Special Topics in Scanning Electron Microscopy

Achieving High Resolution at High Beam Energy High-Resolution Imaging at Low Voltage Contrast Formation in Low Voltage Images Radiation Damage at Low Beam Energies SEM Observation of Non-Conducting Samples at Low Voltage The Effects of the Choice of Electron Energy STEM-in-SEM: High Resolution for the Special Case of Thin Specimens Variable-Pressure and Environmental SEM The Effect of the Gas on Charging Imaging in the VPSEM and ESEM Gaseous SE Detector (GSED)

Achieving High Resolution at High Beam Energy

When low-atomic-number targets, e.g., the typical matrix of biological or polymer samples, are to be imaged, the low SE yield typical of such compositions creates limitations to high-resolution imaging that arise from problems of poor signal-to-noise ratio. The signal-to-noise ratio can be improved by the application of an ultra thin (3-5 nm) metal coating. Such layers are formed from individual metal crystals 2-3 nm in size. Because this size is comparable with the escape depth for secondary electrons, such layers exhibit a very high secondary electron yield. Au, Au-Pd, and W are the preferred choices for such coatings because they can readily be deposited in a low-cost sputter coater. For magnifications lower than about 100,000x, the grains are sufficiently fine to be effectively invisible, but at higher magnifications the individual particles are discernible and so may produce artifacts in the image or even mask real surface details.

High-Resolution Imaging at Low Voltage

It has been known for quite some time that using a low accelerating voltage on an SEM would provide good results. The main problem has been creating a bright enough source so that the resulting specimen signal would be strong enough for detection. Tungsten filaments, and to some extent LaB6 sources, have not been able to produce adequate signals. The Field Emission SEM, though, provided the means necessary to achieve good results at low voltages. Decreasing the accelerating voltage increases the probe diameter (due to the stronger effects of chromatic aberrations) but decreases the interaction volume. The decrease in volume is much larger than the increase in spot size, so the overall effect is higher resolution. For example, decreasing the voltage from 30 keV to 1 keV increases the spot size by a factor of 5, but decreases the interaction volume by more than 2 orders of magnitude. In this case, the FWHM dimensions of the SE2 and BSE2 components begin to approach that for SE1. This is a desirable situation because now all of the emitted electrons carry information at high spatial resolution. There is no need to separate the weak SE1 signal from the strong but low-resolution SE2 background. Consequently, the imaging process is more efficient and the contrast is higher. This also means that BSE imaging with a resolution similar to that of SE images is possible. Since the interaction volume at low voltage is on the same scale as small surface features, these items are much more noticeable than they would be at higher voltages.

Low Voltage Scanning Electron Microscopy

Low voltage scanning electron microscopy (LVSEM) is the application of the SEM at beam energies below 5keV. The fall in electron beam range compared to its magnitude at higher energies leads to significant changes in the beam interaction volume and in the secondary and backscattered electron yields. The topographic and beam penetration contrast effects which dominate images at high energies are replaced by detector collection efficiency contrast effects giving images which are less three dimensional but which contain more detailed information on the surface morphology and, in some circumstances, the surface chemistry. The high stopping power of electrons at low energy can result in enhanced radiation damage. However, because of the small electron range, such damage is confined to a thin, near-surface region of the specimen.

 One disadvantage is that X-ray analysis can only give the K lines for the very lightest elements and only L & M lines for heavier elements, due to the lower energy of the electrons. Contamination is a serious limitation to low-voltage microcopy because the range of the signals is so short that the contamination may dominate the image as it builds up. The rate of contamination build-up can be reduced by minimizing the electron dose to the specimen with the following procedures: Avoiding high magnification except when essential. Focusing and stigmatizing the image in an area remote from the one that is to be used to record an image. Never using spot or reduced-area raster modes.

Comparison of Interaction Volumes: High Acceleration Voltage vs. Low Acceleration Voltage

The Effects of the Choice of Electron Energy

Reducing the energy of the electrons incident on a solid has a profound effect on the interactions that occur within that material. Stopping power: the rate at which the electron is giving up its energy to the surrounding solid. Fig. 1 shows the variation in the stopping power of an electron traveling through carbon as a function of its energy. As the energy decreases, the stopping power increases from about 1eV/ to a maximum value close to 10eV/ and then falls away again at still lower energies. Electrons in the energy range between about 100eV and a few keV therefore interact much more strongly with the material through which they are traveling than is the case at higher energies. The consequence of this is that the distance that the electron will penetrate will decrease rapidly as the incident energy is reduced. Fig. 2 shows that while there are significant differences in the range at higher energies for the various targets, at the lowest energies all materials have approximately the same range.

