Scanning Probe Microscopy ( STM / AFM )

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Scanning Probe Microscopy ( STM / AFM )
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Topographic scan of a glass surface
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• In the early 1980's two IBM scientists, Binnig
  Rohrer, developed a new technique for studying
  surface structure - Scanning Tunnelling
  Microscopy ( STM ). This invention was quickly
  followed by the development of a whole family of
  related techniques which, together with STM, may
  be classified in the general category of Scanning
  Probe Microscopy ( SPM ) techniques. Of these
  later techniques, the most important is Atomic
  Force Microscopy ( AFM ).
• The development of these techniques has without
  doubt been the most important event in the
  surface science field in recent times, and opened
  up many new areas of science and engineering at
  the atomic and molecular level.

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Basic Principles of SPM Techniques

• All of the techniques are based upon scanning a
  probe (typically called the tip in STM , since it
  literally is a sharp metallic tip) just above a
  surface whilst monitoring some interaction
  between the probe and the surface.

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• The interaction that is monitored in
• STM - is the tunnelling current between a
  metallic tip and a conducting substrate which are
  in very close proximity but not actually in
  physical contact.
• AFM - is the van der Waals force between the tip
  and the surface this may be either the short
  range repulsive force (in contact-mode) or the
  longer range attractive force (in non-contact
  mode).
• For the techniques to provide information on the
  surface structure at the atomic level (which is
  what they are capable of doing ! )
• the position of the tip with respect to the
  surface must be very accurately controlled (to
  within about 0.1 Å) by moving either the surface
  or the tip.
• the tip must be very sharp - ideally terminating
  in just a single atom at its closest point of
  approach to the surface.

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• The attention paid to the first problem and the
  engineering solution to it is the difference
  between a good microscope and a not so good
  microscope - it need not worry us here,
  sufficient to say that it is possible to
  accurately control the relative positions of tip
  and surface by ensuring good vibrational
  isolation of the microscope and using sensitive
  piezoelectric positioning devices.
• Tip preparation is a science in itself - having
  said that, it is largely serendipity which
  ensures that one atom on the tip is closer to the
  surface than all others.

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Let us look at the region where the tip
approaches the surface in greater detail ....
... the end of the tip will almost invariably
show a certain amount of structure, with a
variety of crystal facets exposed ...
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and if we now go down to the atomic scale ....
... there is a reasonable probability of ending
up with a truly atomic tip.
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• If the tip is biased with respect to the surface
  by the application of a voltage between them then
  electrons can tunnel between the two, provided
  the separation of the tip and surface is
  sufficiently small - this gives rise to a
  tunnelling current.
• The direction of current flow is determined by
  the polarity of the bias.

If the sample is biased -ve with respect to the
tip, then electrons will flow from the surface to
the tip as shown above, whilst if the sample is
biased ve with respect to the tip, then
electrons will flow from the tip to the surface
as shown below.
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The name of the technique arises from the quantum
mechanical tunnelling-type mechanism by which the
electrons can move between the tip and substrate.
Quantum mechanical tunnelling permits particles
to tunnel through a potential barrier which they
could not surmount according to the classical
laws of physics - in this case electrons are able
to traverse the classically-forbidden region
between the two solids as illustrated
schematically on the energy diagram below.
This is an over-simplistic model of the
tunnelling that occurs in STM but it is a useful
starting point for understanding how the
technique works.
In this model, the probability of tunnelling is
exponentially-dependent upon the distance of
separation between the tip and surface the
tunnelling current is therefore a very sensitive
probe of this separation.
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• Imaging of the surface topology may then be
  carried out in one of two ways
• in constant height mode (in which the tunnelling
  current is monitored as the tip is scanned
  parallel to the surface)
• in constant current mode (in which the tunnelling
  current is maintained constant as the tip is
  scanned across the surface)

