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4. Cantilever Sensors
5. Future Aspects
5.1. multi-dimensional Scanning Force Microscopy
5.2. Scanning Chemical Force Microscopy
3.5.1. Scanning Chemical Force Microscopy with X-rays
3.5.2. Scanning Chemical Force Microscopy with ToF-SIMS
5.3. Scanning Vector Magnetometry
5.4. Magnetic Resonance Force Microscopy, 3d Imaging of Viruses
1.
General Introduction to
Scanning Probe Microscopy.
• The starting point of SPM was the invention of the scanning tunneling microscope
(STM) by G. Binnig and H. Rohrer in 1982 [1,2] (Nobel prize in physics in 1986).
• The first and most important extension of the STM was the scanning force
microscope (SFM) or atomic force microscope (AFM), invented in 1986 by
Binnig, Quate, and Gerber [3].
• Most of the present scanning probe instrumentation is based on the AFM often
combined with other techniques mapping/controlling properties not accessible
by AFM.
Refs.: [1] G. Binnig and H. Rohrer et al. Helv. Phys. Acta 55, 726 (1982)
[2] G. Binnig and H. Rohrer et al. Phys. Rev. Lett. 50, 120 (1983)
[3] G. Binnig, C.F: Quate, CH. Gerber, Phys. Rev. Lett. 56, 930 (1986)
see also R. Wiesendanger and H.-J. Güntherodt, Vols. 20, 28, 29
Springer Series in Surface Science 1992, 1993, 1994 R. Colton et al., Wiley-VCM, Weinheim 1998
Basic Concepts of an STM
Basic setup of an STM (but • tip-sample stability < 1pm in best instruments
also any other type of SPM) ➜ stiff, high resonance frequency instrument
➜ vibration isolation system
• tip can be scanned in x,y, z (tip-sample distance)
with pm precision
➜ piezo electric scanners
• tip-sample interaction (tunnel current)
is measured
➜ current amplifier for 1pA needed
➜ log I is used for the feedback
• PI-feedback adjusts z to keep log I constant
➜ maximum feedback speed depends on
resonance frequency of instrument and
bandwidth of current amplifier
• Computer controlled electronics is used for
scan-generation, feeback, data recording,
displaying and user GUI
• in other types of SPM other tip-surface
interactions are used to control the tip-sample
distance
In an STM typically two signals are acquired, namely the z-coordinate (topography)
and the tunneling current, or more generally the measured tip sample interaction (error signal)
Vibration Isolation
Ref.: O. Züger, H.P. Ott, and U. Dürig, Rev. Sci. Instrum. 63 (1992) 5634
One & Two Stage Vibration Isolation
olation
n is
ibratio
a ge v
1-st
Only the double vibration isolation stage can provide sufficient isolation @ the
resonance frequency of the microscope. Assume floor vibrations of 100nm (1000Hz).
Then the tip-sample vibration will be less than 10-3nm !
Piezo Electric Actuators
Since the piezo effect exhibited by natural materials (e.g. quartz) is very small, polycrystalline ferroelectric
ceramic materials such as barium titanate and lead zirconate titanate (PZT) with improved properties (e.g.
PZT-5H: d31=-2.62Å/V) have been developed. These ferroelectric ceramics become piezoelectric when
poled.
E
E eletric field, L lengths, ΔL change in length
d31 transversal piezoelectric coefficient
L
Slip-Stick Piezomotoren
Mechanical Challenges Principle stick-slip piezo motor
SPM
signal
sensor
tip
setpoint
+ -
sample
z-piezo
signal
correction
signal
Feedback Setup:
1. experience / trial & error
2. Ziegler-Nichols procedure [1,2]:
- increase P-part until small oscillations of the current are observed.
- reduce P-part to 0.45Pkrit.
- measure oscillation period (Tkrit) and set I-part to 0.85Tkrit.
[1] J. Ziegler, N. Nichols: Trans. ASME 64, 759 (1942)
[2] H. Unbehauen: Regelungstechnik I (Friedr. Vieweg und Sohn, Braunschweig/ Wiesbaden, 1982)
Feedback - Signal and Error Signal
Si(111)-7x7, 10x10nm2
sample tip
where the barrier height Φ is in eV and z in
Angstrom. With a typical barrier height of Φ =
5eV , which corresponds to the work function of
gold, the tunneling current decays by an order
of magnitude when the vacuum gap is
changed by 0.1nm !
