Introduction to Electron Microscopy

Definition of Electron Microscopy

Science of imaging specimens on a very fine scale using an electron beam. Useful in obtaining information on material topography, morphology, composition and crystallographic information

Why use electron microscope

Electron Microscopes were developed due to the limitations of Light Microscopes which are limited by the physics of light to 500x or 1000x magnification and a resolution of 0.2 micrometers

Electron vs. Optical Microscopy

Electron Microscopy Uses electron beam Optical Microscopy Uses visible light

Magnification up to 200K Magnification can be up times to 1000X

Types of Electromagnetic Radiation

Radiation Acoustic Infra red Visible light (Blue to Red) UV X-Rays Electron Wavelength (nm) >1000 900-860 400-700 25-400 0.01-1.5 0.005

History of Microscope
Long before, in the hazy unrecorded past, someone picked up a piece of transparent crystal thicker in the middle than at the edges, looked through it, and discovered that it made things look larger. The earliest records of the use of lenses were in the writings of Seneca and Pliny the Elder, Roman philosophers during the first century A.D. They were named lenses because they are shaped like the seeds of a lentil.

Forerunners of compound microscope and telescope 1590

History of Microscopy

Zaccharias Janssen and his son Hans 1590, Two Dutch spectacle makers discovered that nearby objects appeared greatly enlarge while experimenting with several lenses in a tube

Developed the Telescope in 1609

History of Microscopy

Galileo Galilei from Venice constructed a 10power telescope working only on instinct and bits of rumors, never having actually *seen* the Dutch spyglass of Zaccharias and Hans He used his telescope to study the heavens. Some of the radical findings his discovered during his time was that the moon was not smooth but "uneven, rough, full of cavities and prominences." and that the Earth is not the center of the universe which later caused him to be accused of heresy by the Vatican church.

Developed Single Light Microscopy in 1675

History of Microscopy

Antoine van Leeuwenhock 1632-1723, (Father of Microscopy) taught himself new methods for grinding and polishing tiny lenses of great curvature which gave magnifications up to 270 diameters, the finest known at that time. This lead to the building of the first microscope that was instrumental in viewing and describing for the first time bacteria, yeast plant and other microorganisms.

Developed First Compound Microscope in 1677

History of Microscopy

Robert Hook 1632-1723, (English Father of Microscopy) English father of microscopy, re-confirmed Anton van Leeuwenhoek's discoveries of the existence of tiny living organisms in a drop of water. Hooke made a copy of Leeuwenhoek's microscope and then improved upon his design

Resolution dependency on wavelength of energy source 1873

History of Electron Microscopy

Ernst Karl Abbe & Helmothz, derived mathematical expression for resolution of microscope : Resolution is limited to approximately the wavelength of illuminating source

Negatively charged particles described and was later on called ELECTRONS 1897

History of Electron Microscopy

J.J. Thomson along with a group of his graduate students, set out to investigate this particle using cathode ray tubes. His experiments definitely defined the rays in the tube as actual particles having a negative charge and a finite mass

Theory of wave nature of electrons 1924

History of Electron Microscopy

Prince Louis-Victor Pierre Raymond de Broglie , (1929 Nobel Peace Prize in

Physics)
Identifies a wavelength to moving electrons l=h/mv where l = wavelength h = Planck's constant m = mass v = velocity (For an electron at 60kV l = 0.005 nm)

Electron Optics 1924

History of Electron Microscopy

Hermann Heinrich Busch, The same way as light can be deflected by an optical lens, electron path can be deflected by magnetic lenses (axial magnetic field refract electrons)

History of Electron Microscopy

In the early 1930s, the limitation of light microscopy and the scientific desire to see finer details of specimen by 10,000x magnification led to the development of Transmission Electron Microscope (TEM) The TEM was the first type of Electron Microscope to be developed and is patterned exactly on the Light Transmission Microscope except that a focused beam of electrons is used instead of light to "see through" the specimen.

First Electron Microscope developed 1932

History of Electron Microscopy

Max Knoll and Ernst Ruska , Developed the first electron microscope (Siemens) with 10nm resolution in Germany

First Commercial Enterprise to develop a prototype of an electron microscope 1936

History of Electron Microscopy

Metropolitan Vickers in UK first produced EM1low resolution electron microscope (in 1939 Siemens and Halske produce first commercially electron microscopes)

First SEM was constructed 1938

History of Electron Microscopy

Manfred Von Ardenne, a private consultant who has his own laboratory in Berlin developed the first scanning electron microscope (SEM) with a sub-micron probe in two years. He worked for less than two years on scanning electron microscope before concentrating on the development of his universal TEM

First EM built in North america 1939

History of Electron Microscopy

James Hillier and Albert Prebus, built the first EM at the University of Toronto

First ever commercial TEM sold in the US by the RET Group 1941-1963 Continuous improvement in TEM resolution from 0.2 to 0.3 nm 1954 First Commercial SEM introduced in the market by Siemens Elmscope 1958 Stereoscan was introduced for the first time by Cambridge instrument

