Lecture # - Electron Microscopy

References
http://bama.ua.edu/~mweaver/courses/MTE4 81/Electron%20Microscopy.pdf http://tpm.amc.anl.gov/Lectures/Zaluzec-1Instrumentation.ppt.pdf

Timeline
1897 JJ Thompson - Discovery of the Electron 1926 H. Bush Magnetic/Electric Fields as a Lens 1931 Knoll and Ruska 1st EM built 1932 Davisson and Calbrick - Electrostatic Lens 1939 von Borries & Ruska - 1st Commercial EM ~ 10 nm resolution 1945 ~ 1.0 nm resolution (Multiple Organizations) 1965 ~ 0.2 nm resolution (Multiple Organizations) ~ 0.3 nm resolution probe - practical Field Emission Gun 1986 Ruska et al - Nobel Prize 1999 < 0.1 nm resolution achieved (OM ) 2009 0.05 nm (TEAM)

Why Electrons?
Resolution in microscopes is limited by the wavelength of imaging beam (Abbe Diffraction Limit) . = () Where = wavelength of the imaging radiation (400-800nm for light and ~ 0.003nm upper limit for electrons) = index of refraction of the lens = illumination semi-angle NA = numerical aperture = sin ()

Light vs Electrons
0.6 = sin()

Light: 0.6 (400) = = 170nm 1.5sin(70) Electrons: 0.6 (0.06) = = 0.4nm 1sin(1) Electrons offer much better resolution!

Resolution

Human eye

Optical Microscope

Virus Mosquito

X ray Microscopy MEMS Motor

Electron Microscopy Atoms in a lattice

Electron interaction with matter

Incident e- Beam

Backscattered e-

Secondary eCharacteristic X rays

Auger esample

Visible light Electron hole pairs

Bremsstrahlung radiation Elastically scattered elnelastically scattered e-

Directly transmitted e- Beam

Backscattered electrons (BSE)

Formation
Caused when incident electrons collide with an atom in a specimen that is nearly normal to the path of the incident beam. Incident electron is scattered backward (reflected).

Use
Imaging and diffraction analysis in the SEM. Production varies with atomic number (Z). Higher Z elements appear brighter than lower Z elements. Differentiate parts of specimen having different atomic number

Backscattered electrons are not as numerous as others. However, they generally carry higher energies than other types of electrons

Secondary Electrons
Formation
Caused when an incident electron knocks an inner shell electron (e.g., k-shell) out of its site. This causes a slight energy loss and path change in the incident electron and ionization of the electron in the specimen. The ionized electron leaves the atom with a small kinetic energy (~5 eV)

Use
IMAGING! Production is related to topography. Due to low energy, only SE near the surface can exit the sample. Any change in topography that is larger than the sampling depth will change the yield of SE. More abundant than other types of electrons. They are electrons that escape the specimen with energies below ~50eV

Auger Electrons
Formation
De-energization of the atom after a secondary electron is produced. During SE production, an inner shell electron is emitted from the atom leaving a vacancy. Higher energy electrons from the same atom can fall into the lower energy hole. This creates an energy surplus in the atom which is corrected by emission of an outer shell (low energy) electron

Use
AE have characteristic energies that are unique to each element from which they are emitted. Collect and sort AE according to energy to determine composition. AE have very low energy and are emitted from near surface regions.

Exploited in Auger Electron Spectroscopy

X Rays
Formation
Same as AE. Difference is that the electron that fills the inner shell emits energy to balance the total energy of the atom.

Use
X-rays will have characteristic energies that are unique to the element(s) from which it originated. Collect and sort signals according to energy to yield compositional information. Energy Dispersive X-ray Spectroscopy (EDS)

Foundation of XPS (X-ray photoelectron spectroscopy). XPS can be used to determine the state of an atom and to identify chemical compounds.

Transmitted electrons
Can be used to determine: thickness crystallographic orientation atomic arrangements phases present etc.

