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Imageintensities above (or below) this level are taken to correspond to areas ofthe particle being measured. This is demonstrated in Figure 7.8b, wherea threshold was applied to identify the particles. Simple analysis allows thearea and radius of the particle to be determined. In the case of non-sphericalparticles the diameter is determined by the fitting of an ellipsoid. A histogramof the sizes can then be easily determined (Figure 7.8c).Although the threshold method described above is a simple, well-definedand recognised method it does suffer from some significant drawbacks. Thefirst is setting the threshold level, which is difficult for poorly contrastingparticles (such as small polymer particles or inhomogeneous particles (seeFigure 7.9)).
The second, more important, drawback occurs when analysingagglomerated particles. With no significant intensity difference between theparticles a simple threshold is insufficient to distinguish between the particles and hence accurately determine size. It is usually recommended to usea watershed method.7.6 Other particle beam microscopy techniquesIn order to get high-resolution images from any scanning beam microscope one must be able to produce a sufficiently small probe, haveOther particle beam microscopy techniquesFIGURE 7.8 (a) TEM image of nominal 30 nm diameter gold nanoparticles; (b) using threshold to identify theindividual particles; (c) histogram of the measured diameters.a small interaction volume in the substrate and have an abundance ofinformation-rich particles to create the image.
A typical SEM meets allof these requirements, but other particles can be used as well. Recently,a focused ion beam (FIB) [63] has become more and more popular. Theconcept of FIB is similar to that of SEM; however, the electrons arereplaced by ions of much larger masses. As a consequence they can in205206C H A P T ER 7 : Scanning probe and particle beam microscopyFIGURE 7.9 TEM image of 150-nm-diameter latex particles.
This image highlights thedrawback to TEM size measurement using TEM or SEM. The first is that a white ‘halo’surrounds the particle. Should the halo area be included in the size measurement? If sothere will be a difficulty in determining the threshold level. The second is the particles areaggregated, again making sizing difficult.general induce damage to a specimen by sputtering. However, for eachincoming ion two to eight secondary electrons are generated. Thisabundance of secondary electrons allows for very-high-contrast imaging.In addition to secondary electrons, backscattered ions are also availablefor imaging.
These ions are not as abundant as secondary electrons, butdo provide unique contrast mechanisms that allow quantitativediscrimination between materials with sub-micrometre spatial resolution.An electron beam has a relatively large excitation volume in the substrate.This limits the resolution of an SEM regardless of the probe size.
A heliumion beam does not suffer from this effect, as the excitation volume is muchsmaller than that of the SEM. SEMs are typically run at or near theirsecondary electron unity crossover point to minimize charging of the sample.This implies that for each incoming electron, one secondary electron is madeavailable for imaging.
The situation with the helium ion beam is much morefavourable.The helium ion microscope [64] has several unique properties that, whencombined, allow for higher-resolution imaging than that available today withconventional SEMs. In addition to better resolution, the helium ion microscope and the FIB also provide unique contrast mechanisms in bothsecondary electron mode and backscattered modes that enable materialdiscrimination and identification.References7.7 References[1] Binnig G, Rohrer H, Gerber Ch, Weibel E 1982 Surface studies by scanningtunneling microscopy Phys. Rev.
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