Lecture 4 Scanning Probe Microscopy (SPM)

•  General components of SPM;

•  Tip --- the probe;
•  Cantilever --- the indicator of the tip;
•  Tip-sample interaction --- the feedback system;
•  Scanner --- piezoelectric movement at x,y,z;
•  Measurement artifacts: vibration must be isolated.
Basic components of SPM: tip, cantilever, sensor for tip
positioning, scanner, feedback loop (electronic control)
Generation of SPM image

X-Y raster scanning;

Z-modulation (height) by feedback system.
SPM Family

Tip-Sample
SPM
Electrical Current Tip-Sample AFM + Optical Microscopy
Interaction

STM AFM NSOM

Mechanic Force:
Extremely high
•  Contact mode
Resolution at UHV. Scanning Confocal
•  Non-contact mode
•  Tapping (intermittent) mode

Other Interactions:
•  Electrostatic mode (scanning
electrostatic potential microscope)
•  Magnetic mode
•  Chemical Force mode
 Basic components of STM:

The scanner
can be
mounted with Five basic components:
the tip or the
sample stage. 1.  Metal tip,

2.  Piezoelectric scanner,

3.  Current amplifier (nA),

4.  Bipotentiostat (bias),

5.  Feedback loop (current).

•  Tunneling current from tip to sample or vice-versa depending on bias;

•  Current is exponentially dependent on distance;
•  Raster scanning gives 2D image;
•  Feedback is normally based on constant current, thus measuring the height on surface.
Scanning Confocal Microscopy from NSOM

•  NSOM can be modified to be a SCM simply by removing the tuning fork head, the tip.
•  SCM uses the excitation beam through the same objective.
•  Both the excitation and emission shares the same focus on the sample surface.
•  Confocal requires high level alignment of optical accessories.
 Principle of Scanning Confocal Microscope

Co-focus
Comparison of STM, AFM, NSOM

STM NSOM AFM

Comparison of Tips of STM, AFM, NSOM

•  STM tip should be conducting, can be simply cut freshly by normal

wire cutter.
•  STM plays with the very top atom at the freshly cut tip, leading to
atomic resolution.
•  AFM tip should be sharp enough to get good resolution (fat-tip effect);
recently atomically sharp tip obtained by binding a small molecule atop
the tip.
•  AFM tip should be stiff enough to sense the atomic interaction with
sample surface (the distance).
•  AFM tip is not necessary to be conducting.
•  NSOM tip should be sharp enough to get good topography resolution.
•  The aperture of NSOM tip should be small for better optical resolution.
•  The outer surface of NSOM tip should be flat to avoid artificial effects
from the scanning.
Brief History of Scanning Probe Microscopy (SPM): 1

l  The first member of SPM family, scanning tunneling microscopy

(STM), was developed in 1980s.

l  In 1982, Gerd Binnig and Heinrich Rohrer at IBM in Zurich created

the ideas of STM (Phys. Rev. Lett., 1982, vol 49, p57). Both of the
two people won 1986 Nobel prize in physics for their brilliant
invention.

The Nobel Prize in

Physics 1986
Shared with Ernst Ruska
(on electronic microscopy)
Heinrich Rohrer and Gerd Binnig
Brief History of Scanning Probe Microscopy (SPM): STM
Brief History of Scanning Probe Microscopy (SPM): AFM
Cantilever: indicating the tip motion and rotation
Laser sensing to monitor the position of
cantilever:
1.  Contact mode scanning: cantilever is
usually not vibrating, but deflected due
to friction or other forces. Such a
deflection can be detected precisely by
the sensitive photodiode.
2.  Non-contact mode scanning: cantilever
is in vibration with constant frequency
(> 100 kHz). Such vibration can be
monitored precisely by the laser
sensing. To keep the resonance
frequency (the constant height over the
sample) during scanning, the Z-scanner
has to adjust the height of the
cantilever. Such adjustment can be
recorded by the computer to create the
scanning profile, the image.
Laser sensing both tilting and twisting of cantilever
How to create vibration of cantilever?

There are two ways to drive the cantilever into oscillation.

n  One way is accomplished by indirect vibration, in which the cantilever is excited
by high frequency acoustic vibration from a piezoelectric transducer attached to
the cantilever holder. This is called the Acoustic AC mode (AAC).
n  Another, more favored method that is much cleaner and gentler than Acoustic
AC mode is a direct vibration method where the cantilever is excited directly
without having to vibrate the cantilever housing or other parts. This is called
Magnetic AC mode (MAC Mode™). To achieve MAC Mode imaging, a cantilever
coated with a magnetic material is driven into oscillation by an AC magnetic
field generated by a solenoid positioned close to the cantilever housing. The
result of MAC Mode™ is a gentle, clean cantilever response that has no spurious
background signals (“forest of peaks”) like other AC modes can have. MAC Mode
has even greater advantages when the cantilever is vibrated in liquid.
The Feedback in SPM with laser detection
Resonance vibration of cantilever --- spring model

Resonance frequency of the

cantilever,

1.5
1 k 0.5 1 EW ⎛T ⎞
f0 = ( ) = ⎜ ⎟
2π m0 4π m0 ⎝L⎠

•  k the spring constant, m0 the

effective mass of the lever.
•  The softer the lever (smaller
k), the more sensitive for
detecting the deflection, but
requires smaller mass to keep
the high frequency. Why high f
F: the force; k: the spring constant needed? (see next slide)
Environmental vibration should be isolated

ω: the angular frequency, = 2πf0

To remove high frequency noise, floating (vibration isolating) table needed.

