Nano Science

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Images are location specific mapping of the surface characteristics: reflection, absorption, transmission etc

We can map the spectroscopic information also!

Bamboo vascular bundles. (Left to right): light micrograph with safranin/alcian blue stain; SEM at similar scale; TEM of fibre cells (a few of the pink cells from the light micrograph), note the higher magnification and resolution: lamellation of the cell wall is clear

Morphology The shape and size of the particles making up the object; direct relation between these structures and materials properties (ductility, strength, reactivity...etc.). Topography The surface features of an object or "how it looks" its texture; direct relation between these features and materials properties (hardness, reflectivity...etc.).

Magnification is how much bigger we can make something appear. Resolution is how much better we can distinguish two closely spaced points.

A lower limit on resolution is imposed by the fact that we view specimens in an optical microscope using waves. We cannot distinguish details finer than the wavelength of these waves because light diffracts and interferes with itself when moving around very small objects.

Magnification: Ratio of length of the scan line on the monitor or recording device to length of the scan line on the specimen. For Electron Microscopes/Force Microscopes the magnification is independent of the lenses and is changed by changing the scan size. Picture element: The region on the specimen from which information is transferred to a pixel of the image. Hence picture element refers to a position on the specimen, and pixel refers to the corresponding portion of the recorder image. And the image appears to be in focus if the sampling volume of the given signal is smaller than/equal to the picture element size at the given magnification. The above also defines the resolution of SEM. The sampling volume should be smaller than the feature which needs to be resolved.

Depth of field: This the range of distance along the optical axis in which the specimen can move without the image apppearing to lose sharpness. SEM has more than 300 times the depth of field of a light microscope.

In SEM resolution of 1nm is achievable with field emission electron gun. In SEM the magnification varies from 3X to 150,000X Lenses in SEM, unlike the optical microscope are not part of the image formation system, but are used to demagnify and focus the electron beam onto the sample.

Electron microscopy allows one to visualize objects that are as small as 1 nm. Here the specimen is not illuminated with light but bombarded by electrons as a source for image formation.

Energy of an electron Beam: Kinetic energy: 1eV - 1,000 keV The electron beam can be focused with high accuracy, this leads to incident wave having various forms. 1. Raster beam with synchronized signal acquisition. 2. Plane Wave imaging.

Elastic Scattering: imaging measurements Inelastic Scattering: spectroscopy measurements, chemical mapping.

The strength of electron techniques lies in the fact that the electrons can be focused using electromagnetic lenses. This allows one to obtain high resolution topographic images as well as diffraction information from specific regions in space as small as 1nm.

Signal Generation in SEM Probe: focused beam of electrons accelerated of moderately high energy (few hundred eV to 40 keV) and positioned on to the sample by electromagnetic fields (0.4 nm to 5 nm ). The optical column of the SEM is used to ensure that the beam consists of electrons of similar energy and trajectory When the beam impinges on a point on the surface it interacts via a variety of mechanisms which could be either elastic or inelastic. Elastic interactions: change in the trajectory of the beam electrons w/o loss of energy Inelastic interactions: energy is transferred from the beam to the sample. Each electron normally undergoes multiple interactions, so inelastic and elastic interactions result in the beam electrons spreading out into the material and losing energy.

Interaction Volume

The simultaneous loss of energy and change in trajectory produces an interaction volume within the bulk which extends from less than 100 nm to around 5 m into the surface. The size of the interaction volume depends on the electron's landing energy, angle of incidence, the atomic number of the specimen and the specimen's density.

The signals resulting from various interactions will have different depths within the sample from which they can escape due to their unique physical properties and energies. This gives rise to sampling volume, from which a given signal escapes the solid and is a fraction of the interaction volume. The spatial resolution is determined by the sampling volume and the signal distribution within it.

