Why use electrons for microscopy?

Assuming scattering g g g gives y contrast, the you , shorter the wavelength of the radiation, the better your resolution
0.61 = sin

If wavelength = 500nm (visible light), resolution = 300nm If we use electrons with E = 30keV (typical for SEM), wavelength = ?nm

Electron (e-) --> specimen interactions

Very important for studying how to get the most from your samples in the SEM and TEM Defines where contrast comes from Allows us to determine our samples elemental composition quantitatively Things to remember!
e- have mass - can transfer momentum behave e momentum, relativistically at high energies e- are waves - can constructively and destructively interfere

Electron scattering
2 primary classes of electron scattering: p y g
elastic scattering - incident electron will change direction, but not kinetic energy, scales with Z2 inelastic scattering - incident electron will change direction, but also give up some kinetic energy to the sample, scales with Bethe expression p , p will allow for elemental analysis

Ultimately, scattering will lead to the image y g g contrast

Electron scattering probability

Scattering cross section: g
N 1 = 2 nincident nt arg ets E g

Mean free path:

MW = N A

Total mean free path:

totall

+ ....

Interaction Volumes
From the mean free path, we can calculate the interaction volume of electrons and the interaction volume samples
dependent upon incident electron energy, the sample atomic mass, the sample density, and the angle of incidence of the incoming electrons

Interaction Volumes - accelerating voltage dependence (SEM samples)

2kV

10kV

30kV

Interaction Volumes - atomic mass dependence

Al

Fe

Interaction Volumes - sample density dependence

Au 100% dense

Au A 50% dense

Au 25% dense

Interaction Volumes - incident electron beam angle dependence

0 deg g (normal)

45 deg

60 deg

Elastic Scattering - SEM signals

Most elastic scattering signals in the SEM are evident as Backscattered electrons - comparable to reflection microscopy No energy loss, just change in direction d e to scattering and diffraction energ loss j st due - large dependence on surface topography and atomic number

Al

Elastic Scattering - TEM signals

In TEM, elastic scattering is evident as atomic , g number or density contrast or as diffraction

Al 100keV, 50nm thick W

Inelastic Scattering - secondary electron emission

Secondary electrons y Main signal used in the SEM for imaging Due to interactions between the e- beam and weakly bound conduction band e (metals) or valence band e ee(semiconductors or dielectrics) Secondary e- energies are typically 2-10eV, but can range up t 50eV to 50 V Since the scattering cross section increases with g gy g g generally y decreasing e- energy, lower accelerating voltages g give more SE signal

Inelastic Scattering - X-ray emission

After the incoming e- beam excites inner shell e in the sample the esample, excited e- decay back to a ground state In order to obey energy and mass conservation, they emit a X-ray The X-ray energy is dependent upon the elements present within the sample Can quantify composition by measuring these energies (EDX) Most X-rays generated are reabsorbed by the sample

Inelastic scattering - other processes

Auger e- emission
2e- process similar to the X-ray p y scenario, but instead of emitting an X-ray, a weakly bound outer shell e- is emitted (typically from the first 2nm of the surface) outer shell e- can give bonding information about the samples!! very useful in surface science

Cathodoluminescence
again similar to X-ray and Auger X ray Auger, but energy is conserved by the emission of a photon in the IR / g Visible / UV range

Inelastic Scattering - more other processes

Plasmons
incident e introduce electrostatic potential waves ein the solid which forms oscillations of e- (low energy)

Phonons
incident e- introduce lattice vibrations within the solid which causes sample h ti lid hi h l heating

Bremsstrahlung X-ray emission

as th incident e- i t the i id t interact with the electrostatic t ith th l t t ti potential of the sample, they decrease kinetic energy and emit an X-ray to obey conservation of energy does NOT excite an inner shell e- in the sample

Inelastic Scattering - e- beam damage

Inelastic events can produce radiation p damage 2 types of damage:
radiolysis - inelastic scattering produces sample heating and breaks the chemical bonds (polymers and some biological samples) reduced at high e- energies, increased at lower knock-on - direct displacement of atoms due to the knock on incoming electron beam creates point defects (insulators and semiconductors) i increased at hi h e- energies, reduced at l d t high i d d t lower

How the Scanning Electron Microscope works!