Foundation for Transmission Electron Microscopy (TEM)

http://en.wikipedia.org/wiki/Electron_microscope

Components of a TEM
Source
Electron gun Anode

Condenser lens assembly

Electromagnetic lenses

Sample stage
With provisions for tilt and translations

Objective lens Imaging assembly Detectors

 Electron gun provides a steady stream of high energy electrons electron emission
Thermionic Field emission

TEM Electron source

TEM Electron Source

Current density is given by

= ATc2 exp (-/KTc )

k is Boltzmanns constant, TC is the cathode temperature and A and are a constants depending on material. Note that jc T. W has TC of 2500-3000 K (melting point 3650 K) LaB6 has a TC of 14002000 K Heating usually produced by running a current through the material!

Operation of thermionic gun

Apply a positive electrical potential to the anode Heat the cathode (filament) until a stream of electrons is produced >2700 K for W Apply a negative electric potential to the Wehnelt electrons are repelled by the Wehnelt towards the optic axis Electrons accumulate within the region between the filament tip and the Wehnelt. This is known as the space charge. Electrons near the hole exit the gun and move down the column to the target (in this case the sample) for imaging.

 The width b of the potential barrier at the metal-vacuum boundary decreases with increasing electric field E. For |E|>107 V/cm the width b < 10 nm and electrons can penetrate the potential barrier by the wave mechanical tunneling effect.

 Electric/Magnetic fields employed to manipulate path of electron Consist of Cu wire coils around soft Fe cores. sometimes an Fe pole-piece is used to shape the field.

Lenses

Path of an electron in EM field

http://www.schoolphysics.co.uk/

Types of electron lenses

Condenser Lenses ~ Type A, Objective Lenses ~ Type A B or C, Stigmators Type D

Lenses

Magnification is achieved by Stacking Lenses

M= M1 * M2 * M3

TEM sample preparation methods

Tissue sectioning Chemical milling (etching) Mechanical polishing Sample staining Ion milling

http://www.docstoc.com/docs/67848646/TEM-sample-preparation-guide-Slide--Pips

TEM Sample preparation Ion milling

Imaging Methods
Bright field imaging mode Electron energy loss spectroscopy Energy dispersive X ray spectroscopy Selected area diffraction Scanning transmission electron microscopy
Annular dark field imaging High angle annular dark field imaging

TEM Imaging Bright Field

Most common mode of imaging Brightness contrast obtained by absorption of electrons by the sample Higher z absorbs more and hence darker than the lower z regions leads to brightness contrast Some examples of bright field imaging.

Bright field imaging some examples

Electron energy loss spectroscopy

Inelastic scattering

Inelastically scattered electrons have a characteristic energy loss depending on the material it passes through Example: electrons passing through C have an energy loss of 285eV due to inelastic scattering The energies of the scattered electron are estimated using an electron energy loss spectrometer and sample composition is determined

EELS Spectrum - Example

http://web.utk.edu/~gduscher/eels.html

EDX Energy Dispersive X ray spectroscopy

Each element has a characteristic X ray wavelength that is emitted following the above process Detector measures the X rays to determine the composition of the sample

EDX - Spectrum

STEM Scanning Transmission Electron Microscope

focusing the electron beam into a narrow spot which is scanned over the sample in a raster. Scattered electrons are collected by detectors Atomic resolution possible using high angle detectors contrast is directly related to the atomic number (z-contrast image)

STEM imaging - Example

Selected Area Diffraction

Electron beam undergoes Bragg scattering wavelength of high-energy electrons is a few thousandths of a nanometer whereas the spacing between atoms in a solid is about a hundred times larger the atoms act as a diffraction grating to the electrons, which are diffracted.