Refs.: Theoretical: Frenkel: Phys. Rev. B 36, 1604 (1930) & Bardeen, J. PRL, vol. 6, no.2, pp.57-59, 1961
First experiments: R. Young, J. Ward, F. Scire: Phys. Rev. Lett. 27, 922 (1971)
First experiments: R. Young, J. Ward, F. Scire: Rev. Sci. Instr. 43(7), 999–1011 (1972)
First clear demonstration of vacuum tunneling: G. Binnig, H. Rohrer: Appl. Phys. Lett. 40, 178 (1982)
Tunneling: a quantum mechanical effect
sample tip sample & tip @ close distance
Uc
vacuum level t
s t s
Fermi level
z
applying a bias
electrons tunnel
Ub
• from sample to tip
t
(or vice versa if -Ub is applied)
s • out of filled states
• into empty states
tunnel current depends on
• distance z
• overlap of wave functions
z • density of filled and empty states
• ... „sligthly“ on temperature
Bardeen‘s tunnel current formalism [1]
Based on Bardeen, the tunneling current between two electrodes, separated by an insulator, is given by
Fermi function
ρs, ρt are the density of states of sample and tip. The tunneling matrix element M is given by
where ψt, ψt are the wave functions of the sample and of the tip. For low voltages the integral simplifies to
we obtain
Si(111)-7x7, 10x10nm2
reference
Ref phase
x low pass
filter
y
after multiplying:
First Si(111) 7x7 image [1] First Si(100) 2x1 [2] and
STM @ various tip-sample potentials an GaAs
Ga As
Us = +1.9V Us = -1.9V
STM images of the Cu(111) surface in constant current mode. (left) Overview image with monatomic steps
(right) Atomic resolution on Cu(111). The spacing between the protrusions is 2.5Å.
The best resolution was observed with small tunnel resistances of (50-300kOhms), which was
attributed to the interaction between adsorbates at the tunneling tip and the surface atoms.
D. Eigler (IBM Almaden Research Lab) calls these adsorbates “Behm amplifiers”. He often uses a
Xe-atom that is picked up by the tip. Such adsorbates are only weakly bound to the tip. The strong
force field between the tip and the sample leads to a modulation of the position of the adsorbate
within the tip-sample gap. This causes an enhancement of the corrugation and superresolution.
Forces between tip and sample were attributed to play an important role [1].
Scanning tunneling spectroscopy (STS) experiments are important to determine properties, such
as
• LDOS (density of states): vary voltage U
• barrier heights, vary distance z:
There exist a variety of spectroscopic modes, variation of one externally adjustable parameter
and measurement of tunneling current:
• voltage I(V) or dI/dV (often measured with lock-in amplifier)
• z-distance I(z), dI/dz (often measured with lock-in amplifier)
These curves can be either measured at a fixed lateral position or at various lateral positions
(xi,yi). A simple way to get spectroscopic information is to acquire several images at different
voltages or distances. Because of thermal drift this way is not ideal, but feasible. Alternatively, the
tip can be stopped at different positions (xi,yi), the voltage or distance is ramped, and then the tip
moves to the next position. In an ideal STS-experiment the tip DOS should be neglectable, which
seems to be not always the case.
a) Right hand side: Experimental STM image with atomic resolution of three single walled
carbon nanotubes (SWNT) with different chiralities. Left hand side: Atomic model
representation of the three SWNTs.
b) Ball-and-Stick model of a hydrogen chemisorption and a vacancy type defect on a (10,0)
semiconducting SWNT.
c) Upper panel: STM topography image of a (11,1) SWNT with two hydrogen-plasma induced
defect sites. Lower panel: Corresponding scanning tunneling spectroscopy (STS) line scan on
the dashed horizontal line in the topography image showing the band gap of the SWNT and
localized (spatially as well as energetically) states of the defect sites. The paired gap states of
the right defect is characteristic of a chemisorbed hydrogen-dimer [1,2].