Image Formation:
The image is formed in an SEM by raster-scanning an electron beam across a sample and collecting some signal from the beam-sample interaction, which is used to control the intensity of the spot on a television monitor which is scanning in synchronization with the beam on the sample. The picture produced is often a lot like might be envisioned if the operator were standing above the sample and looking down on it with highly magnified vision. Because the probe used for imaging is an electron beam, some interesting contrast mechanisms (and signals) can be produced. The appearance of the image is usually as though the sample were ''illuminated'' by the detector being used to form the image, up to the point of ''shadows'' and the like

Magnification: Ratio of length of the scan line on the monitor or recording device to length of the scan line on the specimen. For Electron Microscopes/Force Microscopes the magnification is independent of the lenses and is changed by changing the scan size. Picture element: The region on the specimen from which information is transferred to a pixel of the image. Hence picture element refers to a position on the specimen, and pixel refers to the corresponding portion of the recorder image. And the image appears to be in focus if the sampling volume of the given signal is smaller than/equal to the picture element size at the given magnification. The above also defines the resolution of SEM. The sampling volume should be smaller than the feature which needs to be resolved.

SEM provides information relating to topographical features, morphology, phase distribution, compositional differences, crystal structure, crystal orientation and the presence and location of electrical defects. By adding an X-ray or electron spectrometer SEM can also determine the elemental composition of micro volumes. And analysis of electron diffraction pattern allows for the determination of phase distribution. Strength of SEM is its inherent versatility due to: The multiple signals generated Simple image formation process Wide magnification range Excellent depth of field

Secondary Electrons (SE): SEs are low energy (2 to 5 eV) electrons ejected from the
outer shell of a sample atom due to the energetic passage of beam electrons. Though the typical energies of SEs are on the order of a few eV, a somewhat arbitrary convention regards anything less that 50eV emitted from a sample as a SE. SEs are emitted throughout the interaction volume, but due to their low energy they don't travel far in the sample before being re-captured (5-50nm). It is for this reason that SEs are thought of as a surface-sensitive signal. The emission of SEs occurs throughout the intersection of the surface with the interaction volume, but as the beam electron flux density is the highest where the beam first enters the sample, the highest concentration of SEs also comes from this region. This fraction of the SE signal is what allows most high resolution SEM imaging. SE intensity is a function of the surface orientation wrt the beam and SE detectors and hence produces an image of the surface morphology. Other factors influencing the SE intensity are chemical bonding, charging effects and Back Scattered electron intensity.

This micrograph shows a secondary electron image of the cadmium telluride surface of a polycrystalline CdS/CdTe cell.

Mosquito Wing

Laser weld of 0.010 inch NiTi Alloy wire

Back Scattered Electrons (BSE): Back Scattered Electrons (BSEs) are primary beam electrons that have have undergone one or more elastic (billiard ball-type) collisions within the sample and eventually have bounced around enough to re-emerge from the surface they came in.

BSE makeup the majority of electrons emitted from the sample at higher beam energies and their average energies are much higher than those of SEs.
The energy spread of BSEs goes from E0, the beam energy, all the way down to zero; typically this energy distribution is peaked somewhere between 0.4E0 and 0.95E0 or so, with the peak being sharper and more pronounced at higher atomic number. The total BSE yield (total fraction of beam electrons that backscatter) tends to increase monotonically with the atomic number, Z and flattening out at higher Z.

Hence BSE is an effective signal for generating compositional images, in which higher Z phases appear brighter than lower Z phases.
For a flat sample surface that is normal to the beam, the BSE distribution is peaked in the normal direction, such that the highest BSE yield comes straight back up. For surfaces at small angles away from the normal, this distribution still more or less holds. In addition to the BSE dependence on Z, surface orientation also affects the total BSE yield, as well as the preferred direction of the BSEs.

Backscattered electron image of a volcanic rock

the brightest areas are magnetite, a high Z Fe oxide. The next brightest areas are pyroxene crystals that contain Fe, but also lower Z elements, such as Si, the medium grey areas are volcanic glass, and the darkest grey areas are feldspar.

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