Electron source Condenser and Objective Lenses F d C Faraday Cup Steering lens Ray traces Detectors Electronics Imaging

Scanning and Image Formation

Scanning - moving beam across sample, sampling specimen at different locations with different detectors p
Analog - beam scanned continuously, but at different rates Digital - beam placed at (x,y) coordinates, intensity recorded at each point Dwell time: amount of time an area is sampled (digital: length of time beam stays in one spot)

Scanning and Magnification

Older systems (JEOL 5800) - CRT is scanned at same rate as beam on specimen using same scan g g generator Need special CRT able to scan at different rates (TV, slow, photo, etc) Also needs to be able to do line scans (no y coordinates just x) y-coordinates, Magnification M = Lcrt / Lspecimen Magnification depends on the size of your monitor and the resolution you have it set If monitor size and resolution are fi d it i d l ti fixed, can only change mag by changing Lspecimen (decreasing the length of beam scan on the sample) ONLY dependent upon the scan coils, NOT the OL strength

More Magnification
e- travel down electron column in helical path, should result in image rotation when WD or focal length is changed
Does not occur due to compensation by the scan coils

Magnification calibration
Completed using ASTM standards Also adjusts scan coils for squareness and roundness

Digital Image Acquisition

Pixel definition size definition, Sampling: Pixel is not necessarily a fundamental unit of the specimen being sampled - depends on spot size, interaction volume

Imaging - Depth of Field

Depth of Field - biggest advantage of SEM
Defined as the distance (D) between where the crossover occurs and the beam broadening is large enough that the broadening (r) is noticeable ( (+ and -) )

r tan = D /2

2r

For CRTs, r = 1pixel ~ 0.1mm r = 0.1mm / Mag 0 1mm D = 0.2mm / ( * Mag) = Raperture / WD

Depth of Field

How the Scanning Electron Microscope works!

Electron source Condenser and Objective Lenses F d C Faraday Cup Steering lens Ray traces Detectors Electronics Imaging

Electron Emitters Specifics

Electrons ejected from the emitter tip current tip, due to gun bias Electrons are then accelerated past the Wehnelt cap (anode) and into the column Fi t crossover occurs First before the anode Brightness can be g affected by filament to Wehnelt distance (in ) addition to Vo)

Electron Beam Sources - Thermionic Emission (type 1) ( yp )

Heat the emitter so that ecan escape the work function of the material into the vacuum Materials:
W (Ewf = 4.8eV), high Jc at T < Tmelting LaB6 (Ewf = 2.5eV), higher Jc b t need l but d lower vacuum for stability

Smaller tip radius, higher Jc due to electric field enhancement

Schottky effect, especially important to LaB6 Can reduce Ew by >0.1eV

Jc = 120A/cm2K2 (T2) exp(-Ew/kT)

Electron Beam Sources - Field Emission (type 2) ( yp )

Small tip radius, extremely high fields allow electron emission without h ti ith t heating, e- t tunnels directly l di tl into vacuum Ewf is reduced due to Schottky effects Bias tip 3-5kV negative relative to first anode Field strengths >107V/cm 10 Fowler-Nordheim tunneling from tip into vacuum Advantages: g
High brightness Narrow e- energy distribution High resolution

More FEG
Types:
C ld cathode (b t need Cold th d (best, d high vacuum) Thermal (bigger energy ) spread) Schottky (thermal, but good energy spread like cold cathode, small current)

Vacuum considerations:
At 10-5 Pa, one monolayer of gas is formed per second Run vacuum at 10-9 Pa to avoid changes in Ew flash heat the tip to bake off gas Use Schottk FE Schottky

FEG Tip Materials

Single crystal W sharpened to ~100nm radius g y p
W good due to high mechanical strength Needed due to high strains put on materials under high fields

How to increase e- current?

W crystal direction <310> t give l t l di ti 310 to i lowest work t k function direction the best look at the first anode Coat W crystal with ZrO (Ew = 2.8eV)

Electron Lenses
How direct electrons into a point? Electromagnets B = magnetic fl d ti flux density, f(I) it B = H in vacuum F = -e (B x v) using right hand rule Iron core wrapped N times with a conductor, pass I (current) through the conductors Bi h is homogeneous b t between th the gaps Produces Fringing Fields near Fringing Fields the optic axis - steer the e-

Lenses - General
e- interact with Br to produce a rotational force and velocity Rotational e- interact with Bz to produce a radial force - causes ee to bend toward optic axis Also causes axial path within the p column - relates as image rotations while changing focal length or spot size

How the SEM works!

Electron source Condenser and Objective Lenses F d C Faraday Cup Steering lens Ray traces Detectors Electronics Imaging

Control of Lenses
Effects of objective lens apertures
Optimizes convergence angle g Controls depth of focus Controls probe current

Control of Lenses
Effects of working distance (WD) di t
Longer WD, larger beam diameter

Control of Lenses
Effects of Condenser lens strength
Stronger CL, smaller spot size

Lens Aberrations
Aberrations are the biggest ultimate gg resolution limiters in SEM and TEMs Types:
Spherical strength of lens on e- at the outside of the lens is stronger than on those at the center Ch Chromatic e- of different energies focus at ti f diff t i f t different places Directly dependent upon focal length and ee energy spread (FEG has smaller Cc) Aperture diffraction produces beam divergence

Lens Aberrations
Aperture Diffraction

Astigmatism Spherical aberration

Chromatic aberration

Astigmatism

Imaging Defects
Tilt distortion
Mag is lower perpendicular to tilt axis (more specimen is mapped) than parallel to the tilt axis Tilt correction D Dynamic f i focus correction