Stopping Power Variation as a Function of Energy for Electron Traveling through Carbon

Fig. 1 Typically between 30 and 100eV corresponding to the energy at which the stopping power reaches its maximum value.

The following figure shows the calculated electron ranges as a function of incident energy for four elements.

Fig. 2 It can be seen that the range decreases rapidly with energy falling from a micrometer or more at 10keV to only tens of nanometers for energies below 1keV. Note that while there are significant differences in the range at higher energies for the various targets, at the lowest energies all materials have approximately the same range.

Contrast Formation in Low Voltage Images

Image contrast in the low voltage SEM is in many aspects different from that of the conventional SEM. More of the image information now comes from closer to the surface and so may be affected by the presence of contamination and surface defects. The low voltage image is less sensitive to the surface topography and its form is dependent on the orientation of the detector to the region being observed. Because of the decrease in the size of the interaction volume, all of the SE generated in the sample, whether by incident or backscattered electrons, are capable of carrying high resolution informationgiving a useful improvement in the contrast of such images. Although metal coatings are an essential tool for building contrast in high resolution microscopy, for low voltage microscopy, even the thinnest film obscures the surface to some degree and so coating is to be avoided if possible. If a coating is to be used, it must be chosen carefully since the task of a metal coating is twofold: To form a local ground plane at the surface, eliminating fields from any charge stored within the sample. The additional SE and BSE production at the film reduces the amount of charge retained in the specimen. The ideal coating is a thin film of a material such as Cr or W which has a high SE yield, good conductivity, and a low surface energy to ensure a continuous, structureless film even at nanometer thicknesses.

Radiation Damage at Low Beam Energies

A low energy electron beam actually damages a sample more rapidly than a higher energy beam because the energy deposited per unit volume in the sample is greater. For instance, damage in biological and polymeric materials occurs through the breaking of bonds within the sample, and the energy required for this is only on the order of a few eV, much lower than the energy of any normal incident electron. The reason that radiation damage caused by high beam energies seems more obvious than that caused by low beam energies can be explained by the following facts: At low voltage, the damage is confined to the top few nanometers of the sample, while at energies of 10keV or higher the damage although less in magnitude is spread through a volume a micrometer in radius of more of the sample. Artifacts such as shrinkage are thus much more significant and noticeable at high beam energies than at low energies. Other effects may also contribute. For example, charging at high energies produces electrostatic fields of 106 V/cm or more which are high enough to cause dielectric breakdown, mechanical deformation, and changes in the chemistry of the sample. Even though it is more limited in physical extent, low voltage damage may still have significant effects. For example, in inorganic and dielectric materials, such as the gate oxides used in the semiconductor industry, it is found that while the electrical defects induced throughout the volume of the sample by high energy electrons are readily removed by low temperature annealing, to remove the damage caused by low energy irradiation may require both heating and optical bleaching.

SEM Observation of Non-Conducting Samples at Low Voltage

Charging: A specimen becomes electrically charged when it is receiving more electrons than it is emitting or emitting more than it is receiving. The presence of this charge generates an electric field which may interfere with the collection of secondary electrons, deflect the incident beam, or can even damage the specimen.

is the SE yield, is the BSE yield

Schematic representation of the spatial distribution of SE1 and SE2 electrons at (a) high energy (20keV) and (b) low energy (1keV)

At high beam energies the total electron yield (+) is less than unity, so charge is being injected into the specimen, which therefore acquires a negative charge. Negatively charged regions appear bright in the SE image. This is because the negative charge repels secondary electrons from the surface, decreases the landing energy of the incident beam (so raising the SE yield) and increases the collection field between the sample and the detector (so enhancing the detection efficiency). At low energies the total electron yield (+) may becomes greater than unity, so that charge is being removed from the specimen which then acquires a positive charge (since initially it was electrically neutral). Positively charged areas can recollect their own SE emission, and so they appear dark in the SE image. As a special case, if (+) equals unity then there is a dynamic charge balance and no net charging occurs even though the sample is not conducting. This will clearly be the optimum choice of operating energy in most cases. Because of the rise and subsequent fall of SE production with accelerating voltage, there are two incident beam energies at which this condition might be met, a lower value E1 typically between 50 and 150eV and a higher value E2 which is typically between 0.5 and 3 keV. The fact that E2 is in the few keV range of materials of technological importance such as semiconductors, polymers, and ceramics, has been an important factor in the development of low voltage SEM techniques.

