Materials Characterization

NANO 52 Foothill College Spring 2007

Magnification and Resolution

By using more lenses microscopes can magnify by a larger amount, but this doesn't always mean that more detail can be seen. The amount of detail depends on the resolving power of a microscope, which is the smallest separation at which two separate objects can be distinguished (or resolved).

Magnification is how much bigger a sample appears to be under the microscope than it is in real life.
Overall magnification = Objective lens x Eyepiece lens

Resolution is the ability to distinguish between two points on an image i.e. the amount of detail

Magnification and Resolution

The resolution of an image is limited by the wavelength of radiation used to view the sample. This is because when objects in the specimen are much smaller than the wavelength of the radiation being used, they do not interrupt the waves, and so are not detected. The wavelength of light is much larger than the wavelength of electrons, so the resolution of the light microscope is a lot lower. Using a microscope with a more powerful magnification will not increase this resolution any further. It will increase the size of the image, but objects closer than 200nm will still only be seen as one point.

Optical Microscopy/Light Microscopy

Uses visible light and a series of glass lenses to magnify an object

Light Microscopy Basics http://virtual.itg.uiuc.edu/training/LM_tutorial/

Electron Microscopy
An electron microscope can magnify 100 to 1000 times more than a visible-light microscope. This uses a beam of electrons, rather than electromagnetic radiation, to "illuminate" the specimen. This may seem strange, but electrons behave like waves and can easily be produced (using a hot wire), focused (using electromagnets) and detected (using a phosphor screen or photographic film). A beam of electrons has an effective wavelength of less than 1 nm. Electrons accelerated by voltages on the order of 10,000 Volts (10 kV) have wavelengths on the order of 0.004 nm. Theoretically this would be the resolution, but in actuality, due to aberrations in the magnetic lenses, the resolution is more like 0.1 to 0.5 nm.

Scanning Electron Microscope

The scanning electron microscope (SEM) scans a fine beam of electrons onto a specimen and collects the electrons scattered by the surface. Electrons are reflected off the surface of the specimen as it has been previously coated conductive material. It is these reflected electron beams that are focused on the fluorescent screen in order to make up the image. Larger, thicker structures can thus be seen under the SEM as the electrons do not have to pass through the sample in order to form the image. This gives excellent 3-dimensional images of surfaces. The resolution of the SEM is lower than that of the TEM.

SEM
A beam of electrons is produced at the top of the microscope by an electron gun. The electron beam follows a vertical path through the microscope, which is held within a vacuum.

The beam travels through electromagnetic fields and lenses, which focus the beam down toward the sample. Once the beam hits the sample, electrons and X-rays are ejected from the sample.

Detectors collect these X-rays, backscattered electrons, and secondary electrons and convert them into a signal that is sent to a screen similar to a television screen. This produces the final image.

Electron Microscopy Basics http://virtual.itg.uiuc.edu/training/EM_tutorial/ Preparing a Sample for the Scanning Electron Microscope (SEM) http://virtual.itg.uiuc.edu/training/esem-prep.mov

Transmission Electron Microscope

The transmission electron microscope (TEM) works much like a light microscope, transmitting a beam of electrons through a thin specimen and then focusing the electrons to form an image on a screen or on film.

Pass a beam of electrons through the specimen. The electrons that pass through the specimen are detected on a fluorescent screen on which the image is displayed.
Thin sections of specimen are needed for transmission electron microscopy as the electrons have to pass through the specimen for the image to be produced. This is the most common form of electron microscope and has the best resolution.

Comparison of the light and electron microscope

Light Microscope Cheap to purchase Cheap to operate. Small and portable. Simple and easy sample preparation. Material rarely distorted by preparation. Vacuum is not required. Natural color of sample maintained. Magnifies objects only up to 2000 times Specimens can be living or dead Electron Microscope Expensive to buy Expensive to produce electron beam. Large and requires special rooms. Lengthy and complex sample prep. Preparation distorts material. Vacuum is required. All images in black and white. Magnifies over 500 000 times. Specimens are dead, as they must be fixed in plastic and viewed in a vacuum The electron beam can damage specimens and they must be stained with an electrondense chemical (usually heavy metals like osmium, lead or gold).

Stains are often needed to make the cells visible

Scanning Tunneling Microscope

Developed in the 1980s contains a tiny probe, whose tip may be only a few atoms wide. The tip is moved across the sample surface. The tip, as it scans, remains very close to the surface of the specimen, about 1nm above it.