2 ML of Fe on W(110) crystal
Refs.: [1] M. Bode, et al. PRL81 4256 (1998) A. Kubetzka, et al. PRL88 057201 (2002)
[2] A. Kubetzka, et al. PRL88 057201 (2002)
[3] S. Heinze et. al. Science 288 1805 (2000) and A. Wachowiak,Science 298 577 (2002)
Note: other SPT-methods described in Meyer, Hug, Bennewitz „Scanning Probe Microscopy“ Springer ISBN 3-540-43180-2 (2004)
SP-STM: Revealing Magnetic Interactions from Single-Atom
Magnetization Curves
STM topograph colored with spin-pol. dI/dV map
Individual Co adatoms on the Pt(111) surface (blue) (A and B) Topographs of an area with several adatoms
and Co ML stripes (red and yellow) attached to the colorized with the spin-pol. dI/dV map at B = −0.5 T
step edges An external B can be applied perp. to parallel to the tip magnetization MT (A)
the sample surface to change the magnetization of and B = +0.5 T antiparallel to MT (B) (T = 0.3 K).
adatoms M, ML stripes M, or tip MT at different T. (C) M(B) curves from the same adatom taken at different
The ML appears red when M ML is parallel to MT temperatures as indicated (dots). Reversal of MT is
and yellow when M ML is antiparallel to MT. corrected. (D) Magnetization curves of four adatoms at
(Tunneling parameters are as follows: I = 0.8 nA, V = 0.3 K with fit curves and resulting Bsat of 99% saturation.
0.3 V, modulation voltage Vmod = 20 mV, T = 0.3 K.)
action spectroscopy:
Here:
vibronic and electronic
excitation
stick-slip motion
(pulling)
stick-slip motion
(pulling)
continuous motion
(pulling)
stick-slip motion
(pushing)
Ref.: [1] L. Bartels et al., Phys. Rev. Lett. 79, 697 (1997)
STM Manipulation of single Fe-Atoms on Cu(111)
• more complex than STM, but more versatile and a much higher challenge, so more fun ... but STM can still be done!
Cantilever modeled as driven damped oscillator
Amplitude of Cantilever Phase Loss of Cantilever relative to Excitation
0∘
on resonance the
cantilever lags
-90∘ 90o behind the
excitation
-180∘
Example of Measurement Physics: Dynamic Operation
cantilever resonance low Q, wide resonance: lock-in amplifier
in air
-> low quality factor of cantilever
-> excitation with fixed frequency
-> lock-in amplifier
in vacuum
-> high quality factor
-> excitation on resonance
-> requires phase locked loop
57
AFM - SFM - or? - Possible Classification Schemes
1. operation mode bases schemes
measured cantilever property per imaged xy (z, other parameter) point:
a) Static Modes: (dc) deflection (flexural or torsional) of cantilever
b) Dynamic Modes: dynamic cantilever properties
i. oscillation amplitude, phase
ii. required drive amplitude, frequency shift
iii. overtones (harmonic & non-harmonic), intermodulation products
single cristalline silicon cantilevers high-aspect ratio tips ultrasharp tip tuning fork sensor
radius
>10µm < 3nm
general solution
dispersion relation
and
with
Rabe, Rev. Sci. Instrum., 67 (1996) 3281 & Refs. therein 62
Cantilever, a mass-loaded beam - Flexural theory - Results
solutions for non-harmonic resonances
static
At higher frequencies the probability for the excitation of torsional modes increases compared to that of the flexural
modes, because the former are spaced equidistantly while the spacing of the latter increases.
torsional spring constant (for static (friction) measurements with tip-sample contact
= 16,3590 N/m
excellent agreement
fT1 f4
excellent agreement
\omega _n ^2
\Gamma _n =
with and dissipation term [kg/s]
with flat thermal noise spectrum that is related to the thermally excited cantilever amplitude as
For a measurement bandwidth B, this spectral density gives a minimum detectable force of
note: make sure that the native Qn is used here. Any quality factor that is changed with a non-stochastic feedback drive
circuitry must NOT be used !