Monte Carlo simulation of the electron trajectories in the specimen with respect to the variation in beam interaction volume with energy plotted at a constant scale of magnification shown below:

This confirms that while scanning microscopy at conventional energies (10-30keV) can observe the bulk of a specimen, operation at low beam voltages restricts the interaction to the near-surface regions of the material.

Fig. 4 Images of a 20nm thick carbon film stretched over a copper grid at (a) 20keV and (b) 1keV. The image shows a 200 thick carbon film stretched over a copper mesh grid obtained at 20keV. The film is almost invisible because the majority of the incident electrons traverse the carbon without producing any interaction. But at 1keV, Fig. (b), all of the electron interaction volume is contained within the thickness of the carbon, and the resultant SE and BSE emissions from the film make it appear solid and opaque.

The strategy of lowering the beam energy to improve the lateral spatial resolution by restricting the range of the beam electrons is useful for surface imaging. As incident beam energy decreases and the BSE2 and SE2 ranges approach the BSE1 and SE1 ranges, the image sampling depth is also greatly restricted. Because we are often dealing with an unknown surface chemistry/structure both in depth and laterally, the best approach may be to consider a systematic imaging study of the material as a function of beam energy. By comparing a series of images to search for changes, surface features such as discontinuous surface layers can often be revealed. When the same area is compared during a beam energy image series, care must be taken not to confuse contamination deposited during the earlier stages of the image series with the true specimen information. Minimum dose microscopy principles should be followed, with specimen exposure only occurring during image collection. Since the low-beam energy images are the most sensitive to prior contamination, these images should be recorded first in a beam energy sequence, finishing with the high-beam-energy images.

STEM-in-SEM: High Resolution for the Special Case of Thin Specimens

When the dimensions of the object of interest approach and then become less than that of the interaction volume, progressively more of the electron scattering occurs from the substrate and progressively less from the object. This situation is frequently encountered in the case of particles. An improvement for the detection and visualization of particles in SEM images is to employ the technique of scanning transmission electron microscopy (STEM) in the SEM. By placing a suitable detector below the specimen on its thin-carbon-film support, as shown in Fig. 5.9, the transmitted electron signal can be collected and used to form an image. The STEM detector can be constructed from a scintillator-light pipe or solid state detector. Alternatively, a simple, inexpensive STEM detector (so called poor mans STEM detector), illustrated schematically in Fig. 5.10, can be made by placing a highatomic-number scattering surface below the specimen and tilted so that the transmitted electrons are scattered toward the conventional E-T detector in the specimen chamber.

In Fig. 5.11, the images show a similar array of particles and are complementary, in that bright areas in the conventional E-T image, which show areas of strong scattering, appear dark in the STEM image because these scattered electrons are lost to the transmitted signal. The big difference is that the conventional E-T image in (a) is noisier than the STEM-in-SEM mode image.

For very fine particles, the poor mans STEM-in-SEM detector can produce some outstanding images when operated in conjunction with the through the lens (TTL) detector. Fig. 5.12a shows the SEM TTL and Fig. 5.12b shows the STEM in SEM of fine particles attached to lacey carbon film with a beam energy of 25 keV. The internal structure as well as the surface structure can be simultaneously observed.

Variable-Pressure and Environmental SEM Variable-pressure SEM (VPSEM) or environmental SEM (ESEM) is the instrument that can be operated while its specimen chamber contains a gas or a vapor at a pressure in the range of approximately 200 to 2500Pa (2-20 torr). In this case, the SEM may not offer a secondary electron detector for use when there is gas in the chamber, relying only on BSE detection for imaging. Typically these instruments use a relatively modest electron-optical system and a basic thermionic gun because the performance of the machine is ultimately limited by the electron-gas interaction. VPSEMs and ESEMs are also usually designed to operate optimally in the energy range 10-30keV rather than at the lower energy of 1-5 keV favored by conventional high-vacuum machines.

The Vacuum System of VPSEMs and ESEMs

The difference between the vacuum system of conventional SEM and VPSEM and ESEM is that a pressure-limiting aperture (PLA) or differential aperture is usually positioned at the bottom of the objective lens so that the distance that electrons have to travel through the gas to reach the sample is no more than the working distance. Some instruments, however, mount this aperture on an extension tube beneath the lens so that the gas path length can be much smaller than the working distance of the lens. In either case, the aperture is typically a few hundred micrometers in diameter, a figure which is sufficiently small to allow a pressure differential of 100 to 1000 times to be maintained between the specimen chamber and the column. The isolation of the column from the specimen chamber can be improved by reducing the diameter of the PLA, but this leads to a problem when the instrument is used for low-magnification operation because the scanned rays then interact the edge of the aperture, causing vignetting of the image. Depending on the working distance, the lowest useful magnification is therefore typically 50x or more, unless the instrument is specially modified.

