Afm Vs Sem

Complementary Techniques for High Resolution Surface Investigation
Svetlana Santer
SEM and AFM:
Freiburger Materialforschungszentrum
Freiburg, 06.07.2004
Institut fr Mikrosystemtechnik
Svetlana Santer
AFM
SEM
Svetlana Santer
Scanning Electron Microscopy (SEM)

Vacuum: 10-4-10-10 Torr
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Principles of SEM Imaging

When the electron beam hits the sample, the interaction of the beam electrons from the filament and the sample atoms generates a variety of signals. secondary electrons (produced by interaction of primary e with the loosely held outer electrons of the sample), backscattered electrons (beam electrons from the filament that bounce off nuclei of atoms in the sample(elastic-interaction of the primary electrons with the nucleus of the atom), X-rays, light, heat, transmitted electrons (beam electrons that pass through the sample). Secondary electrons: high spatial resolution, good topographic sensitivity Backscattered electorns: they have more energy and can escape from greater depths, carry some informartion of sample composition
Freiburg, 06.07.2004 Svetlana Santer
Scanning Electron Microscopy (SEM)

The SEM uses a beam of electrons to scan the surface of a sample to build a three-dimensional image of the specimen.
Major Components of the Scanning Electron Microscope All scanning electron microscopes consist of: 1. 2. 3. A column which generates a beam of electrons. A specimen chamber where the electron beam interacts with the sample. Detectors to monitor the different signals that result from the electron beam/sample interaction. A viewing system that builds an image from the detector signal.
4.
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Generating the beam of electrons
The electron gun is housed on the top of the column and generates the beam of electrons that rushes towards the sample housed in the specimen chamber. Electrons are very small and easily deflected by gas molecules in the air. Therefore, to allow the electrons to reach the sample, the column is under a vacuum. The vacuum is maintained by two vacuum pumps: a rotary pump and an oil diffusion pump which is housed inside the SEM and is water cooled. Thus, the SEM needs a water cooling line which filters the water before it cools the oil diffusion pump.
Generating the beam of electrons
Within the electron gun is the filament which is the source of the beam of electrons. The filament is made of tungsten and is heated to generate a fine beam of electrons. As the filament gets used, it becomes brittle and coated. If the filament is overheated or too old, it will break.
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Detectors of the SEM
The SEM has several detectors to view the electron signals from the sample. (1) secondary electron detector looks like a Faraday cage, and detects secondary electrons. (2) backscattered electron detector (solid state detector) is located above the sample, consists of a diode with a thin gold conductor across the front surface. Backscattered electrons have sufficient energy to pass through the front surface and produce electron hole pairs which produce a curreent in the diode
Can we see electrons directly by eye?
The SEM scans its electron beam line by line over the sample. It's much like using a flashlight in a dark room to scan the room from side to side. Gradually the image is built on a TV monitor (cathode ray tube or CRT for short). The SEM has buttons on the keyboard that control the scan speed. A fast scan which takes a couple of seconds to generate an image can be very grainy - like you're looking at an object in a snow storm. A slow scan is very clear and sharp - but takes a minute or two to get a picture.
Sample preparation
Samples have to be prepared carefully to withstand the vacuum inside the microscope. Biological specimens are dried in a special way that prevents them from shriveling. Because the SEM illuminates them with electrons, they also have to be made to conduct electricity.
Sputter coater
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Examples
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History Max Knoll and Ernst Ruska -1931

electron microscopy
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History
1938 first SEM by von Ardenne 1942 first SEM for bulk samples by Zworkin 1965 first commercila instrument (Cambridge) Resolution: 50 nm in 1942 0.7 nm today
Basics of AFM
AFM provides very high resolution images of various sample properties
PSD Laser
Cantilever Tip Sample

50 nm
Piezo
Three basic components: Piezoelectric scanner Cantilever with a sharp tip
Digital Instruments (DI) MultiMode Nanoscope IIIa
Position sensitive detector (PSD) coupled with a feed-back system

