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Complementary Techniques for High Resolution Surface Investigation

Svetlana Santer

SEM and AFM:

Freiburger Materialforschungszentrum

Freiburg, 06.07.2004

Institut für Mikrosystemtechnik

Svetlana Santer



Freiburg, 06.07.2004

Svetlana Santer

Scanning Electron Microscopy (SEM)
Vacuum: 10-4-10-10 Torr

Freiburg, 06.07.2004

Svetlana Santer

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

A column which generates a beam of electrons. A specimen chamber where the electron beam interacts with the sample.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. 2. Major Components of the Scanning Electron Microscope All scanning electron microscopes consist of: 1. 4. Freiburg. A viewing system that builds an image from the detector signal. 3. 06.2004 Svetlana Santer . Detectors to monitor the different signals that result from the electron beam/sample interaction.07.

Thus. Electrons are very small and easily deflected by gas molecules in the air.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. to allow the electrons to reach the sample.2004 Svetlana Santer . 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. Freiburg. Therefore. the SEM needs a water cooling line which filters the water before it cools the oil diffusion pump. 06.07. the column is under a vacuum.

Freiburg.07.2004 Svetlana Santer . The filament is made of tungsten and is heated to generate a fine beam of electrons. If the filament is overheated or too old. it will break. As the filament gets used.Generating the beam of electrons Within the electron gun is the filament which is the source of the beam of electrons. 06. it becomes brittle and coated.

(1) secondary electron detector looks like a Faraday cage.2004 Svetlana Santer . consists of a diode with a thin gold conductor across the front surface.07. Backscattered electrons have sufficient energy to pass through the front surface and produce electron hole pairs which produce a curreent in the diode Freiburg. and detects secondary electrons. (2) backscattered electron detector (solid state detector) is located above the sample. 06.Detectors of the SEM The SEM has several detectors to view the electron signals from the sample.

Can we see electrons directly by eye? The SEM scans its electron beam line by line over the sample.07. Gradually the image is built on a TV monitor (cathode ray tube or CRT for short). It's much like using a flashlight in a dark room to scan the room from side to side. Freiburg. A slow scan is very clear and sharp . The SEM has buttons on the keyboard that control the scan you're looking at an object in a snow storm.2004 Svetlana Santer . A fast scan which takes a couple of seconds to generate an image can be very grainy .but takes a minute or two to get a picture. 06.

Sputter coater Freiburg.Sample preparation Samples have to be prepared carefully to withstand the vacuum inside the microscope. they also have to be made to conduct electricity. Because the SEM illuminates them with electrons. Biological specimens are dried in a special way that prevents them from shriveling.2004 Svetlana Santer .07. 06.

Examples Freiburg.07.2004 Svetlana Santer . 06.

2004 Svetlana Santer .07. 06.History Max Knoll and Ernst Ruska -1931 electron microscopy Freiburg.

7 nm today Freiburg.07.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. 06.2004 Svetlana Santer .

07.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 Freiburg.2004 Svetlana Santer . 06.

06.Historical steps of development •1981-invention of STM •1985-invention of AFM •1986-Nobel Price Christoph Gerber IBM‘s Zurich Research Center in Rüschlikon It Vt I t ( z ) = I 0 e −2 kz .07.2004 Svetlana Santer . k = 2mΦ / h ~ 1 Α o −1 Restriction: conductive samples Freiburg.

General components and their functions Freiburg.2004 Svetlana Santer .07. 06.

Control of the cantilever deflection Optical Lever STM Tunneling sensor (Binnig.07.2004 Svetlana Santer . 06. Rohrer) tip I V t t Optical interferometer detection system Piezoresistive detection •special design of cantilever •changing of resistivity with the applied stress Freiburg.

06.07. 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 Freiburg.2004 Svetlana Santer . Digital Instruments scanners have AC voltage ranges of +220 to –220V +V -V 0V No applied voltage Extended Contracted •In some versions.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.

