strength of transmission electron microscopy crystals [33”]. A unique feature of this technique is the beam interaction volumes but this raises the practical ability to synthesize an ‘Orientation Image’ in which. Secondary electron imaging capabilities of the SEhI now exceed those of the TEhl used in this way is. for problem that only low energy X-ray lines are accessible example. Once again if a sequence of images is the reduction in beam energy results in a decline in the obtained as a function of incident beam energy then depth depth of penetration of the electrons so that radiation resolved images can be generated [18*] which in this case induced damage is localized at the surface rather than represent a volume map of parameters such as the minority spread through a large volume. the three colors of an RGB (red-green-blue) and so peak overlaps become a major limitation. because it is a measure of the total electron yield [37’] . the application of one degree [23. A spatial resolution of the order of 1OOnm now a crucial issue. the concentration of dopants in a such an image is often many hours the detail and quality semiconductor [36”] even at levels corresponding to only of the information is unmatched by any other technique about one part per million. and electrically active defects in the structure of the sample to be observed. that approach to the determination of crystallography in the the sample was flat. The attraction of external and internal morphology of the material. These orientation images reveal clearly. This is. the technique is that it permits the successful observation of materials which are difficult or impossible to image The electron-hole pair signal can also be detected from the satisfactorily at higher beam energies. or nonconducting. and all probable peak overlaps can be separated. strategies for microanalysis are also under development. characterization and has been an important application crucial to the behavior of the material. The EBIC signal provides a unique specimens can be imaged without net charge build-up internal view of a semiconducting material. closely related to Auger analysis in their versatility and power. color-coded display are employed to represent the spatial new bolometric device technology for X-ray spectrometers variation of the three Euler angles describing the crystal [35**] offer sufficiently high energy resolution such chat orientation. It is therefore not necessary to use any surface direct visualization of all active junctions as well as of coating to confer conductivity allowing the true surface quantum wells. Schottky barrier. sample by extracting it as a current-the ‘electron beam because the increase in secondary electron emission at induced current’ (EBIC) signal-under the influence of a low energies can result in a state of dynamic charge field from either internal P-N junctions or from a surface balance at the specimen so that poorly. At the same time material [17]. While the fundamental limits set by is possible [ZZ’] with an angular precision of better than the electron-solid interactions remain. However. and also to directly image was chemically homogeneous over at least the beam dislocations in a bulk specimen [Zl]. An entirely different interaction volume of a few micrometers diameter. With the continual reduction in the scale yield the hIiller indices representing the crystallographic of microstructure the spatial resolution of an analysis is orientation. the of high brightness field emission guns on SEMs has now demands placed on microanalysis in the SEM are also made it possible to obtain both crystallographic orientation rapidly changing. SEhl is the technique of electron backscattering patterns For the problems encountered in today’s materials science (EBSP).*]. far below the concentrations and it can be claimed fairly that the crystallographic required for X-ray analysis. effects such as texturing [25’]. The development of the SEM since energy dispersive X-ray spectrometers of the technique of electron channeling [ 191 and the arrival first became available thirty years ago. The LVSEM (low voltage carrier diffusion length in the specimen. (TEM) as a materials characterization technique has been the availability of various modes of electron diffraction for the determination of crystal structure and for the imaging Microanalysis is an essential component of materials of dislocations. However. the sample of only about 0. In fact. So in this case the image is a map of say below 5 keV. which corresponds to an elastic strain within can reliably be detected under optimized conditions [34**]. Historically. control angular rotations as small as 0. with careful experimental hlonte Carlo simulations demonstrate that small features. in part. and other lattice defects. such as is required on the assumptions that the specimen to be analyzed for grain boundary studies [ZO].02% [24”].466 Characterization techniques depends on the type and concentration of dopant species The use of the SEM at low beam energies. the secondary electron image can reveal. detected. in fact. Although the time taken to derive a quantitative manner.01 degrees can be such as a monolayer of an element at a grain boundary. has now become the preferred mode the volume distribution of the chemistry as well as of the of operation for many applications [28]. recovery and recrystallization [26] and grain boundary For example. that is to in the material. In this mode of operation the angular distribution none of these assumptions are likely to be valid and of the backscattered electrons is imaged by a suitable so new procedures for obtaining and interpreting data detector and then analyzed automatically by a computer to are required. in misorientations [27*].