Historical steps of development
1981-invention of STM 1985-invention of AFM 1986-Nobel Price Christoph Gerber

IBMs Zurich Research Center in Rschlikon
It Vt
I t ( z ) = I 0 e 2 kz , k = 2m / h ~ 1
o 1
Restriction: conductive samples

General components and their functions
Svetlana Santer
Control of the cantilever deflection

Optical Lever
STM Tunneling sensor (Binnig, Rohrer) tip
I V
t t
Optical interferometer detection system
Piezoresistive detection
special design of cantilever changing of resistivity with the applied stress
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Piezoelectric scanner
SPM scanners are made from a piezoelectric material that expands and contracts proportionally to an applied voltage Whether they expand or contract depends upon the polarity of the applied voltage. Digital Instruments scanners have AC voltage ranges of +220 to 220V +V -V 0V
No applied voltage
Extended
Contracted
In some versions, the piezo tube moves the sample relative to the tip. In other models, the sample is stationary while the scanner moves the tip
PZT
Cantilever
Solenoid
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Piezoelectric scanner Material Properties

Piezoelectric ceramics are a class of materials that expand or contract when in the presence of a voltage gradient Lead (plumbum) zicronate titanate (PZT) crystallites exhibit tetragonal or rhombohedric structure Due to their permanent electrical and mechanical asymmetry, they exhibit spontaneous polarization and deformation
Perovskite-type PZT unit cell (1) in the symmetric cubic state, (2) distorted
Poling, an intense electric field (>2000V/mm) is applied
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Geometry of PZT scanner

Tube scanner The tripod
Not stable
The outer electrode is segmented in four equal sectors of 90 degrees The inner electrode is driven by the z signal
Model Bipolar configuration A E J Scan Size 0.4 m 10 m 0.4 m 10 m Vertical Range 0.4 m 2.5 m 5 m Svetlana Santer
x = KV , K ~ 3nm / V
125 m 125 m Freiburg, 06.07.2004
Triangular pattern
Fast scan speed
v f = 2lv Hz
l v Hz N
Slow scan speed v s = Fast scan direction
Slow scan direction
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Feedback loop
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AFM Probe Construction

Low spring constant (k - 10-2 to 102 N/m) Sharp protruding tip (r=5-50 nm) High resonance frequency
1 = 2
k m
Three common types of AFM tip

normal supertip ultralever
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A few requisites for cantilevers

1. Must be soft
F = kz
Minimize k
For rectangular cantilevers Example: t=10 m, w=1mm, l=4mm k (C-C stretch.)~500N/m k~1N/m
k (C-C-H bend)~50 N/m
2. Must be insensitive to external vibrations
Maximize eigenfrequencies
k m
Minimize m L=140m, w=40m, t=1.5 m, k~0.7 N/m, ~60 kHz

Ex: Si or Si3N4
Common types of cantilevers Si3N4 Si
Diamond
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Fabrication of cantilevers
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Calibration of cantilever
Theoretical method
E=300 GPa
Static method
Dynamic method
E=238 GPa
Measuring of thermal response of the cantilever Measuring of the change of resonance frequency caused by the addition of known masses
(Z
t'
Z t k s = Z t kc
Superposition of two geometries
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Reconvolution of the tip shape I II
d D=dreal D
D2 d= 4r
Deconvolution of the tip shape

Tobacco Mosaic Virus (TMV) d~18 nm r-?
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AFM Tip Artifacts
We start off with an example of a good AFM image of 300 nm polystyrene spheres.....
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AFM Tip Artifacts
Similar spheres imaged with a supposedly sharp tip
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AFM Tip Artifacts
This image should only contain images of large polysterene spheres
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Blind Reconstruction
AFM profile of a single bump
What does this single scan line tell us about the topography of the tip and sample?
The tip geometry can be no bigger than the obtained profile
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Blind Reconstruction
Line scan having two bumps
What does this tell us about the shape of the tip? Case 1: Tip with single apex
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Case 2: double tip
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True three-dimensional scanning?