Q-control does NOT change Fmin, n . Be aware of interferometer-induced cantilever heating/cooling phenomena
derived from D. Rugar et al., Appl. Phys. A 72 (2001) 3 note: this is what the PLL should be capable of doing
Thermal noise of cantilevers for the nth mode
For a measurement bandwidth B, this spectral density gives a minimum detectable force of
F_{min,\,n}
derived from D. Rugar et al., Appl. Phys. A 72 (2001) 3, Grütter et al., Appl. Phys. Lett. 71 (1997) 279
Most force sensitive cantilevers
using and
we find
• Qmount : energy dissipated through the mounting of the cantilever in the force microscope
• Qair : energy dissipated by viscous damping of oscillating cantilever
use vacuum
• Qsupport : energy dissipated from cantilever to support chip of cantilever
do not use too hard and too short cantilevers or torsional oscillators, do not coat across support
• QTED : energy loss by thermoelastic damping
• Qsurface : energy dissipated by cantilever surface losses
do not coat surface, be careful with reflective coatings
bake cantilevers in UHV @ 150C to remove H2O
bake cantilevers in UHV @ 800C to remove oxide or perform HF etch
• Qvol : energy dissipated in cantilever inside, can be neglected for single crystalline cantilevers
Thermoelastic loss: Any bending of the cantilever is with very low T & thin is better
related to temperature changes, and an irreversible
flow of heat driven by the generated temperature
gradients gives rise to TED. or with
See Lifshitz Phys. Rev. B61 (2000) 5600
Support loss: see Yasumura et al, J. small w and no additional coating is better
Microelectromech. Syst. 9 (2000 ) 117
thickness of surface layer property of surface layer
as sensitive as best
NEMS
Q can be increased
by more than 10, if
surface loss is
removed !
100‘000 0.32
Q up to 100‘000 at LT
sensitivity 2 x increased
• conventional cantilevers used for atomic resolution are 40 times more sensitive than tuning forks, but they
need to be operated under similar conditions!
• a cantilever with a similar stiffness is still 10 times more sensitive, and again 40 times more sensitive after
annealing.
However: tuning forks are successfully used for true atomic resolution imaging
3.1.2. Deflection Sensors
Deflection Sensors
A laser beam is reflected off the rear side of the cantilever. Angular deflections of the laser beam are measured
with a position sensitive detector (4-quadrant photo diode). The A-B-signal is proportional to the
normal force and the C-D-signal is proportional to the torsional force.
Beam Deflection Principle
A laser beam is reflected off the rear side of the cantilever. Angular deflections of the laser beam are measured
with a position sensitive detector (4-quadrant photo diode). The A-B-signal is proportional to the
normal force and the C-D-signal is proportional to the torsional force.
Interferometer Optical Deflection Sensor
interferometer inside force microscope
2x2 coupler
4% reflection
@ fiber end
foto foto &
diode diode reflection
@ cantilever
amplifier amplifier
cantilever
signal reference signal
Inside the SFM only limited space is required. The fiber-cantilever distance is around 10um. A highly stable
laser power supply, stable (optically isolated) monomode laser diodes and temperature stabilization of the
laser is required to obtain maximal sensitivity. The fiber can usually be adjusted relative to the cantilever in
order to work at the point of maximum sensitivity.
Ref.: D. Rugar, H. Mamin, P. G¨uthner: Appl. Phys. Lett. 55, 2588 (1989)
A. Moser, H. J. Hug, Th. Jung, U. D. Schwarz, and H.-J. Güntherodt, Meas. Sci. Technol. 4, 769-775 (1993).
Interferometer Optical Deflection Sensor
inside force microscope
4% reflection
@ fiber end
&
reflection
@ cantilever
λ/2
cantilever
Note:
• WP1 and WP2 are the most sensitive operation points
• the w-Piezo (piezo to control fiber-to-cantilever distance) is used to move fiber to one of
these operation points
• then a feedback keeps fiber at this position
• small cantilever deflections can now be detected
Ref.: D. Rugar, H. Mamin, P. G¨uthner: Appl. Phys. Lett. 55, 2588 (1989)
A. Moser, H. J. Hug, Th. Jung, U. D. Schwarz, and H.-J. Güntherodt, Meas. Sci. Technol. 4, 769-775 (1993).
3.1.3. relevant Forces
Relevant Forces tip
> 1nm
forces in liquids:
• hydrophobic / hydrophilic forces
• steric forces
sample
• solvation forces
tip
sample
• When the tip is in contact with the sample, a large, repulsive tip-sample force may
occur to the tip apex due to the possibly large long-ranged attractice forces !!!