06.2004 Svetlana Santer . they exhibit spontaneous polarization and deformation Perovskite-type PZT unit cell (1) in the symmetric cubic state.07. (2) distorted Poling.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. an intense electric field (>2000V/mm) is applied Freiburg.

5 µm 5 µm Svetlana Santer ∆x = K∆V .4 µm 2.4 µm 10 µm 0.4 µm 10 µm Vertical Range 0.2004 . K ~ 3nm / V 125 µm 125 µm Freiburg. 06.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 0.07.

2004 Svetlana Santer . 06.07.Triangular pattern Fast scan speed v f = 2lv Hz l ⋅ v Hz N Slow scan speed v s = Fast scan direction Slow scan direction Freiburg.

06.2004 Svetlana Santer .Feedback loop Freiburg.07.

07.2004 Svetlana Santer .AFM Probe Construction Low spring constant (k .10-2 to 102 N/m) Sharp protruding tip (r=5-50 nm) High resonance frequency 1 ω= 2π k m Three common types of AFM tip normal supertip ultralever Freiburg. 06.

06. l=4mm k (C-C stretch. w=40µm. k~0. w=1mm.5 µm.7 N/m. ~60 kHz Freiburg.07. Must be soft F = k∆z Minimize k For rectangular cantilevers Example: t=10 µm. t=1.A few requisites for cantilevers 1.)~500N/m k~1N/m k (C-C-H bend)~50 N/m 2.2004 Svetlana Santer Ex: Si or Si3N4 . Must be insensitive to external vibrations Maximize eigenfrequencies ω= k m Minimize m L=140µm.

07.2004 Svetlana Santer . 06.Common types of cantilevers Si3N4 Si Diamond Freiburg.

07.Fabrication of cantilevers Freiburg.2004 Svetlana Santer . 06.

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 Freiburg. 06.2004 Svetlana Santer ) .07.

2004 Svetlana Santer .Superposition of two geometries Freiburg. 06.07.

06.2004 Svetlana Santer .07.Reconvolution of the tip shape I II r d D=dreal D D2 d= 4r Freiburg.

06.07.Deconvolution of the tip shape Tobacco Mosaic Virus (TMV) d~18 nm r-? Freiburg.2004 Svetlana Santer .

06...2004 Svetlana Santer .AFM Tip Artifacts We start off with an example of a „good“ AFM image of 300 nm polystyrene spheres.. Freiburg..07.

2004 Svetlana Santer .AFM Tip Artifacts Similar spheres imaged with a supposedly sharp tip Freiburg.07. 06.

06.AFM Tip Artifacts This image should only contain images of large polysterene spheres Freiburg.07.2004 Svetlana Santer .

07.2004 Svetlana Santer .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 Freiburg. 06.

06.07.Blind Reconstruction Line scan having two „bumps“ What does this tell us about the shape of the tip? Case 1: Tip with single apex Freiburg.2004 Svetlana Santer .

2004 Svetlana Santer . 06.Case 2: double tip Freiburg.07.

06.2004 Svetlana Santer .07. No matter how sharp the tip. „Petticoat“ effect-all images of objects having steep walls or undercut regions appear to have flared sides Freiburg.True three-dimensional scanning? One of the drawbacks of typical AFM is that the images obtained are not truely threedimentional. the data collected can never access the underside of the sample.

07. Phys Lett 1994. 64. Wickramasinghe. 2498 Can we get a similar image using a typical AFM and the boot-shaped tip? No! Freiburg.2004 Svetlana Santer .Method for imaging sidewalls by AFM Martin. Appl. 06.

06.Calibration of the tip shape 2r L L 2 h L R= 4r L2 R= 2h Freiburg.07.2004 Svetlana Santer .

10:1 •Radius r~1nm Freiburg.Oxide-Sharpened Tips increasing aspect ratio reducing tip radius SiO2 HF etching •Aspect ration. 06.07.2004 Svetlana Santer .

06.07.Electron beam deposition (EBD) High-aspect-ratio tips L=(1-5)µm R=(20-40)nm Carbon materials are deposed by the dissociation of background gases in the SEM vacuum chamber Freiburg.2004 Svetlana Santer .