One of the drawbacks of typical AFM is that the images obtained are not truely threedimentional. No matter how sharp the tip, the data collected can never access the underside of the sample.
Petticoat effect-all images of objects having steep walls or undercut regions appear to have flared sides
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Method for imaging sidewalls by AFM
Martin, Wickramasinghe, Appl. Phys Lett 1994, 64, 2498
Can we get a similar image using a typical AFM and the boot-shaped tip?
No!
Calibration of the tip shape

2r L L
2
L R= 4r
L2 R= 2h
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Oxide-Sharpened Tips
increasing aspect ratio reducing tip radius
SiO2
HF etching
Aspect ration- 10:1 Radius r~1nm

Electron beam deposition (EBD)

High-aspect-ratio tips
L=(1-5)m R=(20-40)nm
Carbon materials are deposed by the dissociation of background gases in the SEM vacuum chamber
Svetlana Santer
Carbon Nanotube Tips

Single-walled carbon nanotubes (SWNT), d=(0.7-3)nm Multiwalled carbon nanotubes (MWNT) (nested, concentrically arranged SWNT, d=(3-50)nm High-aspect-ration AFM probes Very stiff, E=1012 Pa (the stiffest known materials) Buckled nanotubes
Labor intensive Not amenable to mass production

Pick-up Tips
d=0.9nm
d=2.8nm
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Chemical Vapor deposition (CVD)

Direct grow nanotubes onto AFM tip
Heating of nanocatalyst particle (r~3.5 nm) Presipitates carbon nucleates a grow of nanotube
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Direct grow of nanotubes

Alumina/iron/molybdenumpowdered catalyst
2 nm in diameter 2m in length
Labor intensive Not amenable to mass production

Modes of operation
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The common AFM modes

contact mode tapping mode
Contact mode Non-contact mode Intermittent mode
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Contact mode AFM

A tip is scanned across the sample while a feedback loop maintains a constant cantilever deflection (and force) The force on the tip is repulsive ~ a few nN The tip senses lateral and normal forces The tip contacts the surface through the adsorbed fluid layer Forces range from nano to micro N in ambient conditions and even lover (0.1 nN or less) in liquid
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Force curve
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Contact mode
Force Static mode Dynamic mode
F = kz , k = 0.01 0.1 N / m , z = 0.1nm F ~ 1 pN
Probe-sample distance, z
B C D
A
F > k, z at " B" is jump into a contact to " C"
Oscillation amplitude
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Problems of the contact mode

Large deformation forces ~ 100 nN Capillary forces
Fcap = 4R1 cos ~ 22nN
To solve the problem
operation in liquid
Elimination of capillary forces Reduction of van der Waals forces

Different types of forces relevant to AFM

4 3 r g 3 1 g / cm3 r = 25 nm Fg = mg = g = 9.8 m / sec 2
Fg 109 nN
(a)
FvdW =
A r 6D 2 A = 1019 J
= 4r F adh = 2 1/ 2
s p
D = 0.3 nm r = 25 nm
s = 100 mJ/m 2 silica surface energy = 25 mJ/m 2

p
FvdW ~ 5 nN
polymer surface energy
Fadh ~ 30 nN
(b) Capillary forces (d) Deformation forces

Fcap = 4R1 cos ~ 22nN
Ka 3 ~ 6nN , a ~ 5 nm, the typical contact radius Fd = R


Large lateral (shear) forces ~ 100 nN
To solve the problem
non-contact mode
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Non-contact Mode AFM
Highly unstable mode
Ultra high vacuum at low temperature
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Tapping mode AFM

A cantilever with attached tip is oscillated at its resonant frequency and scanned across the sample surface A constant oscillation amplitude (and thus a constant tip-sample interaction) are maintained during scanning. Typical amplitudes are 20-100 nm Forces can be 200 pN or less The amplitue of the oscillations changes when the tip scans over bumps or depressions on a surface
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Tapping mode AFM
0 50 500kHz A0 10 100nm
Tapping mode AFM

