Scanning Probe Microscopy
Scanning Probe Microscopy
Introduction,
Quantum tunneling in STM
STM Instrumentation
STM Operation modes
STM Examples
Manipulation of individual atoms
Forces in AFM
AFM instrumentation
AFM Examples
Magnetic force microscopy
Lateral force microscopy
Other SPM Techniques
Introduction
The scanning tunneling microscope (STM) is the ancestor of
all scanning probe microscopes. It was invented in 1981 by
Gerd Binnig and Heinrich Rohrer at IBM Zurich. Five years
later they were awarded the Nobel prize in physics for their
invention. The STM was the first instrument to generate real-
space images of surfaces with atomic resolution.
Equally important was
the development of the
atomic force microscope
(AFM) invented by Gerd
Binnig in the mid-
eighties. Other related
SPM techniques were
developed subsequently
in last 15 years.
Scanning Tunneling Microscopy
Quantum Tunneling in STM
Tip-to-Sample Separation
STMs use a sharpened, conducting tip with a bias voltage applied
between the tip and the sample. When the tip is brought within about
10 Å of the sample, electrons from the sample begin to "tunnel"
through the 10 Å gap into the tip or vice versa, depending upon the
sign of the bias voltage.
The resulting tunneling
current varies with tip-to
sample spacing, and it is the
signal used to create an STM
image. For tunneling to take
place, both the sample and
the tip must be conductors or
semiconductors.
STM Instrumentation
Tip
Scanner
Sample positioner
Vibration isolation
Control electronics
Preamplifier
Feedback
Scan control
Computer and software
Piezoelectric materials are ceramics that change dimensions in
response to an applied voltage. Conversely, they develop an
electrical potential in response to mechanical pressure.
Piezoelectric scanners can be designed to move in x, y, and z by
expanding in some directions and contracting in others. Piezoelectric
scanners for SPMs are usually fabricated from lead zirconium
titanate, or PZT, with various dopants added to create specific
materials properties.
STM Tips
1. For atomic resolution STM studies on relatively flat sample
surfaces, the STM tip should terminate in a single atom.
2. For topographic STM studies of large scale structures on relatively
rough surfaces, a tip with a small cone is required.
3. The chemical composition at the front end of the tip is important
for the tunneling properties. Oxide or contamination layer should
be removed.
Choice of Tip Material
1. Since contact between tip and sample surface can occur
during scanning, it is necessary to choose a relatively hard
material for the tip.
2. For UHV, W tips have been widely used. Also Pt/Ir, Mo tips.
3. For air or poor vacuum, an inert material is favorable:
Pt or Au: soft
Pt/Ir alloy hard
Tip Preparation Methods
Electrolytical etching
Active tip radius: 100 Å or less
W wire 0.1 – 1 mm
In KOH or NaOH solution: 5 – 12 V/10 mA, Counterpart electrode can be
graphite. Breaks when the tensile strength of the notched region can no
longer sustain the weight of the small lower end. Etching stopped when tip
falls off
Au wire: 32% HCl working electrode Pt-Ir ring;
Au rotation 950 rpm: ac 5 V/ 1 kHz + dc offset
2.5 V
Pt-Ir (10%) wires: 20% KCN solution and ac
3 – 15 V.
Very sharp tips can be made, but an unwanted oxide layer can form on the
surface of the tip. A HF-dipped is performed before using the tip.
(2) Focused Ion Beam Milling
(3) Mechanically cutting
For air STM
Not suitable for the
study of rough surface
(4) Combined electrolytical etching and mechanical pulling
The pulling apart
step can be done
in UHV to avoid
oxide formation
(5) Electron beam induced chemical vapor deposition
(6) Field evaporation Field evaporation
Sample Positioner
The STP devices need to move the sample far enough away
from the tip to allow sample transfers and then approach the
sample to within the range of the z-axis of the scanner.
Schematic diagram of a UHV STM unit. (A) the macor block onto which
the x,y,z piezo scanners are mounted, (B) the microscope base plate, (C)
carriage rods, (D) stop, (E) ball bushing assembly, (F) connecting arms to
sample, (G) sample and sample holder, (H) catch, (I) foot, and (J) probe tip
mounted on the top of the x-y piezoelectric drive
Vibration Isolation
• Floor vibration amplitudes: 0.1-1 µm
• Requirement of a stability of the tip-to-sample spacing: 0.01 Å
Two typical vibration isolation techniques
(1) Coiled spring suspension with magnetic damping
(2) A stack of metal plates with viton dampers between each
pair of steel plates
In addition, rigid and compact STMs are more immune to vibration.
STM Operation Modes
In constant-height mode, the tip
travels in a horizontal plane above the
sample and the tunneling current varies
depending on the topography and local
surface electronic properties of the sample.
The tunneling current measured at each
location on the sample surface constitute
the data set, the topographic image.
In constant-current mode, STMs use
feedback to keep the tunneling current
constant by adjusting the height of the
scanner at each measurement point. For
example, when the system detects an
increase in tunneling current, it adjusts the
voltage applied to the piezoelectric scanner
to increase the distance between the tip
and the sample.
In constant-current mode, the motion of the scanner constitutes the
data set. If the system keeps the tunneling current constant to within
a few percent, the tip-to-sample distance will be constant to within a
few hundredths of an angstrom.
Each mode has advantages and disadvantages. Constant-height
mode is faster because the system does not have to move the
scanner up and down, but it provides useful information only for
relatively smooth surfaces. Constant-current mode can measure
irregular surfaces with high precision, but the measurement takes
more time.
As a first approximation, an image of the tunneling current maps the
topography of the sample. More accurately, the tunneling current
corresponds to the electronic density of states at the surface. STMs
actually sense the number of filled or unfilled electron states near
the Fermi surface, within an energy range determined by the bias
voltage. Rather than measuring physical topography, it measures a
surface of tunneling probability.
Scanning Tunneling Spectroscopy
Scanning tunneling spectroscopy
(STS) studies the local electronic
structure of a sample's surface.
The electronic structure of an atom
depends upon its atomic species
and also upon its local chemical
environment.
Energy level diagram for sample and tip.
(a) Independent sample and tip.
(b) Sample and tip at equilibrium,
separated by a small vacuum gap.
(c) Positive sample bias: electron tunnel
from the tip to the sample.
(d) Negative sample bias: electron tunnel
from the sample into the tip
STS Encompasses Many Methods:
• Taking "topographic" (constant-current) images using
different bias voltages and comparing them;
• Taking current (constant-height) images at different heights;
• Ramping the bias voltage with the tip positioned over a
feature of interest while recording the tunneling current.
The last method results in current vs. voltage (I-V) curves
characteristic of the electronic structure at a specific x, y
location on the sample surface. STMs can be set up to collect
I-V curves at every point in a data set, providing a three-
dimensional map of electronic structure.
Plotting of STM images