1940-1941

History of Electron Microscopy

1957

History of Electron Microscopy

1959 1960

Bernard and Devoine built SEM with 1 micron probe size at the Institute of Applied Science in France UKs AEI, then a major TEM manufacturer, developed and sold first SEM instrument - At the Westinghouse Laboratories in Pittsburgh, Wells, Everhart, Matta and others built an advanced SEM for semiconductor studies and microfabrication and demonstrated EBIC imaging - Moscow University in USSR obtained their first SEM

1964

History of Electron Microscopy

1965 1982

Prototype of steroscan obtained by Dupont Chemical Corp in the US Six months after, Japan firm JEOL marketed their JSM-1SEM The use of commercial SEMs became more widespread STM was invented by Gerd Binnig and Heinrich Rohrer who won the Physics Nobel Prize in 1986 for this achievement.
Binnig Rohrer

Leading TEM Manufacturers

Hitachi (JPN) JEOL (JPN) Topcon (Korea) Philips (Holland) LEO (Germany)

Leading SEM Manufacturers

AMRay (US) Leica (UK) VG (UK) Hitachi (JPN) TOP CON JEOL (JPN) Philips (Holland) RT Leo (US) LEO

Optical, SEM and TEM microscopy Comparison

Light vs Electron Microscope

Electron-Specimen Interaction

e-

backscattered eelemental contrast

http://www.jeol.com/sem_gde/imgchng.html http://www.unl.edu/CMRAcfem/ http://www.ou.edu/research/electron/www-vl/ http://www.mwrn.com/guide/electron_microscopy/microscope.htm

ePrimary or unscattered eprojected sample image transmission electron microscopy

e- secondary esurface topography

- the resulting elastic scattering process can be used to form images and diffraction patterns in the TEM -the inelastic scattering induces secondary emissions, such as secondary electrons, Auger electrons and X-rays, which are the signals in the SEM, TEM, and STEM. EELS

Backscattered Electrons:
Formation -Caused by an incident electron colliding with an atom in the specimen which is nearly normal to the incident's path. -The incident electron is then scattered "backward" 180o Utilization -The production of backscattered electrons varies directly with the specimen's atomic number. -Higher atomic number elements to appear brighter than lower atomic number elements. -This interaction is utilized to differentiate parts of the specimen that have different average atomic number.

Secondary Electrons:
Source - Caused by an incident electron passing "near" an atom in the specimen, near enough to impart some of its energy to a lower energy electron --> a slight energy loss and path change in the incident electron and the ionization of the electron in the specimen atom resulted. - This secondary ionized electron leaves the atom with a very small kinetic energy (<50 eV) - Each incident electron can produce several secondary electrons. Utilization - Due to their low energy, only secondaries that are very near the surface (<10 nm) can exit the sample and be examined. - Collection of these electrons is aided by using a "collector" in conjunction with the secondary electron detector.

Auger Electrons
Source -Caused by the relaxation of the specimen atom after a secondary electron is produced -Since a lower energy electron was emitted from the atom during the secondary electron process an inner shell now has a vacancy -A higher energy electron from the same atom can "fall" to a lower energy, filling the vacancy - falling electron may transfer its energy to an Auger electron which is emitted Utilization - Auger electrons have characteristic energies, unique to each element from which it was emitted from - Since Auger electrons have relatively low energy they are only emitted from the bulk specimen from a depth of <3 nm.

X-rays
Source - Similar to Auger phenomenon but instead of electrons being ejected, radiation is generated during relaxation - X-ray fluorescence is the emission of characteristic "secondary" (or fluorescent) x-rays from a material that has been excited by bombarding with high-energy X-rays or gamma rays. Utilization -is widely used for elemental and chemical analysis, particularly in the investigation of metals, glass, ceramics and building materials

Thin Specimen Interactions Unscattered Electrons

Source - Incident electrons which are transmitted through the thin specimen without any interaction occurring inside the specimen. Utilization The transmission of unscattered electrons is inversely proportional to the specimen thickness -Areas of the specimen that are thicker will have fewer transmitted unscattered electrons will appear darker -Thinner areas will have more transmitted unscattered electrons appear lighter

Elastically Scattered Electrons

Source -Incident electrons that are scattered by atoms in the specimen in an elastic fashion -These scattered electrons are then transmitted through the remaining portions of the specimen. Utilization -All electrons follow Bragg's Law -All incident electrons have the same energy and enter the specimen normal to its surface. -All incidents that are scattered by the same atomic spacing will be scattered by the same angle. -These "similar angle" scattered electrons can be collated using magnetic lenses to form a pattern of spots; each spot corresponding to a specific atomic spacing (a plane). -This pattern can then yield information about the orientation, atomic arrangements and phases present in the area being examined.

Inelastically Scattered Electrons

Source -Incident electrons that interact with specimen atoms in a inelastic fashion, losing energy during the interaction -These electrons are then transmitted trough the rest of the specimen Utilization Electron Energy Loss Spectroscopy: -The inelastic loss of energy by the incident electrons is characteristic of the elements that they interacted with. -These energies are unique to each bonding state of each element and thus can be used to extract both compositional and bonding (i.e. oxidation state) information on the specimen region being examined.

Electron-Specimen Interaction
Secondary electrons (SEM)

Electron-Specimen Interaction
Ugly BUGS