If the tip is scanned at what is nominally a
constant height above the surface, then there is
actually a periodic variation in the separation
distance between the tip and surface atoms. At
one point the tip will be directly above a
surface atom and the tunnelling current will be
large whilst at other points the tip will be
above hollow sites on the surface and the
tunnelling current will be much smaller.
A plot of the tunnelling current v's tip position
therefore shows a periodic variation which
matches that of the surface structure - hence it
provides a direct "image" of the surface (and by
the time the data has been processed it may even
look like a real picture of the surface ! ).
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In practice, however, the normal way of imaging
the surface is to maintain the tunnelling current
constant whilst the tip is scanned across the
surface. This is achieved by adjusting the tip's
height above the surface so that the tunnelling
current does not vary with the lateral tip
position. In this mode the tip will move slightly
upwards as it passes over a surface atom, and
conversely, slightly in towards the surface as it
passes over a hollow.
The image is then formed by plotting the tip
height (strictly, the voltage applied to the
z-piezo) v's the lateral tip position.
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How an STM works
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AFM
The AFM consists of a microscale cantilever with
a sharp tip (probe) at its end that is used to
scan the specimen surface. The cantilever is
typically silicon or silicon nitride with a tip
radius of curvature on the order of nanometers.
When the tip is brought into proximity of a
sample surface, forces between the tip and the
sample lead to a deflection of the cantilever
according to Hooke's law.
Typically, the deflection is measured using a
laser spot reflected from the top of the
cantilever into an array of photodiodes.
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If the tip were scanned at a constant height,
there would be a risk that the tip would collide
with the surface, causing damage. Hence, in most
cases a feedback mechanism is employed to adjust
the tip-to-sample distance to maintain a constant
force between the tip and the sample.
Traditionally, the sample is mounted on a
piezoelectric tube, that can move the sample in
the z direction for maintaining a constant force,
and the x and y directions for scanning the
sample.
The AFM can be operated in a number of modes,
depending on the application. In general,
possible imaging modes are divided into static
(also called Contact) modes and a variety of
dynamic (or non-contact) modes.
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AFM cantilever (after use) in the SEM,
magnification 1,000 x
AFM cantilever (after use) in the SEM,
magnification 3,000 x
AFM cantilever (after use) in the SEM,
magnification 50,000 x
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   The atoms of a Sodium Chloride crystal
viewed with an Atomic Force Microscope
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Lithography and micromanipulation

• The interactions between the STM tip and
  substrate can be used to modify the surface in a
  controlled way.
• This can be done in a number of ways.
• Eg Eigler and Schweizer manipulated xenon atoms
  on a Nickel(110) surface under UHV conditions,
  with everything at 4K.
• They reported that under these conditions
  everything was stable for days.
• This allowed them to move single atoms at a time
  until they achieved the following result.

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• Obtained by manipulating CO on a Pt(111) surface.

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The first Atomic Force Microscope - Science
Museum London
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• Typically resolution achieved by AFM is less than
  that achieved using STM.

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AFM vs SEM

• The AFM has several advantages over the scanning
  electron microscope (SEM). Unlike the electron
  microscope which provides a two-dimensional
  projection or a two-dimensional image of a
  sample, the AFM provides a true three-dimensional
  surface profile. Additionally, samples viewed by
  AFM do not require any special treatments (such
  as metal/carbon coatings) that would irreversibly
  change or damage the sample. While an electron
  microscope needs an expensive vacuum environment
  for proper operation, most AFM modes can work
  perfectly well in ambient air or even a liquid
  environment. This makes it possible to study
  biological macromolecules and even living
  organisms. In principle, AFM can provide higher
  resolution than SEM. It has been shown to give
  true atomic resolution in ultra-high vacuum
  (UHV). UHV AFM is comparable in resolution to
  Scanning Tunneling Microscopy and Transmission
  Electron Microscopy.
• A disadvantage of AFM compared with the scanning
  electron microscope (SEM) is the image size. The
  SEM can image an area on the order of millimetres
  by millimetres with a depth of field on the order
  of millimetres. The AFM can only image a maximum
  height on the order of micrometres and a maximum
  scanning area of around 150 by 150 micrometres.

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• Another inconvenience is that an incorrect choice
  of tip for the required resolution can lead to
  image artifacts. Traditionally the AFM could not
  scan images as fast as an SEM, requiring several
  minutes for a typical scan, while a SEM is
  capable of scanning at near real-time (although
  at relatively low quality) after the chamber is
  evacuated. The relatively slow rate of scanning
  during AFM imaging often leads to thermal drift
  in the image (Lapshin, 2004, 2007), making the
  AFM microscope less suited for measuring accurate
  distances between artifacts on the image.
  However, several fast-acting designs were
  suggested to increase microscope scanning
  productivity (Lapshin and Obyedkov, 1993)
  including what is being termed videoAFM
  (reasonable quality images are being obtained
  with videoAFM at video rate - faster than the
  average SEM). To eliminate image distortions
  induced by thermodrift, several methods were also
  proposed (Lapshin, 2004, 2007).

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• Due to the nature of AFM probes, they cannot
  normally measure steep walls or overhangs.
  Specially made cantilevers can be modulated
  sideways as well as up and down (as with dynamic
  contact and non-contact modes) to measure
  sidewalls, at the cost of more expensive
  cantilevers and additional artifacts.

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