• So zero cantilever deflection does not mean that the tip apex force is zero !!!
Refs.:
J. Israelachvili
Intermolecular and Surface Forces with Applications to Colloidal and Biological Systems, Academic Press (1985)
D. Tabor
Gases, liquids and solids, Cambridge University Press (1979)
Short-Range Forces
• due to overlap of electron wave functions and from the repulsion of the ion cores.
• can be both attractive:
• attractive when the overlap of electron waves reduces the total energy.
These situations are comparable to molecular binding.
• around 0.5 - 1 nN per interacting atom at tip-sample distances typical for STM operation.
• decay length of the order of atomic units, i.e. 0.05 nm for metallic adhesion, but around
0.2 nm for covalent bonding.
• true atomic resolution AFM operates with these forces
• or repulsive:
• repulsive when strong electron wave overlap (Pauli exclusion principle). These forces are
directly connected to the total electron density.
• The ionic repulsion acts for small distances, where the screening of the ion cores by the
electrons falls away.
• usual contact AFM operates with these forces.
• Model potentials like the Lennard-Jones or the Morse potential are used to describe the
short-range forces.
Because the range of van der Waals forces is limited, the tip-sample geometry of the force
microscope can be well approximated as a sphere approaching a semi-infinite body. For this
configuration, the van der Waals force is
where H denotes the Hamaker constant, R the tip radius, and D the distance between tip and
sample surface.
• The value of the Hamaker constant H is of the order of 10-19 J. For materials with high dielectric
constant like metals it is about a factor of ten higher than for insulators.
• For a tip of radius R = 30 nm, the van der Waals force in vacuum at a distance of D = 0.5 nm is
of the order of FvdW = 2 nN.
• The van der Waals force can also be determined for more complex tip-sample geometries like a
half-sphere at the end of a truncated cone.
Van der Waals Forces
• are attractive in vacuum and in most cases
• Lifshits theory predicts that the force is proportional to (ε1-ε3)(ε2-ε3) and (n12-n32)(n22- n23),
where ε and n are dielectric constant and refractive index of tip (1), sample (2), and medium (3) in
between.
• medium with ε and n close to the respective values of tip and sample will greatly reduce van der
Waals forces.
• immersing liquid can lead to a negative Hamaker constant and to repulsive van der Waals forces.
• repulsive van der Waals Forces in liquids are used to stabilize suspensions of (nano)particles
• repulsive van der Waals Forces have also been used for the first AFM experiments showing true
atomic resolution [1]
where Ubias is the bias voltage and Ucpd is the contact potential difference due to different
work functions.
• zero bias voltage normally does not correspond to a minimal electrostatic force but that the
contact potential difference has to be compensated.
• the work function is very sensitive to perturbations at of the surface. The irregular shape of a
the tip gives rise to patch charges, which can not be completely compensated by a bias
voltage.
• For tip radius R = 20 nm at a tip-sample distance of z = 0.5 nm and Ubias - Ucpd = 1 V the
electrostatic force is about Fel = 0.5 nN.
Contact Potential
Band alignment under zero sample bias.
Ucpd
The Fermi levels match, no net tunnel or
contact current is flowing.
Quadratic dependence of measured force (or here frequency shift) on tip-sample bias
Magnetic Forces
• The forces that act on magnetic dipoles located in a magnetic field are called magnetic forces.
• In force microscopy experiments the magnetic dipoles are usually contained in the ferromagnetic
material on/of the tip of the cantilever and the magnetic sample.
• A field is produced by a ferromagnetic sample or a current distribution located in close proximity
of the tip. The current distribution may be the one of a current carrying device or be present in a
superconductor.
• The force on the tip is then given by the derivative of the magnetostatic energy.