A small voltage is applied between the probe and the surface causes electrons to leave the surface and pass through the vacuum to the probe (tunneling). The tunneling current is very sensitive to the gap width, so a feedback mechanism can be used to raise and lower the probe to maintain a constant electron current.
The probes vertical motion, following the surface of the specimen, is then plotted as a function of position, producing a three dimensional image of the surface. Surface features as fine as the size of an atom can be resolved (0.1nm laterally and 0.01nm vertically. The topographic image of a surface actually represents the distribution of electron charge.

Scanning Probe/Atomic Force Microscopy Basics http://virtual.itg.uiuc.edu/training/AFM_tutorial/ http://virtual.itg.uiuc.edu/training/AFM-prep-large.mov

Atomic Force Microscope (AFM)

Developed in the 1980s.
Very similar to the STM, but can be used on a wider range of sample materials.

Instead of detecting an electric current, the AFM measures the force between a cantilevered tip and the sample, a force which depends strongly on the tip sample separation at each point.
The tip scans the surface of the sample, just like the STM.

Focused Ion Beam (FIB)

The FIB instrument consists in an ion gun and electrostatic lenses, generally mounted on a scanning electron microscope. The secondary electrons generated by the primary ion beam give an image (ion image), which is used to control the machining process. The milling can also be followed in real time by the scanning electron image (electron image). FIB typically operates with gallium ions and at an accelerating voltage of 1-30 keV. The ion probe size is around 10 nm in diameter.

A metal evaporation source (Pt, W, etc) is used to coat the sample surface to protect it under a metal film.
An internal or external micromanipulator is required to extract the slice.

The system contains both a focused Ga+ ion beam and a field emission scanning electron column. The ion column can be used for selective removal of material by ion beam milling. In addition, the ion beam can be used for ion-enhanced imaging of fine texture analysis in crystalline materials. The high resolution field emission electron beam can be used for chemical analysis through either electron dispersive spectroscopy or z-contrast imaging using a scanning transmission electron microscope (STEM) detector, or can be combined with an electron backscatter detector for orientation imaging analysis.

CPN FIB Movie

The Spin-Polarized Low-Energy Electron Microscope (SPLEEM)

SPLEEM is a unique low-voltage electron microscope for the study of surfaces and interfaces. The instrument is very sensitive to structural and electronic properties of sample surfaces and is well-suited for in-situ research within a highly controlled sample environment. Spin-polarization of the electron beam permits imaging of magnetic domain microstructure

Analytical Techniques
Holography Energy-filtered Imaging Annular Dark Field TEM Imaging Electron Tomography

High-Resolution Z-contrast Imaging

STEM images of La, Sm, Er, Yb, and Lu-doped Si3N4. The matrix grain is oriented along the [0001] zone axis such that the open Si3N4 crystal structure is clearly visible at the atomic level and its prismatic plane faces an amorphous intergranular phase. The images show how the Si3N4 crystal structure ends with open hexagonal rings. For a material with strong covalent bonding this seems unusual, but it indicates that the prismatic plane may contain dangling bonds that can attract atoms from the intergranular phase. The attachment of the heavy atoms is proven by the Z-contrast technique, in which the heavier atoms appear brighter.

Core-Loss Spectroscopy
Oxygen K-edges (left) of a silicate particle containing nanopores filled with gaseous matter (right); (from top to bottom) spectrum recorded on a pore, spectrum from the silicate matrix, and the difference spectrum, which shows strong absorption features characteristic for oxygen gas (O2, p* and s* peaks) and weaker ones for water (534 and 536 eV). The spectra were recorded using a ~1-nm diameter monochromated electron probe, with 0.2 eV energy resolution.

Low-Loss Spectroscopy
Room-temperature valence electron energy-loss spectrum of a superconducting Y1Ba2Cu3O7-d sample in [100] direction (red), revealing a band gap of 1.4 eV. A Kramers-Kronig analysis yields the real (green) and the imaginary (blue) part of the dielectric function describing the dispersion and absorption characteristics of the material. The energy resolution is 0.2 eV, the spatial resolution ~1 nm.

High-Resolution TEM Imaging

Twin boundary in gold imaged by high-resolution phase contrast imaging (left) and the same area imaged using Z-contrast imaging in scanning mode (right). The arrows indicate the {111}-type twin plane.