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What is needed for High Resolution

SEM?
A small probe size
High beam current
A mechanically
stable microscope
and a quiet lab
environment
A skilled operator

Lens performance
The probe size is determined by the
aberrations of the lens
The magnitude of the aberrations vary
with the focal length of the lens - which is
about equal to the working distance
Some lens designs are more capable than
others at combining both high
performance and good sample access

Lens performance cont.


Aberrations including spherical and
chromatic are correctable to varying
degrees
Corrections depend on a variety of factors
including pole piece quality, aperture size,
aperture, angle and electron wavelength

Pinhole Lens
The original SEM lens designed to produce no
magnetic field in the
sample chamber
Good sample access
Long focal length and a
big working distance so
high aberrations
Poor EM screening
Asymmetric SE
collection due to
position of ET

ET
sample

Immersion Lens
Short focal length so low aberrations
Good EM screening
Very stable specimen
mounting in lens
Symmetric SE
collection using the
through the lens
(TTL) detector system
Restricted to small
samples (3mm disc)

det

magnetic
field

Snorkel Lens
Short focal length so low aberrations
and high
performance
Good EM screening
The sample is
outside the lens so
there is no
limitation on the
size of the specimen

TTL

Magnetic field
projected out
of lens

ET

S4700 Snorkel Lens


Up to 45 degrees of sample
tilt even at short WD and
permits EDS operation at WD
of 12mm
Biased deflector plates
optimize SE collection for
either or both detectors
Improved magnetic screen
and stronger stigmators can
image magnetic samples at
all WD
The lens also acts to filter
the SE signal to the TTL

S4700 lens configuration


Excitation - 1000 amp.turns

S4700 detector
Snorkel lens permits multiple
detectors to be used
In-lens (TTL) detector gives a
shadow free image with ultrahigh topographical
resolution. Super efficient
Lower (ET) detector gives SE
images with material contrast
information and high
efficiency at high tilt angles
These detectors can be used
separately or combined as
desired for maximum
flexibility
Snorkel lenses allow multiple detectors

Detector Flexibility

DRAM with both Upper and Lower detectors

MO layer in BSE mode

(DRAM stands for dynamic random access memory, a type of memory)

Multiple imaging modes provide flexibility and


problem solving power

What determines spot size?


The spot size depends on
the beam energy, WD,
and the final aperture
convergence angle
Performance improves
with higher energies
On the S4700 the
aperture size is set
automatically
Changing the CL (spot
size) does not affect
resolution much

Variation of probe size with energy


and beam convergence for S4700

Working Distance
Working distance is the
most important user
controlled parameter
Always use the
smallest WD that is
possible for a given
specimen
Note also that the
image resolution is
almost independent of
the beam energy

Microanalysis

Imaging

Beam current
Typical contrast levels
are 3-10% on most
samples
Improving contrast
lowers required IB ,
beam current, and
improves resolution
Increase IB by raising
the tip emission
current from 10A to
20 or 30 A if
necessary

Resolution
The pixel size is
equal to the CRT
pixel size divided
by the actual
magnification e.g a
100m pixel at
100x gives 1m
resolution
Probe size only
limits resolution at
high magnifications

Image at 1kx magnification


has 0.1m pixel resolution

Image Content
SE1 - high
resolution
SE2 - low (BSE)
resolution
SE3 - tertiary
signal, interactions
of the BSE with the
pole piece and
chamber walls
ET sees 40% SE3,
45% SE2, 15% SE1
TTL sees 75% SE2
and 25% SE1

SE1
TTL
SE2
Lens

Detector
ET

BSE
SE2

SE escape

SE1

SE3

SE1/SE2 interaction volumes


The SE1 signal
comes from a few
nm area at all
energies
The SE2 signal
comes from an area
that can be up to a
few microns in
diameter at high
energies

Pixel size and SE2


At low and medium
magnifications the
pixel size ( a few m)
is comparable with SE2
interaction volume
So the image is mostly
from the BSE
generated SE2
component
The SE1 are not a
significant contributor

SE2
area

pixel

Medium magnification
Medium
magnification
images have a
resolution limited
by SE2 interaction
volume
SE and BSE images
will look similar
but not necessarily
identical

Image at 20kx - 50
pixels

High magnification images


pixel

Field of view is
about size of the SE2
interaction volume so
that signal remains
about constant as
beam scans
The pixel size is
about equal with the
SE1 area so the SE1
component now
provides the image
detail
field of view

Pixels - a summary
High resolution requires the use of a high
magnification to keep the pixel size at a
small enough value not to limit the
resolution
High resolution at high beam energies
also requires a high magnification so as to
separate the SE1 signal from the lower
resolution SE2 signal

High resolution imaging


On the S4700
imaging in SE mode
with a resolution into
the nanometer range
is readily possible
What is the ultimate
resolution limit?
Optical performance,
signal origination,
and current to
establish sufficient
signal quality
Imaging a 10nm thick oxide layer

How good is SE resolution?


The production of SE
occurs over a finite
volume of space
The initial SE event
produces additional SE
and so on, leading to a
diffusing cloud of SE
around the impact point
How far do they travel?
Depends on the MFP
(mean free path)

SE resolution
The diffusion effect is visible at the
edges of a sample as the bright
white line' due to extra SE emission
The width of this line is a measure
of the SE MFP
The presence of this SE1 edge effect
sets an initial limit to the achievable
SE image resolution

SE diffusion volume

Molybdenum tri-oxide crystals


Hitachi S900 25keV

Classical resolution limit


When the object is large
its edges are clearly
defined by the white
lines
But as the feature
reaches a size which is
comparable with the
edge fringes begin to
overlap and the edge
contrast falls

Width =

20nm

10 nm

Classical resolution limit


When the feature size is
equal to or less than the
edge lines overlap and the
object is not resolved at all
since it has no defined size
or shape
This is Gabors resolution
limit for SE imaging
The resolution in SE mode
therefore depends on the
value of

width =

5 nm
Particle contrast

High Resolution Imaging


On a high atomic
number, very dense ,
material such as
tungsten the SE MFP is
only a nanometer or
so
So a spatial resolution
of about 1nm is likely
to be possible
In fact ...