lvanov LN. 1996:150-l 52. Ajayan PM. An enormous range Zaluzec NJ. Drouin D. . . Brostin J: Scanning probe microscopy of polymers in the field- . Zaluzec NJ. Shimiru R: Monte Carlo modeling of electron interaction with solids. of corrosion [42’]. Excellent example of the synergism between the SEM and scanned probe The single most exciting recent contribution of the microscopies. published within the annual period of review. for three-dimensional reconstruction of luminescent materials. Balladore JL. 1996:676-678. As most of the standard imaging and analysis modes of the SEM can also be performed 11. Lloyd DJ: The structure of in the scanning electron microscope. Gerard P. unchanged. Howell PGT: A computer program to illustrate macro- . Beauvais J. Edited by . personal products [45’]. and NSEM configurations liberate the user from the prob. the formation of cement [43*]. 31:661-666. the 15426433. Hardingham C: Use of electron-beam induced current in a SEM 1. the variety and quality of the data that can be obtained principles. Dimlich R. Edited by promising new tool for characterization. References and recommended reading Papers of particular interest. Obyden SK: Morphologic and cathodolumines- cence studies of diamond films by scanning electron mi- croscopy. Ouabou A: Experimental micro-miniature three-dimensional structures [47”]. 1996:944- of real-world problems immediately become accessible for 946. Dimlich R. environment in which the pressure can be as high as 20 SCANNlNG 1996. Saparin GV. imaging effects such as the ability to see to the bottom of gutstanding mathematical description of the processes involved deep cracks and holes [41”]. J Microsc 1997. SCANNlNG 1996. development of the environmental (ESEM) or nature Kozlovskaya ED. Gauvin R. Michael JR. Sartore RG: Using secondary electrons to obtain improved lems associated with preparing specimens for observation linewidth measurements. Hovington P. Rau El. SCANNlNG 1996. Ruble M: Structure of carbon nanotube. Zaluzec NJ. 15119-l 24. Lowney JR: Monte Carlo simulation of scanning electron water vapor or moist air. dynamic charge neutralization of the specimen permitting 7. 16. study of pharmaceuticals [44] and common household and Good review of the procedures required to interpret surface topography in a quantitative manner by employing Monte Carlo simulations. SCANNlNG 1996. Edited by Bailey GW. In Microscopy and Microanalysis Condusions 7996. Melikhov IV. 16. Edited by Bailey GW. typically saturated 6. Hovington P: Energy-filtered backscattered . SEM to materials characterization has been through the 4. McComb DW. Saparin GV. torr (2. SCANNING 1995. Ion production in the gas results in for the use of the SEM as a metrological tool. even be used to deposit metal on the specimen surface The combination of a selected incident energy and a selected imaging en- ergy provides depth-resolved imaging. Saparin GV: A study of the kinetics of SEM (NSEM). San Francisco: San Francisco Press Inc. Corbett JM. Czepkowski T.17:371- 376.165:275-262. Bailey GW. SCANNfNG 1996. emission SEM. SCANNING 1996. Yang W. Dimlich R. Gauvin R. The determination of angular-energy distributions of electrons SEM as a tool for materials characterization thus becomes backscattered by bulk gold and silicon samples. image processing. SCANNING 1995. examination in this way for example. Most importantly the ESEM in electron-solid interactions. Joy DC: Characterization of Schottky depletion zone using EBIC have been highlighted as: imaging. 155:292-302. or other.39’. 16433-447. Thus. Martinez JP. Ding Z-L.. 17:377-307. Corbett JM. based nanocomposites. Scanning electron microscopy for materials characterization Joy 467 and if it can made fully quantitative. Joy DC: Monte Carlo Simulation for Microscopy and poorly conducting materials to be successfully imaged at Microanalysis. for the fabrication of connector lines [46”] or to form 13. Michael JR. images of 10 nm NbC and AIN precipitates in steels computed by Monte Carlo simulations. Obyden SK. the potential scope of this 12. around the specimen has been relaxed so that the 5. Bozhevolnov VE. modeling techniques has resulted in a significant enhancement in 15. 16:556-562. Dorozhkin SV: Procsss of epitaxial crystal growth for C&O. San of special interest l * of outstanding interest Francisco: San Francisco Press Inc. 14. In these instruments the vacuum condition topochemical reactions by SEM. In Microscopy and Microanalysis 1996. 9.300Pa). Michael JR. Michael JR. 15:92-l 14. 15261-291. for analysis of space solar cells.40) as well as producing novel 6. 