• Note that the z-derivative of the stray field is inside the integral expression. Thus when the inte-
gration is performed along a long slab like tip (see figure), the integration along the z-axis will
lead to an expression for the force that is proportional to
the stray field times the magnetic charge at the lower tip
end (plus the stray field times the magnetic charge at the upper tip end – however for a long
tip this part can be neglected).
Attention:
• the magnetic force is rather proportional to the stray field (and NOT to the derivative
• of the stray field as documented in many
• manuals of SPMs and publications !!!)
Capillary Forces
• microcontacts act as nuclei of condensation.
• In air, water vapor plays the dominant role.
• If the radius of curvature of the microcontact is below a certain critical radius (approximately
equal to the Kelvin radius) a meniscus will be formed.
• The Kelvin radius is given by
where γ is the surface tension, R the gas constant, T the temperature, V the molar volume and pS
the saturation vapor pressure.
• The surface tension of water is γ = 0.074 N/m at T = 20 C which gives the parameter γV/RT =
0.54 nm. Therefore we obtain for p/ps = 0.9 a Kelvin radius of 100 nm.
• In Scanning Force Microscopy, typical tips having radii of less than 100 nm are possible nuclei of
condensation. If a meniscus is formed an additional capillary force acts on the tip. A simple
estimation is given by:
• where R is the radius of curvature, Θ the contact angle, D the distance between tip and sample
and φ the angle of the meniscus. The maximum force is given by Fmax =4πRγ cosΘ .
• For a tip radius of 100 nm we obtain a force Fmax=9.3·10-8N, which is significantly stronger than
the corresponding van der Waals force.
• Typical force vs. distance curves in ambient conditions reveal forces of the order of 10-8-10-7N,
which mainly originates from capillary forces.
• These adhesion forces limit the minimum force which acts on the outermost tip region, and have
to be equilibrated by the repulsive force in this small contact region. Consequently, capillary
forces can determine the size of the contact and play an essential role in force microscopy
measurements in air.
Capillary forces
Fmax = 4 π R γ cos(Θ)
R
γ (H2O) = 0.074N/m R=100nm
Contact angle foir hydrophilic surfaces Θ ≈ 0°
⇒ Fmax = 90nN
3.2. Contact Mode
Scanning Force Microscopy
3.2.1. Principles of SFM in Contact
Snap to Contact
critical tip-sample distance tip in contact with sample multi-atom tip-sample
contact
tip
tip
tip
snap-in
Contact Radius:
• in atmosphere: 2-10nm @ 1nN < F < 100nN
• in UHV: 1-4nm @ 0.1nN < F < 10nN
Force versus Distance Curves
92
Unzipping Bacteriorhodopsin
1nm
3.2.2. Examples of Dynamic Force Microscopy
with Tip in Contact
Force Modulation Scanning Force Microscopy
Lock-in In-phase
Frequency Oscillation Ref Amplifier
Generator
Laser
Normal Lock-in In-phase
Deflection Ref Amplifier
Cantilever
Topography
Sample
x
Scan
Generator y Feedback z
Scanner Setpoint Control
3.2.3. Scanning Friction Force Microscopy
Friction Contrast
Circular areas of
hydrocarbon molecules
are surrounded by
fluorocarbon molecules.
Within the hydrocarbon
islands, material has
been removed by the
action of the tip (low
scanning velocity, high
load).
Experiment Theory
Ref.: A. Socoliuc, R. Bennewitz, E. Gnecco and E. Meyer, Phys. Rev. Lett. 92, 134301 (2004)
Controlling Friction by Actuation of
Nanometer-Sized Contacts
A. Socoliuc, E. Gnecco, S. Maier, O. Pfeiffer, A. Baratoff, R. Bennewitz, E. Meyer, Science 313, 207 (2006)
3.3. Intermittent Contact Mode
and Peak Force Microscopy
Advantages of the Intermittent Contact Mode
but: • the cantilever oscillation can be strongly non-harmonic, i.e. bent resonance
curves with instabilities
• stable operation is obtained at high amplitudes and with hard cantilevers
• but the highest phase contast is obtained close to the critical points
Intermittant Contact Mode
Tapping Mode Phase reveals Local Stiffness
Peak Force Tapping – Force Monitor
• Force curves are displayed in the Force Monitor and are useful for monitoring feedback conditions.