07.2004 Svetlana Santer . 06. 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 Freiburg. d=(0.Carbon Nanotube Tips •Single-walled carbon nanotubes (SWNT).7-3)nm •Multiwalled carbon nanotubes (MWNT) (nested. concentrically arranged SWNT.

06.9nm d=2.8nm Freiburg.2004 Svetlana Santer .Pick-up Tips d=0.07.

07. 06.5 nm) •Presipitates carbon nucleates a grow of nanotube Freiburg.2004 Svetlana Santer .Chemical Vapor deposition (CVD) Direct grow nanotubes onto AFM tip •Heating of nanocatalyst particle (r~3.

06.2004 Svetlana Santer .Direct grow of nanotubes Alumina/iron/molybdenumpowdered catalyst •2 nm in diameter •2µm in length Labor intensive Not amenable to mass production Freiburg.07.

2004 Svetlana Santer .Modes of operation Freiburg. 06.07.

2004 Svetlana Santer . 06.The common AFM modes contact mode tapping mode Contact mode Non-contact mode Intermittent mode Freiburg.07.

1 nN or less) in liquid Freiburg.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 (0.07. 06.2004 Svetlana Santer .

Force curve Freiburg.07.2004 Svetlana Santer . 06.

Contact mode Force Static mode Dynamic mode F = kz . z B C D A ∂F > k.01 ÷ 0. z = 0. k = 0. ∂z at " B" is jump into a contact to " C" Oscillation amplitude Freiburg.2004 Svetlana Santer .07.1 N / m .1nm F ~ 1 pN Probe-sample distance. 06.

Problems of the contact mode Large deformation forces ~ 100 nN Capillary forces Fcap = 4πRγ1 cos θ ~ 22nN To solve the problem operation in liquid Elimination of capillary forces Reduction of van der Waals forces Freiburg.2004 Svetlana Santer . 06.07.

8 m / sec 2 Fg ≈ 10−9 nN (a) FvdW = A⋅ r 6D 2 A = 10−19 J = 4πr ⋅ γ F adh γ = 2 γ γ 1/ 2 ( s p ) D = 0. the typical contact radius Fd = R Freiburg.07.Different types of forces relevant to AFM 4 3 πr ρg 3 ρ ≈ 1 g / cm3 r = 25 nm Fg = mg = g = 9. 06.2004 Svetlana Santer . a ~ 5 nm.3 nm r = 25 nm γ s = 100 mJ/m 2 silica surface energy γ = 25 mJ/m 2 p FvdW ~ 5 nN polymer surface energy Fadh ~ 30 nN (b) Capillary forces (d) Deformation forces Fcap = 4πRγ1 cos θ ~ 22nN Ka 3 ~ 6nN .

07.Problems of the contact mode Large lateral (shear) forces ~ 100 nN To solve the problem non-contact mode Freiburg.2004 Svetlana Santer . 06.

2004 Svetlana Santer .07. 06.Problems of the contact mode Freiburg.

06.Non-contact Mode AFM Highly unstable mode Ultra high vacuum at low temperature Freiburg.07.2004 Svetlana Santer .

2004 Svetlana Santer .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 Freiburg. 06.07.

07.2004 Svetlana Santer .Tapping mode AFM ω0 ≈ 50 ÷ 500kHz A0 ≈ 10 ÷ 100nm Freiburg. 06.

2004 Svetlana Santer .Tapping mode AFM Force Static mode Dynamic mode Probe-sample distance. 06.07. z B C D A Oscillation amplitude Freiburg.

2004 Svetlana Santer .7 ≤ rsp ≤ 1 rsp = Asp A0 (ii) Moderate tapping 0.3 ≤ rsp ≤ 0.Tapping mode AFM Three regimes of tapping mode: (i) Light tapping 0.07. 06.7 (iii) Hard tapping 0.01 ≤ rsp ≤ 0.3 Freiburg.

06.07.Tapping mode AFM Phase Imaging Driven force Actual responce Different characteristics of the sample different offset the phase Freiburg.2004 Svetlana Santer .