Force Static mode Dynamic mode Probe-sample distance, z
B C D A
Oscillation amplitude
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Tapping mode AFM
Three regimes of tapping mode: (i) Light tapping

0.7 rsp 1
rsp =
Asp A0
(ii) Moderate tapping 0.3 rsp 0.7 (iii) Hard tapping

0.01 rsp 0.3
Tapping mode AFM

Phase Imaging
Driven force Actual responce
Different characteristics of the sample
different offset the phase

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Examples of Phase Images AFM
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Advantages and Disadvantages

Contact Mode Advantages high scan speeds the only mode that can obtain atomic resolution images rough samples with extreme changes in topography can sometimes be scanned more easily Disadvantages lateral (shear) forces can distort features in the images the forces normal to the tip-sample interction can be high in air due to capillary forces from the adsorbed fluid layer on the sample surface the combination of lateral forces and high normal forces can result in reduced spatials resolution and may damage soft samples (i.e. biological samples, polymers) due to scraping
Advantages and Disadvantages

Tapping mode Advantages higher lateral resolution on most samples (1 to 5 nm) lower forces and less damage to soft samples imaged in air lateral forces are virtually eliminated so there is no scraping Disadvantages slightly lower scan speed than contact mode AFM
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Cantilevers used in contact and tapping modes
k 0.01 1 N / m
k ~ 50 N / m
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Contact vs Tapping modes
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Scanning Probe Microscope (SPM)

A family of microscopy forms where a sharp probe is scanned across a surface and some tip/sample interactions are monitored Scanning Tunneling Microscopy (STM) Atomic Force Microscopy (AFM) contact mode non-contact mode tapping mode Other forms of SPM lateral force magnetic or electric force thermal scanning phase imaging
Comparison of Techniques: AFM vs SEM

Surface structure: atomically smooth surfaces
On a sample this smooth, the SEM has difficulty resolving these features due to the subtle variations in height
TM-AFM image of 0.14 nm monoatomic steps on epitaxial silicon deposited on (100) Si. 1 m scan, RMS=0.07 nm Freiburg, 06.07.2004
Svetlana Santer

Surface structure: Thin films
SEM
On most thin films, the SEM and AFM produce a similar representation of the sample surface
AFM
Polysilicon thin film at approximately the same lateral magnification. But they differ in the other types of information AFM provides with roughness and height SEM provides a large area view Freiburg, 06.07.2004 Svetlana Santer

Surface structure: Thin films: interpretation of height
In the SEM image, it can be sometimes be difficult to determine whether the feature is sloping up or down
GaP on Si during chemical beam epitaxy deposition Freiburg, 06.07.2004 Svetlana Santer

Surface structure: High Aspect Ration Structures
SEM provides measuring the undercuts of these lines
With AFM one can measure the structure nondestructively, but without details on the sides
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Surface structure: Rough surfaces
SEM has a large depth of field: Ability to image very rough surfaces

Environment:
SEM is conducted in a vacuum environment AFM is conducted in vacuum, gas, liquid, vapour, and in an ambient environment
Liquid cell AFM
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Although SEM and AFM appear very different , they share a number of similarities Both techniques raster a probe across the surface Similar lateral resolution Both techniques can produce artifacts AFM can provide measurements in all three dimensions, with a vertical resolution of <0.05 nm SEM has the ability to image very rough surfaces SEM and AFM are complementary techniques that provide a more complete representation of a surface when used together than if each were the only technique available
Review of Harmonic Oscillators

