In the arena of
microscopy techniques, the scanning probe microscope, with its many
derivitives, is still in its infancy. Binning and Rohrer won the 1986
Nobel Prize for work performed with the scanning tunneling microscope.
Shortly thereafter, atomic force microscopy was realized. For convenience,
these two techniques have been lumped under the header of scanning probe
microscopy. A discussion of these technologies follows.
SPM techniques all
use piezo-electric ceramics and computers. The differences among the
techniques comes down to the 'probe' that is being used to 'sense' the
sample, and what phenomenon the 'probe' is 'sensing.' How the piezo-electric
ceramics are utilzed on a certain manufacturers instrument most likely
comes down to their attempt at avoiding copyright infringement. The
Digital Instruments Nanoscope III System that I am most familiar with
uses piezo-electric ceramics to scan (move) the specimen in relationship
to the probe. Other companies might use the piezo material to move the
probe in respect to the sample. What are piezo-electric ceramics?
Piezo-electric ceramics
are materials whose crystal planes slip on one another when a current
is applied across them. This slippage causes shrinkage or elongation
of the crystal (depending on the current applied). Segmented tubes of
this material are made. The tubes are usually segmented into five zones,
two being x, two being y, and one z axis. Two x and y axes are needed
so that they can 'fight' themselves. As the current to one x axis is
increased, the current to the other x axis is decreased at the same
rate. Thus, one side of the tube is expanding while the the other side
is contracting. This causes the tube to 'lean,' scanning the sample
back and forth under the probe. The y component of the scan is achieved
in the same fashion. The current applied to the x and y portions determine
the area of the specimen that is scanned. The z portion of the tube
is used to keep the sample in close proximity to the probe when sample
surface detail changes. The current to the z portion can be used to
map the surface of the sample. An image formed by this current is referred
to as a height mode image.
We now know about
the scanning action, and it's time to start discussion of the many 'probes'
one can employ. Since scanning tunneling microscopy (STM) was first,
let's start there. The 'probe' used in STM is most often a very sharp
section of Pt/Ir wire. A sample is placed onto the scanner, and the
wire is brought into close proximity of the sample surface. The computer
is allowed to take control of the wire/sample separation, bringing them
closer together until a predetermined tunneling current is established
between the wire and sample surface. This current is usually on the
nano-to pico-ampere scale. Once this current is established, we have
two modes of operation by which to form an image of the sample. One
mode is the constant current mode. This tells the computer that is controlling
the scanning to make necessary corrections to the z portion of the scanner
so that the tunneling current is always the same. Tunneling current
might change due to surface roughness (increasing the gap between the
wire and the surface), or change in atomic number of the sample (one
area might be a better conductor). The other mode of operation would
be the constant height mode, where the sample is held the same distance
below the wire as the scan is performed, and the image is formed from
the variations in tunneling current that this causes. Scanning tunneling
can provide atomic force microscopy (AFM) techniques. STM requires that
a sample be conductive, where this is not a requirement of AFM.
The scanners and
computers used for STM can be used for Atomic Force Microscopy (AFM).
AFM can be either contact mode AFM, or tapping mode AFM (tapping is
a registered trademark of Digital Instruments, Inc). Both of these modes
make use of a laser beam being reflected off of the back of a cantilever
to generate an image of the sample surface. This laser is housed in
the AFM head. In this head are the laser, the cantilever, a mirror,
and a four quadrant photodiode array. The laser has x and y positioning
so that it can be positioned on the back of the cantilever. Proper positioning
of the laser enhances its reflectance toward the mirror. The reflected
laser strikes the mirror. The angle of the mirror can be changed so
that the laser hits the photodiode array. The photodiode array is divided
into four quadrants. In which quadrant, and where in the quadrant the
laser strikes determines the voltage that comes out of the photodiode
array. One can tell the computer that the voltage coming out of the
photodiode array must remain constant. Therefore, if the scanning cantilever
encounters a surface change on the specimen, it must move specimen up/down
with the z portion of the scanner so that cantilever deflection doesn't
occur (deflection of cantilever=position change of laser on photodiode=change
in voltage output). This type of data (not allowing the cantilever to
be deflected and using the voltage change of the z portion of the piezo
scanner) is referred to as height mode. Deflection mode imaging is when
the sample is allowed to cause deflection of the cantilever. This deflection
causes the laser to change position on the photodiode array, changing
the voltage output of the photodiode array. An image can be made using
this changing voltage. It should be readily apparent that deflection
and heigh mode images can not be optimized at the same time.
Normal contact mode
AFM utilizes the top and bottom portions of the four quadrant photodiode
array. Lateral Force Microscopy (LFM), or also called frictional force
microscopy, makes use of the left and right hand portions of the photodiode
array. The cantilevers used for contact AFM are bi-legged silicon nitride
semi-conductor material that has a pyrimidal tip. Normally, the sample
is scanned perpendicular to the base of the pyrimidal tip. The software
allows one to choose the angle that the sample is scanned in respect
to the tip. If one scans in a direction parallel to the base of the
pyramid, differences in 'stickiness' of the sample can cause the cantilever
to torque, deflecting the reflected laser light between the left and
right quadrants of the photodiode array. This deflection, as measured
by the photodiode array output, can be used to map different frictional
characteristics of the sample's surface.
During contact mode
AFM imaging, the cantilever is physically touching the sample. This
contact can alter surface structures. Tapping or 'non-contact' mode
avoids this, and has become the most popular mode of SPM operation.
Ideally, the tip of the cantilever used in tapping never makes contact
with the sample being imaged. The design of the cantilever used for
tapping is different from those used for contact. The tapping mode cantilever
is a single 'plank' or spring board of silicon. The laser is focused
on the back of the cantilever in much the same fashion as in the contact
mode. In the cantilever holder, there is a stack of piezoelectric material,
the resonance frequency of the cantilever can be found. As the cantilever
bounces, the laser reflectance moves over a fairly constant line length
on the photodiode array. With the cantilever vibrating at it's oscillating
frequency, it is brought into close proximity of the sample surface.
Air that is trapped between the cantilever and the sample surface dampens
the vibration of the cantilever, changing the laser line length on the
photodiode array. Different line lengths cause the different voltage
outputs of the photodiode array. The most common approach to forming
an image is to have the software set up so that it moves the sample
up or down to keep the coltage output of the photodiode array constant.
The voltage to the piezo responsible for moving the sample is used to
create an image of the surface of the sample.