Freiburg.07. 06.2004 Svetlana Santer .

2004 Svetlana Santer . 06.07.Freiburg.

2004 Svetlana Santer . 06.07.Examples of Phase Images AFM Freiburg.

07. 06.2004 Svetlana Santer .Freiburg.

06.07.2004 Svetlana Santer .Freiburg.

biological samples.07.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. 06.2004 Svetlana Santer .e. polymers) due to scraping Freiburg.

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 Freiburg. 06.2004 Svetlana Santer .07.

06.07.2004 Svetlana Santer .01 ÷ 1 N / m k ~ 50 N / m Freiburg.Cantilevers used in contact and tapping modes k − 0.

07. 06.2004 Svetlana Santer .Contact vs Tapping modes Freiburg.

06.07.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 Freiburg.2004 Svetlana Santer .

06.07. RMS=0.14 nm monoatomic steps on epitaxial silicon deposited on (100) Si.2004 Svetlana Santer .07 nm Freiburg. the SEM has difficulty resolving these features due to the subtle variations in height TM-AFM image of 0. 1 µm scan.Comparison of Techniques: AFM vs SEM Surface structure: •atomically smooth surfaces On a sample this smooth.

Comparison of Techniques: AFM vs SEM
Surface structure: •Thin films

On most thin films, the SEM and AFM produce a similar representation of the sample surface

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

Comparison of Techniques: AFM vs SEM
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

Comparison of Techniques: AFM vs SEM
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
Freiburg, 06.07.2004

Svetlana Santer

Comparison of Techniques: AFM vs SEM
Surface structure: •Rough surfaces

SEM has a large depth of field: Ability to image very rough surfaces
Freiburg, 06.07.2004 Svetlana Santer

liquid. 06. and in an ambient environment Liquid cell AFM Freiburg.Comparison of Techniques: AFM vs SEM Environment: SEM is conducted in a vacuum environment AFM is conducted in vacuum. vapour.2004 Svetlana Santer . gas.07.

Comparison of Techniques: AFM vs SEM Although SEM and AFM appear very different . 06. 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.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 Freiburg.07. with a vertical resolution of <0.2004 Svetlana Santer .

07. driven oscillators: ∑ m F = Fspring + Fdamping + Fdriving = − kz − γ = − kz − γ dx + F0 cos( ωt ) dt dz + F0 cos( ωt ) dt d 2z dt 2 Using expresion for quality factor: γ= mω 0 mω0 .2004 Svetlana Santer . we get the equation for damped.Review of Harmonic Oscillators Summing the forces.Q = γ Q mω0 dz d 2z m 2 = − kz − + F0 cos(ωt ) dt Q dt 2 ω0 ≡ k m 2 = − ω0 z − d 2z dt 2 ω0 dz F0 + cos( ωt ) Q dt m Freiburg. 06.

z ) = − AR . 2 6( z c + z ) z c + z > a0 πηR AR 4 E R dz + ( a0 − z − z c ) 3 / 2 − ( a0 − z − z c ) . z ) Q dt F(zc. zc+z <ao) or not (zc+ z > ao) F ( zc .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 m = −kc z − mω0 dz + F0 cos( ωt ) + F ( z c .e.z) term inserted to account for the surface interactions.2004 Svetlana Santer .07. z ) = − F ( zc . z c + z ≤ a0 2 6a0 3 − 3ν 2 h dt Freiburg.. This term depends on whether or not the tip in contact with the surface (i. 06.

06.Modeling the AFM cantilever d 2z dt 2 mω0 dz AR 4 E R dz πηR + F0 cos( ωt ) − 2 + ( a0 − z − z c )3 / 2 − ( a0 − z − z c ) .2004 Svetlana Santer .07. Q dt h dt 6a0 3 − 3ν 2 m = − kc z − Freiburg.

frequency. 06.07.2004 Svetlana Santer . friction) and scanning parameters (amplitude.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. cantilever position) The interpretation of the phase and amplitude images becomes especially intricate for viscoelastic polymers Freiburg. adhesion.