 Atomic interaction (force)

1.5
1 k 0.5 1 EW ⎛ T ⎞
f0 = ( ) = ⎜ ⎟
2π m0 4π m0 ⎝ L ⎠

1013
10-25

10 N/m

A distance of 0.1 nm (or 1 Å, typical chemical bond length) between tip and
sample means a force of 10-9 Newton, which is enough for deflecting the
cantilever (commercial cantilever has k between 10-2 N/m ≤ kc ≤ 102 N/m).

ω: the angular frequency, = 2πf0

 Vibration between two atoms
•  Taking m = 10-25 kg and ω0 = 1013 Hz for atomic masses and vibrational
frequencies, the spring constant of bi-atom vibration kc = 10 N/m = 10 nN/nm.
(proton mass = 1.672 621 71 × 10−27 kg, neutron mass = 1.674 927 29 × 10−27
kg, atoms mass ~ a few tens of protons or neutrons) (The unified atomic
mass unit (u), or dalton (Da), is a small unit of mass used to express atomic
and molecular masses. It is defined to be one twelfth of the mass of an
unbound atom of 12C at rest and in its ground state) (12C is the most abundant
of the two stable isotopes of the element carbon, accounting for 98.89% of
carbon; it contains 6 protons, 6 neutrons and 6 electrons)

•  Even smaller spring constants can be easily obtained by minimizing the

cantilever´s mass. Commercial cantilevers have a typical spring constant in
the range of 10-2 N/m ≤ kc ≤ 102 N/m, typical resonant frequencies in the range
of 1 kHz ≤ f0 ≤ 500 kHz, a radius of curvature of the probing tip as small as 10
nm, and are usually fabricated of Si, SiO2 or Si3N4.
Atomic interaction
Atomic interaction at different tip-sample distances

Repulsion:
At very small tip-sample distances (a few angstroms) a very strong repulsive force
appears between the tip and sample atoms. Its origin is the so-called exchange
interactions due to the overlap of the electronic orbitals at atomic distances. When
this repulsive force is predominant, the tip and sample are considered to be in
“contact”.

Attraction (Van der Waals):

A polarization interaction between atoms: An instantaneous polarization of an atom
induces a polarization in nearby atoms – and therefore an attractive interaction.
Raster scanning of piezoelectric scanner

S – Strain [Å/m], d – Strain coefficient [Å/V], E – Electric field [V/m]

Ideally, a piezoelectric scanner varies linearly with applied voltage.
Scanning step (resolution): 0.1 nm
Scanner Intrinsic Nonlinearity

Ideally, the intrinsic nonlinearity is the ratio Δy/y of the maximum

deviation Δy from the linear behavior to the ideal linear extension y
at that voltage. It is in the range 2-25%.
Scanner Hysteresis

The hysteresis of a piezoelectric scanner is the ratio of the maximum divergence

between the two curves to the maximum extension that a voltage can create in the
scanner: ΔY/Ymax. Hysteresis can be as high as 20% in piezoelectric materials.
Scanner Creep
Scanner Aging

The aging rate is the change in strain coefficient (Å/V) per decade of time.
The piezoelectric strain coefficient, changes exponentially with time:
increases with regular use, decreases with no use.
Software correction of scanner
Hardware correction of scanner

A sensor “reads” the scanner actual position, and a feedback

system applies voltage to drive the scanner to the desired position,
the total nonlinearity can be reduced to 1%.
Scanning artifacts

•  Not-in good feedback (tip far from the sample surface).

•  Electrical noise (particularly the periodical noise added to the
internal signal).
•  Environmental vibration (particular when the frequency is close
to that of the tip oscillation).
•  Fat-tip effect.
•  Unknown tip-sample interaction (slowing down the scanning
speed…).
Test of scanning artifacts

•  Repeat the scan to ensure that it looks the same.

•  Change the scan direction and take a new image.
•  Change the scan size and take an image to ensure that the features scale
properly.
•  Rotate the sample and take an image to identify tip imaging
•  Change the scan speed and take another image (especially if you see
suspicious periodic or quasiperiodic features).
Advantages of
Scanning Probe Microscopy (SPM)

l  Angstroms (atoms) to Nanometers (molecules);

l  Digitalized and Computerized;

l  Experimentally Versatile;

l  Highly Tunable and Flexible to be Combined with Others;

l  Wide Application in Surface and Nanotechnology.

Scanning Probe Microscopy (SPM)

Double functions: scanning and probing.

Scanning: piezo raster 2D (X-Y) scanning;

Probing: sharp tip mounted to a Z-scanner.
Comparison between traditional optical and electron
microscopes and SPM

probe Mechanism Sample Resolution

High vacuum
Using properties of chamber,
Å – µm,
waves: Strict sample pre-
Traditional Light/electron good for X-Y lateral
diffraction, deflection, treatment (e.g.
imaging
scattering conducting stain)
required

Usually under
ambient conditions,
Using interaction though high imaging Å – nm,
between tip and sample: resolution also good for Z-height
SPM Tip
mechanic, electrostatic, requires high vacuum measurement, thus
magnetic. to keep clean surface, topography imaging
Highly flexible with
other techniques

•  SPM cannot replace electron microscopes, but complementary each other.

•  SPM is not just superior in high resolution imaging, but more importantly it
can target and manipulate just ONE atom or molecule.