Summing the forces, we get the equation for damped, driven oscillators:
F = Fspring + Fdamping + Fdriving = kz = kz dx + F0 cos( t ) dt
dz + F0 cos( t ) dt
d 2z dt 2
Using expresion for quality factor:
m 0 m0 ,Q = Q
m0 dz d 2z m 2 = kz + F0 cos(t ) dt Q dt
2 0
k m
2 = 0 z
d 2z dt 2
0 dz F0 + cos( t ) Q dt m
Modeling the AFM cantilever

the cantilever is essentially a driven damped oscillator
d 2z dt 2
kc Z=0 zc S>a0 z S<a0 z
= kc z
m0 dz + F0 cos( t ) + F ( z c , z ) Q dt
F(zc,z) term inserted to account for the surface interactions. This term depends on whether or not the tip in contact with the surface (i.e., zc+z <ao) or not (zc+ z > ao)
F ( zc , z ) = F ( zc , z ) =
AR , 2 6( z c + z )
z c + z > a0
R AR 4 E R dz + ( a0 z z c ) 3 / 2 ( a0 z z c ) , z c + z a0 2 6a0 3 3 2 h dt
Modeling the AFM cantilever

d 2z dt 2 m0 dz AR 4 E R dz R + F0 cos( t ) 2 + ( a0 z z c )3 / 2 ( a0 z z c ) , Q dt h dt 6a0 3 3 2
= kc z
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Restrictions
The direct asignment of the phase contrast is hadly possible: (i) The abrupt transition from an attractive force regime to strong repulsion which acts for a short moment of the oscillation period
(ii) Localisation of the tip-sample interaction in a nanoscopic contact area (iii) The non-linear variation of both attractive forces and mechanical compliance in the repulsive regime (iv) The interdependence of the material properties (viscoelasticity, adhesion, friction) and scanning parameters (amplitude, frequency, cantilever position) The interpretation of the phase and amplitude images becomes especially intricate for viscoelastic polymers
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Afm Vs Sem

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Complementary Techniques for High Resolution Surface Investigation

SEM and AFM:

Scanning Electron Microscopy (SEM)

Principles of SEM Imaging

Scanning Electron Microscopy (SEM)

Generating the beam of electrons

Generating the beam of electrons

Detectors of the SEM

Can we see electrons directly by eye?

History Max Knoll and Ernst Ruska -1931

Cantilever Tip Sample

Three basic components: Piezoelectric scanner Cantilever with a sharp tip

Digital Instruments (DI) MultiMode Nanoscope IIIa

Position sensitive detector (PSD) coupled with a feed-back system

Historical steps of development

1981-invention of STM 1985-invention of AFM 1986-Nobel Price Christoph Gerber

Restriction: conductive samples

General components and their functions

Control of the cantilever deflection

STM Tunneling sensor (Binnig, Rohrer) tip

Optical interferometer detection system

special design of cantilever changing of resistivity with the applied stress

Piezoelectric scanner Material Properties

Poling, an intense electric field (>2000V/mm) is applied

Geometry of PZT scanner

125 m 125 m Freiburg, 06.07.2004

Slow scan speed v s = Fast scan direction

Slow scan direction

AFM Probe Construction

Three common types of AFM tip

A few requisites for cantilevers

k (C-C-H bend)~50 N/m

2. Must be insensitive to external vibrations

Minimize m L=140m, w=40m, t=1.5 m, k~0.7 N/m, ~60 kHz

Common types of cantilevers Si3N4 Si

Superposition of two geometries

Reconvolution of the tip shape I II

Deconvolution of the tip shape

AFM Tip Artifacts

AFM Tip Artifacts

Similar spheres imaged with a supposedly sharp tip

AFM Tip Artifacts

This image should only contain images of large polysterene spheres

The tip geometry can be no bigger than the obtained profile

Case 2: double tip

True three-dimensional scanning?

Method for imaging sidewalls by AFM

Martin, Wickramasinghe, Appl. Phys Lett 1994, 64, 2498

Calibration of the tip shape

Aspect ration- 10:1 Radius r~1nm

Electron beam deposition (EBD)

Carbon Nanotube Tips

Labor intensive Not amenable to mass production

Chemical Vapor deposition (CVD)

Direct grow of nanotubes

Labor intensive Not amenable to mass production

The common AFM modes

Contact mode Non-contact mode Intermittent mode

Contact mode AFM

F = kz , k = 0.01 0.1 N / m , z = 0.1nm F ~ 1 pN

Problems of the contact mode

To solve the problem