• The Vertical axis displays the Vertical Deflection data from the photo detector. The axis is labeled
Force and the units are always in Volts for ScanAsyst.
Pull-off ringing
• Every tap on the surface produces additionally a force curve, which is extracted
• Force-curves are acquired more than 1000x faster than in standard force distance spectroscopy
Z Drive (~2KHz)
Derjaguin-Muller-Toporov (DMT) model and E1,E2 are the elastic moduli and ν1,ν2 the Poisson's ratios associated with each
body.
in contact:
Hertz Theory
New Applications – Li Battery
Tip
Z Z
Sample Sample
• With the same tip sample distance, van der Waals forces increase a lot due to the
contribution from the side wall
• Capillary force also proportional to effective tip radius and can be 10-20 times larger
inside the trench
Real Advantages
Deep (~65 nm), narrow (~50 nm) trenches are difficult to image with TappingMode due to
excessive damping of the probe oscillation. But here ScanAsyst easily reaches the bottom
of the trenches. Scan size 1 µm on a Dimension Icon.
3.4. non-contact AFM (ncAFM)
or Dynamic Force Microscopy (DFM)
3.4.1. Principles and Instrumentation
Principle of Dynamic Force Microscopy
with Atomic Resolution
feedback system
FM Detection:
T.R. Albrecht et al., J. Appl. Phys. 69, 668 (1991)
minimal describe an FM demondulation technique for
tip-sample fast measurement of frequency shift.
distance:
tip U. Dürig et al., J. Appl. Phys. 82, 3641 (1997),
Incipient 0.2 - 1nm Ch. Loppacher et al., Appl. Phys. A66, 215 (1998)
chemical - adjust frequency of oscillation circuit to keep
bond phase between excitation and cantilever oscillation
constant (phase locked loop)
- keep cantilever oscillation amplitude constant, i.e.
cantilever excitation signal is proportional to
surface of sample energy dissipation
- conservative and non-conservative interactions
can be separated
frequency shift, ∆f
Modeling dynamic AFM
q(t) q‘(t)
with
with d+2A A
cantilever
d -A
which is justified for larger A, because d
0
sample
for A = 5nm
For small amplitudes, the frequency shift is a very simple function of the tip-sample forces:
• it is proportional to the tip-sample force gradient kts .
• for large amplitudes, the frequency shift is given by the rather complicated equations (see above).
• with integration by parts, the complicated formula transform into a very simple expression
with
with
relevant issues
• large amplitudes reduce <kts>; cantilever does not snap
• large amplitudes reduce signal, but improve noise
• large amplitudes suppresses non-harmonic terms and
higher harmonics
• large A:
Thermal noise
Example:
Absolute
value
of
resolution
depends
on: k=2000N/m,
f0=
1.6MHz,
Q=100
000
probe
specifications
(f0,
k,
Q)
Ath=
1440fm
@300K
Ath=
170fm
@4.2K
detector
sensitivity
Required
sensitivity
of
detector
@1kHz
BW:
Anoise<
50fm
@300K
Anoise<
6fm
@4.2K
1nm
measurement parameters
∆f = -31Hz, scan speed 0.6nm/s
Cantilever: cL = 28.6 N/m, 200
150
z [pm]
f0 = 155 719.3 Hz, Q = 370‘000
temperature: 7.2K 100
50
0
0 1 2 3 4 5
cross section [nm]
M. A. Lantz and H.J. Hug et al., Phys. Rev. Lett. 84, 2642 (2000)
K. D. Brommer, et al., Phys. Rev. Lett. 68, 1355 (1992) &
I. Stich, et al., Phys. Rev. Lett. 68, 1351 (1992).
Site Specific Forces
0
0
frequency shift. [Hz]
@ Corner
Hole vdW force
force [nN]
-40
-1
short-range force
@ Adatom -2
-80 total force
-3
2 4 6 8 10 12 14 2 4 6 8 10 12 14
tip-sample distance [Å] tip-sample distance [Å]
[1] U. Dürig, APL. 75, 433 (1999) and APL 76, 1203 (2000) and other inversion methods ...
