Académique Documents
Professionnel Documents
Culture Documents
The main feature that all SPMs have in common is that the measurements
are performed with a sharp probe scanning over the surface while
maintaining a very close spacing to the surface. With most SPM
technologies, this produces an atomically short depth of focus such that
only the top layer of rigidly bound (chemisorbed) atoms is seen.
Excellent spatial resolution can be obtained by using a very sharp probe
(on the order of a few nanometers radius of curvature at the end, and with
a very steep sidewall angle) and keeping it's spacing from the surface
very small (usually within a nanometer). These instruments were the first
to produce real space images of atomic arrangements on flat surfaces.
SPMs are most commonly used to perform very precise, three
dimensional measurements on the nanometer-to-micron scale.
Until recently, researchers have relied upon other instruments for imaging
and measuring the morphology of surfaces. On the microscopic scale, the
optical microscope has been the most widely used tool since the 1600s.
These microscopes produce excellent images of surfaces that are at least
partially optically opaque. They can measure the size of features in the x
and y directions (in the sample surface plane) but, except in very special
cases, cannot provide any measurements in the z direction (normal to the
sample surface plane) in the micrometer and below range. They are also
typically limited in resolution by the Nyquist relation to the wavelength
of the light they use (typically about 1 m).
Originating in the 1940s, the next most widely used instrument for
measuring surface morphology has been the scanning electron
microscope (SEM). SEMs image only the near surface of samples so
their optical properties are no longer a consideration. Like optical
microscopes, SEMs only measure the x and y (and not the z) dimensions
of samples. With today's general purpose SEMs, resolution is limited by
the properties of the electromagnetic lenses to about 50 angstroms.
Scanning probe microscopes are the newest entry into the surface
metrology field. As opposed to optical microscopes and SEMs, they do
measure surfaces in all three dimensions: x, y, and z. Like SEMs, they
image and measure the surface of the sample. X and y resolution in an
SPM is typically 20 angstroms and, with the best instruments and the
right sample, can be better than 1 angstrom. Z resolution is typically
better than 1 angstrom.
Probe: Another key component in the system is the probe, or tip. The
probe can be scanned over the sample or it can be stationary and the
sample can be scanned under it. With today's sophisticated
semiconductor technology, tips and cantilevers are produced in large
quantity with consistently shaped, very sharp tips. These tips are secured
on the end of cantilevers with a wide range of properties designed for a
variety of scanning probe technologies. Cantilevers are available with
spring constants less than interatomic bond strengths (about 1 Newton/m)
and will therefore allow topographic imaging of surface atomic structure
by sliding the tip/cantilever assembly across the surface and monitoring
cantilever deflection (contact AFM). These cantilevers can be made with
resonant frequencies >10khz to allow rapid scanning over surfaces with
high spatial frequency roughness. At the other extreme, the cantilever
oscillation techniques (e.g., non-contact AFM, MFM, TappingMode
AFM, etc.) require very stiff cantilevers with high resonant frequencies.
There are also many types of tips available with varying shapes (for
probing different morphologies and scales of surface features) and
materials (conducting, magnetized, very hard, etc.).
Probe Motion Sensor: This system senses the spacing between the
probe and the sample and provides a correction signal to the piezoelectric
scanner to keep the spacing constant. For STM, the tunnelling current is
used to sense the spacing between the probe and the sample surface. For
AFM, the most common design for this function is called an optical lever,
or beam deflection system. This design uses a laser shining onto and
reflecting off the back of the cantilever and onto a segmented photodiode
to measure the probe motion. There are other systems, e.g.,
interferometers, piezoelectric cantilevers and probe oscillation systems
that detect forces by the change in the resonant frequency, phase, or
amplitude of oscillation. However, the beam deflection system is the
most widely used because it is the lowest noise, most stable and most
versatile system available.
Electronics: The electronics interface unit provides interfacing
between the computer and the scanning system. It supplies the voltages
that control the piezoelectric scanner, accepts the signal from the position
sensing unit and contains the feedback control system for keeping the
spacing between sample and tip constant.
The scanning tunnelling microscope was the first SPM and was first
recognized as having atomic resolution capability in 1981. It works by
mechanically scanning a very sharp conducting tip over the surface of a
conducting sample. A bias voltage is applied between the tip and the
sample causing a tunnelling current to flow when the tip is kept near the
sample.
It = Ve-Cd
Like the STM, the AFM also uses a very sharp tip to probe and map the
morphology of a surface. The key element of the AFM is its microscopic
force sensor, or cantilever. The cantilever is usually formed by one or
more beams of silicon or silicon nitride with a dimension of 100 ~ 500
microns long and 0.5 ~ 5 microns wide. Mounted on the end of the
cantilever is a sharp tip used to sense the force between the tip and the
sample surface.
For normal topographic imaging, the probe tip is brought into continuous
or intermittent contact with the sample and raster-scanned over the
surface by a piezoelectric scanner that generate the precision motion
needed for topographic images and force measurements.