1995. Redlich P. Lcellent demonstration of the power of the EBIC technique in the SEM for . San Francisco: San Francisco Press Inc. Innovative approach to three-dimensional reconstruction of both chemical of microcharacterization continues to increase the SEM and morphological data remains fully capable of meeting these challenges. data acquisition. then it may be a 3. 1996:146- While the basic capabilities of the SEM have remained 150. electron energy analyser for use in scanning electron The interaction of the electron beam with the gas can microscopy. Joy DC. The presence of a gas. Corbett JM. J Mater Sci 1996. Nikolaev AL. Zatuzec NJ. Davidson DL: Electron channeling patterns 2. SCANNlNG from materials. 17 Drouin D. In Microscopy and Microanalysis 7996. lvannikov PV: A nondestructive method . Weathetfy GC. Sic-reinforced Mg casting alloys. Robinson VNE: An annular toroidal backscattered machine for real materials characterization is considerable. the imaging mechanisms and on the types of sample that A definitive statement of the computational and practical techniques required can be examined. Slowko W: Some limitations of surface profile reconstruction in SEM. has significant effects on both . strategies and the use of Monte Carlo. while the complexity of the task 1996. microscope signals for lithographic metrology. the in situ observation 10. Corbett JM. on conventional high vacuum has been replaced by a gaseous a surface of dissolving fluorapatfte crystals studied by SEM. 17:337-340. topography on electron backscattering. l&291-301. high beam energies (38*.he high resolution surface images of an SEM provide complementary data the characterization of complex three-dimensional device structures. Bailey GW. the combination of innovative operating Detailed calculations which support the principle of depth-resolved imaging discussed in reference 1131. Dimlich R. 53:RBl -R102. J Appf Phys 1962. to structural infonnation obtained from a TEM. In Microscopy and Microanalysis 7996. in conventional high vacuum SEMs. New York: Oxford University Press.. in the gaseous microscope. San Francisco: San Francisco Press Inc. 19. J Microsc 1997. SCANNlNG 1995. Newbury DE. in turn a new tool for the fabrication of still more complex materials.

Legros M. Hoyberg K: ESEM of personal and household products. Michael JR. 40.468 Characterization techniques 20. Perovic DD. SCANNlNG 1996. microanalysis. inalysis of the behavior of the emitted secondary electron signal as it is af- rotations using EBSP. Edited by recovery and recrystallization from orientation imaging Bailey GW. Michael JR. Proc W/E 1996. Donald AM. 66:117-l 31. Krause SJ: Low voltage scanning tion of consumer products. 38. . and frost In Microscopy and 47. Gilpin C: Applications of the ESEM to the 30. Joy DC. Festag R. Jennings HM: The role of the ESEM in the . Bewlav BP: Orientation imaaina of a Nb-Ti-Si Demonstration of the power of the ESEM to study real world problems. Brown GM. in Microscopy and Microanalysis 7996. to observe icicles.. or poorly conducting. Butler JH.. 1996:836-837. 27:265-280. SCANNlNG 1996. Appl Pbys Left 1996. 1996. Corbett JM.. X-ray Spectrometry 1996. resolution. . rime. Pirttiaho L. Joy DC. analysis. 62:237-242. Wunderlich B.. Beeman J. materials. Simkin BA.‘Dimlich R. Kenik EA: Spatial resolution of EBSP diffraction in a FEG-SEM. Francisco: San Francisco Press Inc. Microanalysis 1’996. versus environmental electron beam deposition. gas of the ESEM. . Silver E. Wilson AR: Monte Carlo and finite element calculations of Michael JR. Edited imen chamber makes it possible to form satisfactory images from the bottom by Bailey GW. Folch A. Dimlich R. In Microscopy and Microanalysis 1996. Edited by Bailey GW. 36:1781-l 790. SCANNlNG 1996. SCANNING 1996 18~474-483. provided that conditions are properly optimized. 27. In Microscopy and Microanalysis 18:522-528. conducting. San Francisco: San Francisco Press Inc. . Edited by Francisco: San Francisco Press Inc. 2809:155-l 65. deformation and resiudal strain can be observed and measured using the EBSP technique. idited by Bailey GW. directionally solidified in-situ composite. Edited by Bailey GW. 45.. Organometallic gases deposit metal films on to a substrate under electron beam impact in the SEM. Zaluzec NJ. Joy DC. 1996:344-345. San 41. vacuum SEM. SCANNlNG 1996. San Francisco: San Francisco Press Inc. polymer blends using LVSEM. X-ray production at interfaces in bulk materials. 34. An important new analytical rareful analysis of the errors which set a limit to orientation analysis using tool in the SEM. 21. Francisco Press Inc. Watanabe T: SEM-ECP analysis of grain-boundary character Beautiful application of the SEM to the study of the fragile and complex distribution in oolvcrvstalline materials. electron microscopy of polymers. 