TOPIC: HIGH RESOLUTION ELECTRON MICROSCOPY

COURSE: ELECTRON MICROSCOPY (MM-535) CONDUCTED BY: Dr. ASHRAF ALI MEO PRESENTATION PREPARED BY: SYED UMAIR AZHER (MM-03) DATE: 02-11-2009
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HIGH RESOLUTION ELECTRON MICROSCOPY

HIGH RESOLUTION ELECTRON MICROSCOPY is an imaging mode

of the electron microscope that allows the imaging of the crystallographic structure of a sample at an atomic scale. High resolutions is not high magnifications; its primarily about being able to see more, see smaller, etc. At present, the highest resolution realised is 0.8 with microscopes. At these small scales, individual atoms and crystalline defects can be imaged. HREM technique allows the direct observation of crystal structure and therefore has an advantage over other methods in that there is no displacement between the location of a defect and the contrast variation caused in the image.

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WORKING PRINCIPLE
Image formation: Contrast arises from interference of the electron wave with itself. Phase contrast imaging: When the sample is thin enough and the amplitude variations do not contribute to the images. We generally consider images formed from one beam, either a diffracted or undiffracted beam, and these are examples of amplitude contrast. If more than one beam is selected in the objective aperture, interference between these beams leads to image contrast arising from phase differences between the beams.

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WORKING PRINCIPLE

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WORKING PRINCIPLE
For two beams at the Bragg condition, the interference pattern generated has an intensity: Ig = A2 + B2 2AB sin 2|g.r| Were, g = k-k, A, B are the amplitudes of the two waves. This results in an image with a sinusoidal oscillation of intensity normal to g with periodicity 1/|g| In the image plane:

In the back focal plane:

Fringe spacing is proportional to 1/|g|

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WORKING PRINCIPLE
If an array of diffracted spots were included in the aperture centered on the direct (unscattered) beam, then the image will be a cross-grating of sine fringes arising from interference between all of the beams included in the aperture. These lattice fringes are not necessarily direct images of the structure because the phase relationship between the beams is distorted by the aberrations of the lenses. Chromatic aberrations. Spherical aberrations. Astigmatism.

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WORKING PRINCIPLE: Lens aberrations

Spherical aberration: The magnetic field of the electron lens is not uniform causing the off axis electrons to be focused more strongly, thus creating a variable focal length with distance from the optic axis.

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WORKING PRINCIPLE: Lens aberrations

Chromatic aberration: Focal length depends on wavelength of electrons. All electron sources demonstrate a degree of temporal coherence, with a range of electron energies emitted.

Astigmatism: Focal length of the lens varies azimuthally. At the disc of least confusion the beam is circular, away from this point the beam is elliptical.

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DRAWBACK:
One of the difficulties with HREM is that image formation relies on phase contrast. In phase-contrast imaging, contrast is not spontaneously interpretable as the image is influenced by strong aberrations of the imaging lenses in the microscope. Resolution of the HREM is limited by spherical and chromatic aberration, but a new generation of aberration correctors has been able to overcome spherical aberration. For exemple, software correction of spherical aberration has allowed the production of images with sufficient resolution to show carbon atoms in diamond separated by only 0.89 and atoms in silicon at 0.78 at magnifications of 50 million times. Improved resolution has also allowed the imaging of lighter atoms that scatter electrons less efficiently lithium atoms have been imaged in lithium battery materials.

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Why HREM:
High resolution electron microscopy can resolve object details smaller than 1 nm (10-9 m). It can be used to image the interior structure of the specimen (comparing to atomic resolution scanning tunneling microscopy, only at the surface). Comparing to atomic resolution provided by X-ray diffraction (averaging information), HREM can provide information on the local structure. Direct imaging of atom arrangements, in particular the structural defects, interface, dislocations. The ability to determine the positions of atoms within materials has made the HREM an essential tool for nanotechnology research and development in many fields, including heterogeneous catalysis and the development of semiconductor devices for electronics and photonics.

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High-Resolution Electron Microscopy: Carbon nanotube

Discovery of the carbon nanotube S. Iijima, Nature 354, 56 (1991).

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High-Resolution Electron Microscopy: Au Nanoparticles

Shape Determination of Au Nanoparticles

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High-Resolution Electron Microscopy: Interface

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INTERPRETATION OF HREM IMAGES

The use of HREM images and/or electron diffraction patterns for structure determination is called electron crystallography. Two electron crystallography techniques based on HREM images have recently emerged: 1- The reconstruction of the exit wave by acquiring HREM images at different defocus values named through focus exit wave reconstruction (TF-EWR). The resulting structure is refined with the diffraction intensities recorded on a CCD camera, with a software which includes the excitation error and the dynamical effects, called multi-slice least squares (MSLS). 2- The processing of HREM images of thin samples by crystallographic image processing (CRISP). This permits to extract the phase and the amplitudes of the HREM image and correct them by considering the changes introduced by the transfer function, the astigmatism (and possibly the tilt).

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REQUIREMENTS FOR HIGH RESOLUTION WORK

The microscope site must be acceptable. Mechanical vibration, stray magnetic fields, and room temperature must all be within acceptable limits. In order to record an image at a specified focus defect it will be necessary to measure the change in focus between focus control steps (clicks) using different methods. The resolution obtained in a transmission image depends amongst other things on the specimen position in the objective lens. The optimum specimen height must be found by trial and error. In reducing the specimen height and so increasing the objective lens current needed for focus, the lens focal length and spherical aberration constant are reduced, leading to improved resolution.

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REQUIREMENTS FOR HIGH RESOLUTION WORK

A vacuum of 0.5 107 torr or better is needed (measured in the rear pumping line). The simplest way to trace vacuum leaks is to use a partial pressure gauge. A reliable, constant temperature and pressure supply of clean cooling water must be assured. The microscope high voltage must be sufficiently stable to allow highresolution images to be obtained. The room containing the microscope must be easily darkened completely.

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REFERENCES:
Spence, J. C. H. (2003). High-resolution electron microscopy, New York Agar, A. W., Alderson, R. H., and Chescoe, D. (1974). Principles and practice of electron microscope operation. In Practical Methods in Electron Microscopy (ed. A. M. Glauert). North-Holland, Amsterdam. Alderson, R. H. (1974). The design of the electron microscope laboratory. In Practical Methods in Electron Microscopy (ed. A. M. Glauert). North-Holland, Amsterdam. Bennett, A. H., Jupnik, H., Osterberg, H., and Richards, O. W. (1951). Phase Microscopy. Principles and Applications. Wiley, New York. Cosslett. V. E. (1958). Quantitative aspects of electron staining. J. R. Microsc. Soc. 78, 18. Downing, K. H. and Siegel, B. M. (1973). Phase shift determination in single-sideband holography. Optik 38, 21.

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REFERENCES:
Lipson, S. G. and Lipson, H. (1969). Optical Physics. Cambridge University Press, London. Spence, J. C. H. (1974). Complex image determination in the electron microscope. Opt. Acta 21, 835. Unwin, N. (1971). Phase contrast and interference microscopy with the electron microscope. Phil. Trans. R. Soc., Lond. B261, 95. Goodman, J. W. (1968). Introduction to Fourier Optics. McGraw-Hill, New York. Rambu, A. P, Curecheriu. L. P & Mihalache, G. High Resolution Electron Microscopy of Soft Condensed Matter Systems. University Alexandru Ioan Cuza, Romania

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