[2] Lantz and Hug et al., Science 291, 2580 (2001)
ncAFM and Atom Manipulation
Vertical atom manipulation Dissipation
Oyabu et al., PRL 90, 176102-1 (2003) Oyabu et al., PRL 96, 106101 (2006)
Vdc=0 if Ucpd=Utip-sample
Error of
Kelvin
Frequency Oscillation Ref Signal
Generator Lock-in Feedback z
In more sophisticated setups the input
Amplifier Control Contact
of the Kelvin Lock-in can be driven by:
- the frequency shift signal Potential
Setpoint = 0 or Kelvin
- by the phase Normal
- etc Signal
Deflection
ac-Signal
Ucpd
Normal
Deflection
Laser „dc“-Signal
-
Utip-sample
Summation Cantilever
+
Sample Feedback z
Control Topography
Setpoint
x
Scanner
Scan
y
Generator
Surface Potential on a CD-RW
Environments
→ ambient air, vacuum, UHV
→ various temperatures & magnetic fields
Resolution:
white domains
with 10nm diameter
are visible.
Improved tips
can go below 10nm.
1µm
200nm 1µm
200nm 1µm
200nm
MFM Image Formation ➜ Transfer-Function Theory
• The force on the MFM tip at position frequency shift proportional to force derivative:
>10µm radius +
< 3nm +
+
qtip
+
++
proportional to
H.J.Hug et al., J. Appl. Phys. 83 (1998) 5609, P.J.A. van Schendel et al., J. Appl. Phys. 88 (2000) 435
Calibration of the MFM tip
F-layer data magnetization pattern
FFT( )
= FFT( )
FFT( )
3500 Oe 4500 Oe
+
Sample courtesy of J. Ahner, Seagate, USA
Vortices in superconducting Nb
- +
= =
500 nm 500 nm
Heat Drain
www.concentris.com Supported by
Cantilever based chemical Nose
Quantitative Analysis
Principle
147
AFM in UHV - Challenges toward Ultimate AFM
measure forces simultaneously in multiple directions
• while manipulating of single atoms and molecules
• mapping surface potentials, local reactivity
• measure quantum pressure
• magnetic exchange interactions
measure tip-sample force or bonding energy @ each image point
• measure 3d force/energy map in single scan
• intelligent feedback working. e.g. working on local bonding energy
• evaluate force curves at each xy-position from non-harmonic distortions or inter-modulation
measure force and do (state-of-the art) STM simultaneously
• inelastic tunneling / spin flip tunneling
• mapping of atomic/molecular vibrations/instabilities by AFM
ultimate force sensitivity
• UHV preparation of ultrasmall cantilevers
• ultimate MFM, EFM (single spin level)
• Casimir forces
• atomic charge distributions
• cantilever cooling to quantum limit
Laser
˦˥˨
diode 20µm
Core: 5 µm Step
Beam
splitter PD
Reference
Lens surface, R~90% Chip
thermal noise data (flexural modes) (torsional modes)
SPM
Polymer Blend imaged at different x-ray Energies
Materials: poly(3-hexylthiophene) (P3HT) and polystyrol (PS)
PFB = poly(9, 9 '-dioctylfluorene-co-bis-
N,N '-(4-butylphenyl)-bis-N,N '-
phenyl-1,4-phenylenediamine
B. Watts et el (2012) @ x07da PolLux
Magnetic Domains imaged by MFM and XMCD
5.2.1. Scanning Chemical Force Microscopy
combination with ToF-SIMS
Time-of-Flight Scanning Ion Mass Spectrometry (ToF-SIMS)
157
Surface Spectroscopy: Mass Resolution
3D retrospective analysis: LCD Switch
© Ion-Tof GmbH
Concept of combining SFM & ToF-SIMS for the in-situ measurement of
direct 3D chemical information
... after 4 Years of Development
3D NanoChemicope instrument:
IONTOF
♥
inside
NanoScan
@ IONTOF laboratories
… inside the 3D NanoChemicope instrument