Contact AFM
To help examine the basics of AFM force measurements, the figure above
shows a typical force-versus-distance curve or force curve. Force curves
typically show the deflection of the free end of the AFM cantilever as the
fixed end of the cantilever is brought vertically towards and then away
from the sample surface. By applying a triangle-wave voltage pattern to
the electrodes for the z-axis scanner, the scanner expands and then
contracts in the vertical direction, generating relative motion between the
cantilever and sample. The deflection of the free end of the cantilever is
measured and plotted at many points as the z-axis scanner extends the
cantilever towards the surface and then retracts it again. By controlling
the amplitude and frequency of the triangle-wave voltage pattern, one can
also vary the distance and speed that the AFM cantilever tip travels
during the force measurement.
Example: Force curves on patterned regions for different tip and sample
functional group terminations
TappingMode Operation
First, the constant downward force of the tip onto the sample surface is
not always low enough to avoid damaging some sample surfaces. These
include most biological surfaces, most polymer surfaces, and even many
surfaces of seemingly harder materials - a prime example being silicon
wafer surfaces.
The reason for the lack of force control is that in a typical atmospheric
ambient environment, surfaces are always covered by 10 to 30
monolayers of adsorbed gas. The adsorbed gas layer is mostly water
vapor, hydrocarbons, nitrogen, and carbon dioxide that is physisorbed
onto the surface or held there by the interatomic van der Waals attractive
potential. This adsorbed gas layer has associated with it a surface tension
that causes the layer to wick up onto the AFM tip when the tip comes into
contact with it. This pulls the tip toward the surface with a force that can
damage some samples.
Another problem that arises with contact AFM is that it is often desirable
to examine items that are only loosely bound to a substrate. Examples of
this are DNA stretched across a mica surface, particles on a silicon wafer,
or particulate samples which are difficult to sufficiently adhere to a
substrate. The contact AFM probe pushes these items around on their
substrate, either pushing them completely out of the area being analysed
or creating streaked, non-physical images. Further more, as the contact
AFM tip rubs across the sample, the tip can also cause sufficient
frictional force to produce shear forces that can tear surface features.
TappingMode inherently prevents the tip from sticking to the surface and
causing damage during scanning. Unlike contact mode, when the tip
contacts the surface, it has sufficient oscillation amplitude to overcome
the tip-sample adhesion forces. Also, the surface material is not pulled
sideways by shear forces since the applied force is always vertical.
LiftMode Operation
In LiftMode, the tip makes a first pass across the sample surface using
TappingMode to measure the topography of that line. It then raises up an
operator-selected amount and retraces the surface topography while
performing non-contact measurement of the electric or magnetic field
near the surface. It then repeats these measurements over the entire area
of interest. In this way, in one scan of the area, the system acquires a
topographic map of the surface and a field map of the same area. These
are displayed separately and in real time during the measurement and,
upon completion of the area scan, can be stored and analysed
independently.
When the probe is brought into contact with a sample, the surface resists
the oscillation and the cantilever bends. Under the same applied force, a
stiff area on the sample will deform less than a soft area; i.e., stiffer
surfaces cause greater resistance to the vertical oscillation and,
consequently, greater bending of the cantilever. The variation in
cantilever deflection amplitude is a measure of the relative stiffness of the
surface. Topographical information (DC, or non-oscillatory deflection) is
collected simultaneously with the force modulation data (AC, or
oscillatory deflection).
Force modulation imaging can be used in a wide range of applications
including identifying transitions between different components in
composites, rubber and polymer blends, evaluating polymer homogeneity,
imaging organic materials on hard substrates, detecting residual
photoresist on integrated circuits, and identifying contaminants in a
variety of materials.
Nanoindentation
Barriers
The most important characteristic of an SPM is its ability to very
accurately measure surface topography. In all of its modes of operation,
it is either measuring topography or using topography to track the surface
in the measurement of another parameter (magnetic field, electric field,
etc.). This need for high accuracy in measuring surface topography has
produced conflicting demands on scanning force microscopy. The
dichotomy derives from the requirement that the tip move across the
surface very rapidly while following the surface topography very closely
(i.e., the tip is tightly coupled to the surface through the feedback loop).
This requires, in some cases, forces on the surface are in excess of the
yield force or binding force of a feature on the surface. The unfortunate
result is that surface features of interest can be modified by the scanning
probe.
Summary
Force Modulation:
Measures relative stiffness of surface features.
TappingMode AFM:
Measures topography by tapping the surface with an oscillating probe tip;
eliminates shear forces which can damage soft samples and reduce image
resolution.
Phase Imaging:
Measures variations in surface properties (stiffness, adhesion, etc.) as the
phase lag of the cantilever oscillation relative to the piezo drive.
Nanoindentation:
For indenting and scratching thin films and other surfaces.
Lithography:
Use of probe tip to write patterns in either STM or AFM contact mode.