192. Klimkiewicz M: Application of ESEM to micro- Microanalysis 7996. Zaluzec NJ. A technical tour de force. 181:23-36. X-ray Spectrometry 1996. 27:247-265. Joy CS: Low voltage scanning electron microscopy. ice fabric. . Houghton DC: Mapping electrically active Important experimental determination of the actual spatial resolution of EBSP . Randle V: Grain boundary characterization in %e conversion of second& electrons to ions in the gas of the ESEM spec- . Meredith P. 1996:350-351. I Microsc 1996. Hailer E: High Francisco Press Inc. 1’996:348-350. the ESEM gaseous detector. Alexandratos SD. San Francisco: San Francisco Press Inc. A new tool for lithography and localized chemistry. Michael JR. Seco M: High vacuum 32. 1996:140-l 42. Zaluzec NJ. The use of the ESEM to build three-dimensional nano-scaled structures us- 1996:146-l 47. Corbett JM. environmental SEM. Dimlich R. . SCANNlNG 1996. . Edited by Bailey GW. Wright SI. Esteve J. particles. 39. 1996:352-354.. 18:515-521. San microscopy. In Microscopy and Microanalysis 1996. Paul BK. Zaluzec NJ. Edited by Bailey GW. The development of a new type of energy dispersive X-ray detector offering Corbett JM. Donald AM: Study of ‘wet’ polymer latex in the . Good real world application of ESEM technology. 98:405-409. EBSP patterns. Meredith P. 24. broad band microcalorimeters for X-ray 22. Madden N. Michael JR. Field DP: Determining deformation. Tejada J. 33. In Microscoov and microstructure of snow. Crimp MA: Dislocation detection depth A demonstration that the spatial resolution limit to microanalysis set by measurements in silicon using electron channeling contrast electron-solid interactions does not prevent the observation of small features In Microscopy and Microanalysis 7996. Dimlich R. Zaluzec NJ. 37. Application of the ESEM to the classic problem of the behavior of cement A definitive analysis of the problems of using electron beams to study non- and related materials. Zaluzec NJ. San Francisco: San an order of magnitude better performance than current detectors. 500. Wilkinson AJ: Measurement of elastic strains and small lattice . 18:490-496. investigation of cement-based materials. mechanical fabrication. 44. Butler JH: A new method for the characterization of analysis of pharmaceutical formulations. Dimlich R. 36. 25. Servat J. J Microsc 1996. l&467-473. 28. Newbury DE: Imaging deep holes in structures in the ESEM. Edited by Bailey GW. . 29. Solid State Commun 1996. Michael JR. Interesting demonstration df the versatility of the ESEM for the characteriza- 31. Micron 1996. San of holes several millimeters in depth. Corbett JM. Cazaux J: Electron probe microanalysis of insulating materials. 26:l 15-l 22. Rango A. Corbett Ji. Corbett JM. D’Emmanuele A. Dingley DJ. fected by Auger emissions. protective oxide of an Ni-Fe alloy. In Microscopy and Microanalysis 7996. 42. consistent with those used in device fabrication. Corbett JM. Dimlich R. Neubauer CM. 18:497- techniques. Wergin WP. &ood analysis of the complex interactions encountered by electrons in the Good illustration of the power of the orientation imaging technique for ma. Bradley GF. San Francisco: San 35. Polymer 1995. Sutcliff JA. Michael JR. J Vat Sci Separation and characterization of single-chain polymer Techno/ 1996. San Francisco: San Francisco Press Inc. 46. 181:72-61. Ultramicrosc 1996. Joy DC: Modeling the electron-gas interaction in low- 26.. 23. Dimlich R. Blakely J: ESEM observations of H.S attack on the Quantitative analysis of grain boundary quality and character using EBSP . ing selective deposition and radiation techniques. Lassen NCK: The relative precision of crystal orientations Secondary electron signals can reveal the presence of dopants at levels measured from EBSP. Thield B: Electron-gas interactions in Michael JR. Turan R. ice and frost. Ultramicrosc 1996:354-356. 43. Michael JR. In Microscopy and Microanalysis 7996. 69:1593-l 595.. Zaluzec NJ. austenitic steel. Bailey GW. Zaluzec NJ. dopant profiles by field emission SEM. Francisco: San Francisco Press Inc. Schroeder S L M: Towards a ‘universal curve’ for total electron- yield XAS. 14:2609-2614. 19:109-l 13. Corbett JM. terials characterization. Corbett JM. Caul MV. Dimlich R. 7996. Zaluzec NJ. Erbe EF: Use of low temperature SEM . 1996:l QO. Dimlich R. SCANNING 1996. Cook K: . In conjunction with reference [36’*] this provides Demonstrates that lattice rotations as small as those associated with elastic a prototype new technique for microanalysis in the SEM.