The Effect of the Gas on Charging

The presence of gas in the specimen chamber of the ESEM or VPSEM can overcome the problem of charging, making it possible to observe all materials including insulating materials. This is because the interactions between electrons and the gas result in the production of ions, which can strip off an outer shell electron, producing a positively charged nucleus and an electron, or by breaking up a molecule to form two charged components. In either case, the interaction results in the production of particles with both positive and negative charges. The positively charged ions will drift to negatively charged areas of the specimen and negative ions will drift toward positively charged areas. If sufficient ions are produced, the charging of the specimen can be neutralized by the flood of positive ions.

Imaging in the VPSEM and ESEM

In VPSEM and ESEM, the imaging formation is based on the collection of backscattered electron signals. The secondary electron signal is not available because the SE only travel a very short distance from the surface of the sample before they interact with and ionize a gas molecule and so it is difficult to collect them. Moreover, the conventional E-T detector used for SE collection relies on a high (+10 kV) bias voltage applied to the scintillator to accelerate the SE to sufficient kinetic energy to stimulate light emission from the scintillator. In the high-gas pressure environment of the specimen chamber, where a potential of more than just a few hundred volts would cause the gas to ionize and to arc to the detector, the E-T detector is thus not a viable option. Because modern BSE detectors are very efficient, the quality of the BSE image is in every way comparable with the corresponding SE image.

Gaseous SE Detector (GSED)

Comparison of the Image Made by BES, SE, and GSED

FESEM Images of CdS Nanowires Show the Effect of the Incident Electron Beam Energy (a) (a) (b)

1 m 100 nm Image obtained at 1keV

100 nm Image obtained at 20keV

 In addition, the probability of an SE, produced at some depth z beneath the surface, escaping from the specimen is proportional to exp(-z/) where is an escape depth and is typically 3 to 6 nm for most elements. With further decrease or increase of the incident energy around the optimum incident energy range (1keV for silver), the yield of SE begins to fall again because of the decrease in the stopping power of the incident electron and the increase in the escape depth, respectively. In general, the yield of SE reaches a maximum value of the order of unity or greater when the electron range RB is about 2.5 . Where is an escape depth.

 The variation in the backscattering yield for a low, a medium, and a high atomic number specimen is shown on the next page. Although the backscattering yield is almost constant for energies above about 10keV, it may show significant variations between 1 and 10 keV. The yield rises for a light element such as carbon or silicon, stays approximately constant for a transitional element, such as copper, and falls for heavier elements such as gold. At energies around 1 keV the effective backscattering coefficients of all materials are thus approximately in the range of 0.2 to 0.3. For energies below 1keV, the backscattering yields are not well-known, but significant variations with energy are very likely.

The backscattering yield coefficient vs. low incident energy

The Relationships Between SE and BSE Images for High Incident Energy and Low Incident Energy
The usual relationships between SE and BSE images may be reversed for low voltage operation. At typical SEM energies (2030keV) the contrast information in the SE image comes from a region about 4 beneath the surface, i.e., about 15 20 nm in extent. By comparison, the average BSE electron is emerging from a depth of about 0.2 RB, i.e., about 0.25m or more. The SE, therefore, carry surface information while the BSE can be said to image the bulk of the sample. At low voltages, however, while the depth of information for the SE is still 1520nm because the energy and distribution of the SE does not change with incident beam energy, the corresponding depth for the backscattered signal of 0.2RB may now only be 3 to 5nm because of the fall in electron range. Thus at low energies SE are emitted from the whole interaction volume while the BSE only emit from a thin surface region and it is the SE which perform the task of bulk imaging.

Effect of Penetration Range of the Incident Electron to the SE Image Contrast

Another significant effect that contributes to SE image contrast is the penetration of the beam into the sample. At high beam energies this occurs over a scale of many micrometers and features raised above the general surrounding surface are filled by the incident beam irradiation, leading to enhanced SE emission from all the free surfaces of the feature and enhancing the characteristic three-dimensional appearance associated with SEM images. At low energies the beam penetration is much smaller than the typical dimensions of a feature and in this case only the edges remain bright. Also, at low voltages, all faces of the sample emit about the same number of SE, and the beam penetration is small so that raised features no longer have enhanced SE emission, thus only the detector contrast efficiency effect remains. Topography is now only visible in as much as the local surface is normal to the detector: the image in general is flat.