Moire effects Scan distortion

Misaligned scan coils give rise to distortions at the edges of the scan

Imaging Detectors - SE
Everhart - Thornley Detector
Converts e- into light, then back into electrical signals Positively biased Faraday cage attracts low E SEs Also collect BSEs present within line of sight

More SE Imaging
Placement of E T detector E-T is important for image interpretation

Imaging Detectors - TTL

Through the lens detectors
Snorkel OL guides SEs back up the beam path t a b th to scintilltor detector with high bias g Eliminates SEs formed via the chamber walls, walls minimizes BSEs formed off-axis (nearly pure SE detector)

Elastic Scattering Backscattered electrons in the SEM

Most elastic scattering signals in the SEM are evident as Backscattered electrons - comparable to reflection microscopy No energy loss, just change in direction d e to scattering and diffraction energ loss j st due - large dependence on surface topography and atomic number Angular dependence of BSE follows a cos distribution

Backscattered electrons - atomic mass dependence

Al

Fe

Backscattered electrons - atomic mass dependence

for pure p compounds

For mixed compositions, backscatter coefficient is the sum of th BSE for each atomic composition within the material

Interaction Volumes - accelerating voltage dependence (SEM samples)

2kV

10kV

No significant accelerating voltage 30kV dependence on BSE

BSE tilt angle dependence

0 deg (normal) Higher tilts, more BSE tilts 45 deg Does not necessarily mean more signal to the detector need to tilt toward detector

60 deg

BSE detectors
Negatively biased E-T detector -Photomultiplier tube same Photomultiplier tube, as for SE -Neg. bias repels low energy SE, only detects BSE

Solid-state detector -p-n junction like a solar cell -detect electronic signal to determine contrast

Solid State BSE detectors

Flat, thin detectors placed directly above sample, allows for high BSE collection efficiency ll ti ffi i Signal is sent through an amplifier to change the brightness and contrast of the image t t f th i Can be formed in arrays signals from the different parts of the arrays can either be combined, subtracted, or viewed separately If A-B, gives topographic contrast If A+B, gives compositional contrast

BSE vs. SE Imaging

Imaging with SE and BSE on the same areas will illustrate the composition changes in the samp Brighter areas - higher atomic number

Special Topics in SEM

What else can we do with the SEM?
HRSEM Low kV imaging STEM Stereomicroscopy Voltage contrast Magnetic field contrast Crystallographic contrast Electron channeling diffraction

HRSEM
High Resolution SEM
Must overcome the contrast limits defined by the threshold equation Dependent upon C (=S/S), defined by IB, , DQE Also dependent upon interaction volume and where the signals are generated SE1 is the HR signal - need to minimize the other signals for HR imaging

More HRSEM
Signal to pixel ratios
At low mag (<1,000x), pixels are generally smaller than the interaction volume At medium mag (10,000x), overlap of pixels and interaction volumes begins to occur For 1nm, 10kV probe into Si, interaction volume is 10,000x larger than the probe size At high mag (100,000x), FOV is smaller than the interaction volume, BSE and SE2 signals get averaged out in the noise Bright edges help with contrast

HRSEM at low kV
Interaction volume smaller Most of the emitted e have high spatial res e Brightness falls off too, must balance

Setting up HRSEM
1. Reduce contamination!! 2. Thin, fine grained metal coating (increase SE1) 3. Small spot size ( p 4. Low kV (balance with spot size to maintain contrast) 5. Short WD 6. Snorkel lens 7. TTL detector 8. STIGMATE!!!!

HRSEM

Low-k / Ru surface

Stereomicroscopy
SEM has large depth of field compared to LM 3-D info is lost when displaying a 2-D image
Can be recovered by stereomicroscopy

Stereomicroscopy: py
Collect (2) 2-D images at different tilts (6 separation) sample must be at eucentric height! Displaying stereopairs: Blue / red 3-d glasses (Image J, instructions in text) Stereoviewer used with printed images p g Can also be done quantitatively using geometry to determine 3-D information about the samples

20 m

10 m

200 m

Voltage and Magnetic Contrast

If high local fields are present, they y g g may be strong enough to either significantly repel e- or attract them back into the surface Voltage Contrast Useful for failure analysis of electronic devices - bias the device in the SEM, look for bright and dark areas to see where the device is failing Which areas will appear bright vs. dark? Also visible during charging

Magnetic Contrast - Type 1

Interactions of SE1 with leakage B
F = -ev x B

Magnetic Contrast - Type 2

Interactions of e- with B inside the specimen

Crystallographic Contrast and Channeling

e- can be Bragg diffracted by individual crystals (grains)
Directionality induced by diffraction gives rise to light / dark areas Contrast determination? Threshold equation? Best to use large solid angle BSE detector

e- channeling can also give rise to diffraction patterns

Strongly affected by surface topography Better to determine crystallography with EBSD (discussed later in the semester)