Lattice fringes
In this image by Kuroda et al
(J.Elect.Micro 34,179, 1985)
fringe structures with a
spacing of 1.4nm are clearly
visible in the SE image
This resolution is consistent
with the diffusion model for
SE production with =1nm
Image recorded at 20keV on
an Hitachi S-900 FEGSEM
The probe size for this
image was about 0.9nm

Surface
Configuration

In other samples...
When an object gets
small enough to be
comparable with
then it becomes
bright all over and
the defining edges
disappear.
For low Z, low
density materials,
this can happen at a
scale of 5-10nm

edge brightness

no edges

Carbon nanotubes

The resolution limit


The resolution of the SEM in SE mode is
thus seen to be limited by the diffusion
range of secondary electrons, especially
in low Z materials
In addition the signal to noise ratio is
always worse for the smallest detail in the
image

Improving the resolution


Improving SEM resolution therefore
requires two steps:
minimizing or eliminating the spread of
secondary electrons
improving the signal to noise ratio so that
detail can be seen

Improving the S/N ratio


Use a metal coat as all
metals give more SE
than carbon
SE yield tends to rise
with Z value
But high Z materials
are denser and cause
more scatter
Usually consider Cr, or
Ti as best choices but
W, Pt are also good
Computed SE1 yield at 2keV

Particulate Coatings
Au produces very big
particles (30nm)
Au/Pd and W make
much smaller (3nm)
particles
These have a very high
SE yield
Can be deposited in a
sputter coater
Coatings are stable
Good below 100kx

3nm of Au/Pd at 100kx

Decoration
In some cases the
sputtered particles
decorate active
features on a
structure, making
them more visible
High Z materials,
such as tungsten
also permit BSE
imaging

Tungsten decorated T4 polyheads


25nm ring diameter
30keV Hitachi S900

Bypassing the limit


Since metals have much lower than
carbon, and a higher SE yield, a thin
metal film coating on a low Z, low
density sample effectively localizes
all SE production within itself. The
resolution now is a function of the
film thickness only and not of
Works even with very thin metal
films (few atoms thick)
Can exploit this effect to give
interpretable contrast at high
resolution

High SE
yield

Low SE
yield

width film even


when <

Mass thickness contrast


The SE1 yield varies
with the thickness of
the metal film
This effect saturates
at a thickness equal
to about 3
The conformation of
the film to surface
topography thus
provides contrast

S
E

bulk value

Y
i
e
l
d

mass thickness
variation

1nm

2nm

Film thickness

3nm

Metal builds contrast


The SE localization in
the film provides edge
resolution
The mass thickness
effect gives extra
contrast enhancement
The feature is now truly
resolved since its size
and shape are visible

2nm metal film

5nm low Z object

SE

SE profile with metal film

Beam position
SE profile without metal

Cr coatings
Cr films are smooth and
without structure even at
thicknesses as low as 1nm
The mass thickness contrast
resolves edges and make
the detail visible down to a
nanometer scale
The high SE yield of the Cr
improves the S/N ratio
However these coatings are
not stable - so use Cr
coated samples immediately
after they have been made

AIDS virus on human cells 500kx


2nm Cr at 20keV Hitachi S900

Coating Summary
Coatings are an essential part of the technique of
high resolution SEM because they generate
interpretable contrast, improve resolution, and
enhance the S/N ratio
Thin coatings are better than thick coatings - do not
make your sample a piece of jewelry
Below 100kx particulate coatings are superior
because of higher SE yields
Above 100kx use chromium or titanium
MRC lab uses Au/Pd coatings on most samples
Carbon is a contaminant not a coating

Getting the most from your SEM


Alignment is crucial. Check aperture
alignment every time you change
areas or imaging conditions and
ensure that the stigmators are
properly balanced
Minimize vibrations by choice of SEM
location. Move pumps away etc.
Keep the room quiet, noise dampening
material on the walls.
Check for stray fields. Remove
fluorescent lights and dimmer controls.
Keep computer monitors away - use
flat screens
Beware of ground loops

Clean Power
Many cases of
jaggies are due to
dirty mains lines
not EM pickup
Check waveform at
your wall plug
Use clean power
from a UPS for
critical electronics
Avoids surges

zero
crossings
AC line
and
EM Field
raster is
synchronized
with field

switching spikes

zero
crossings

raster is now
not synchronized
with field

Operating tips
Allow the SEM to thermally stabilize
and the cold finger to cool down
before attempting high resolution this may take > 1 hour (seldom used
at MRC)
Use the stage lock - but dont forget
to turn it off before unloading sample
Use the beam shift rather than stage
motion - but remember to recenter the
beam before taking a critical image
Look for the scan speed which
minimizes jaggies when viewing the
image live

Getting the best image


Whenever possible take a
single slow speed scan
rather than accumulating
multiple high speed scans
This eliminates blurring
due to drift, and
distortions in the video
amplifier chain and
usually produces a higher
signal to noise ratio and
better contrast

32 high speed
frames

single 20
second scan