Imaging vs. Diffraction

Imaging vs. Diffraction

Example of SAD Imaging

http://www.2spi.com/catalog/standards/niox.shtml

Scanning Electron Microscope

References
http://www.eng.utah.edu/~lzang/images/Lecture_3_conventional -Microscope.pdf

SEM - Basics
In scanning electron microscopy (SEM) an electron beam is focused into a small probe and is rastered across the surface of a specimen. Several interactions with the sample that result in the emission of electrons or photons occur as the electrons penetrate the surface. These emitted particles can be collected with the appropriate detector to yield valuable information about the material. The most immediate result of observation in the scanning electron microscope is that it displays the shape of the sample. The resolution is determined by beam diameter.

Operation of SEM

Electron interaction with matter

Imaging methods
Secondary electron imaging Backscattered electron imaging EDX Energy dispersive X ray imaging

SEM imaging - Secondary electrons

Secondary electron

electrons generated as ionization products. They are called 'secondary' because they are generated by other radiation (the primary radiation) Secondary electrons are collected by the detector and used for imaging Low energy ensures most of the collected secondary electrons are from the sample surface brightness of the signal depends on the number of secondary electrons reaching the detector secondary electron imaging or SEI can produce very high-resolution images of a sample surface, revealing details less than 1 nm in size.

Backscattered electron Imaging

electrons that are reflected or backscattered from the sample by elastic scattering intensity of the BSE signal is strongly related to the atomic number (Z) of the specimen BSE images can provide information about the distribution of different elements in the sample

Backscattered imaging vs. secondary electron imaging

Backscattered electron image

Secondary electron image

http://en.wikipedia.org/wiki/Scanning_electron_microscope

Examples of SEM images

http://tysontrepidations.wordpress.com/2011/07/02/say-cheese-for-scanning-electron-microscopy

Helium Ion Microscopy

References
http://www.zeiss.com/C1256E4600307C70/E mbedTitelIntern/ArticlePhotonics-HeliumIonMicroscopy/$File/Photonics_Spectra_ORIO N.pdf http://www.imec.be/efug/EFUG2012_05_Gna uck.pdf http://www.fibsem.net/web_documents/201 0Presentations/2010DCFIBUGM-HeIM.pdf

State of Affairs
Optical microscope
Very easy to set up, low cost, color images Low resolution due to large wavelengths

Scanning Electron microscope

Use electrons instead of photons, much better resolution (~2nm) Stagnated at 2nm for the past few years

Transmission electron microscope

Resolution lower than 2nm easily achieved Expensive, detailed sample preparation required

Enter - Helium ion microscope

Sub nanometer resolution achieved Better contrast

HIM - Basics
Uses a beam of He ions Larger mass than e and hence smaller de broglie wavelength and hence much better resolution than possible with electrons 0.6 = sin()

HIM - Schematic

http://www.medgadget.com/2007/09/the_orion_helium_ion_microscope.html

HIM Helium source

+V

Needle at cryo temp

He atom

Intense E Field

He ion

HIM imaging - Secondary electrons

Secondary electron

electrons generated as ionization products. They are called 'secondary' because they are generated by other radiation (the primary radiation) Secondary electrons are collected by the detector and used for imaging Detected number of secondary electrons varies with material composition and shape Provides excellent topographical and compositional imaging

HIM imaging- Backscattered electrons

Small fraction of incident He ions are backscattered Probability of backscattering depends on the atomic number of the target element Hence we get an contrast image with brightness dependent on the atomic number

HIM Vs. SEM

HIM vs. SEM

Helium beam generates contrast from atomically thin layers as well as chemical contrast (light grey is NH2 and dark grey is -NO2)

Self Assembled Monolayer of 4 nitro-1,1 -biphenyl-4-thiol (NBPT) exposed with E-beam Lithography which modifies the terminal group from NO2 (dark grey) to NH2 (light grey)

HIM Nanomilling and patterning

HIM Milling and Patterning

Ga FIB ~ 20nm HIM ~ 1nm

Some nanopatterns

Examples HIM nanopatterning

Examples HIM Nanopatterning