Scanning Probe Microscopy

Scanning Tunneling Microscope STM Atomic Force Microscope AFM

HEINRICH ROHRER

GERD BINNIG

IBM spelled in Xenon atoms

Shared* the 1986 Nobel prize in Physics for their invention of the scanning tunneling microscope

HEINRICH ROHRER

GERD BINNIG

IBM spelled in Xenon atoms

Shared* the 1986 Nobel prize in Physics for their invention of the scanning tunneling microscope

* Ernst Ruska was the other winner

Electron Tunneling:
In scanning tunnneling microscopy a small bias voltage V is applied so that due to the electric field the tunneling of electrons results in a tunneling current I.

The height of the barrier can roughly be approximated by the average work function of sample and tip.

When the tip of the STM probe is sufficiently close to the surface of the specimen (~ 1nm) a tunneling current can become established

Ideally a STM probe tip is very pointed (1-2 atoms at the end) and has a relatively low work function. Etched tungsten crystals are ideal and are nearly identical to field emitters.

The tunneling current is exponentially proportional to the distance and thus via a feedback loop the tip can be maintained at a constant distance from the surface by maintaining a constant tunneling current.

If the tunneling current is kept constant the Z position of the tip must be moved up and down. If this movement is recorded then the topography of the specimen can be inferred.

Alternatively if the Z position of the tip is kept constant the tunneling current will change as it moves across the surface. If the changes in current are recorded the then the topography of the specimen can be inferred.

The probe is scanned over the surface in a raster pattern similar to that of a SEM or Confocal. Each coordinate (X,Y, & Z) is recorded by a computer.

The ability to precisely position the probe of an STM is made possible by an XYZ PiezoScanner which coupled to a feedback regulator keeps track of the tunneling current and precisely positions the tip accordingly.

Crystals which acquire a charge when compressed, twisted or distorted are said to be piezoelectric. Piezoelectric ceramic materials have found use in producing motions on the order of nanometers in the control of STMs and other devices.

The Piezoelectric Effect:

Forces applied to a segment of material lead to the appearance of electrical charge on the surfaces of the segment. The specific distribution of electric charges in the unit cell of a crystal is the source of this phenomenon.

Surface of Platinum

Iron corrals on Cu

Positioning of atoms for a mass data storage system

~ ATOMIC FORCE MICROSCOPE ~

HOW DOES IT WORK?
Feedback Loop

Laser V Piezo Crystal Photodiode Mirror

Tip

ThermoMicroscopes Explorer AFM

Substrate

The atomic force microscope (AFM), uses a sharp tip attached to the end of a cantilever rasters across an area while a laser and photodiode are used to monitor the tip force on the surface. A feedback loop between the photodiode and the piezo crystal maintains a constant force during contact mode imaging and constant amplitude during intermittent contact mode imaging.

INTRODUCTION
Atomic Force Microscope(AFM) is a type of scanning probe microscope(SPM) .These microscopes donot use light as conventional microscopes, but rather scan a sharp probe over a surface to image extremely small surface structures(0.1nm resolution).It generates a 3D map of the sample surface.AFM is used to solve materials problems in a wide range of technologies affecting the electronics, telecommunications, biological, chemical, automotive, aerospace, and energy industries. The materials being investigating include thin and thick film coatings, ceramics, composites, glasses, synthetic and biological membranes, metals, polymers, and semiconductors. The AFM is being applied to studies of phenomena such as abrasion, adhesion, corrosion, etching, friction, and polishing. By using AFM one can not only image the surface in atomic resolution but also measure the force at nano-newton scale.

BACKGROUND
The first AFM was made by gluing a tiny shard of diamond onto one end of a tiny strip of gold foil.

In 1986 Binnig and Gerber used the cantilever to examine insulating surfaces. A small hook at the end of the cantilever was pressed against the surface while the sample was scanned beneath the tip. The force between tip and sample was measured by tracking the deflection of the cantilever. This was done by monitoring the tunneling current tot a second tip positioned above the cantilever.
Albrecht, a fresh graduate student, fabricated the first silicon microcantilever and measured the atomic structure of boron nitride. Today the tip-cantilever assembly is microfabricated from Si or Si3N4. The era of AFM came finally when the Zurich group released the image of a silicon (111) 7X7 pattern.

OPERATION
An atomically sharp tip is scanned over a surface with feedback mechanisms that enable the piezo-electric scanners to maintain the tip at a constant force (to obtain height information), or height (to obtain force information) above the sample surface. The nanoscope AFM head employs an optical detection system in which the tip is attached to the underside of a reflective cantilever. A diode laser is focused onto the back of a reflective cantilever. As the tip scans the surface of the sample, moving up and down with the contour of the surface, the laser beam is deflected off the attached cantilever into a dual element photodiode. The photo detector measures the difference in light intensities between the upper and lower photo detectors, and then converts to voltage. Feedback from the photodiode difference signal, through software control from the computer, enables the tip to maintain either a constant force or constant height above the sample. In the constant force mode the piezo-electric transducer monitors real time height deviation. In the constant height mode the deflection force on the sample is recorded.

As with the STM the probe tip of an AFM must be very small but because there is no need to establish a tunneling current one can use a variety of materials, not just those with a low workfunction.

Similar to a phonograph needle the probe is actually in contact with the specimen and is physically moved up and down due to the repulsion of van der Waals forces

The AFM records the position of the probe by bouncing a laser off the back surface of the probe and recording how the light is deflected

By using a four quadrant detector the relative amount of laser light hitting each quadrant can be used to determine how the tip has been deflected as it moves over the surface of the specimen

AFM of Chromosome
Since an AFM relies on AFM derived models of contact rather than nuclear pore complex current many nonconductive materials can be examined

Since the contact of the tip with the specimen can cause physical damage to the specimen many AFMs employ a tapping mode in which the probe vibrates up and down as the sample is moved.

~ ATOMIC FORCE MICROSCOPE ~

WHAT CAN WE LEARN?

Imaging direction
Elasticity
TIP

Rc

Height

Friction
Width

AFM Image and manipulation of an Adenovirus.

Binding

A recent development uses an AFM to write with biomolecules such as DNA sequences. This will allow for the creation of micro DNA chips which can be used a wide variety of applications

AFM vs. STM

Resolution is largely dependent on probe size and the ability to control scanning. STM requires a conductive specimen, AFM do not and both of these can be used in air, vacuum, or in liquids.
AFM physically contact the specimen but STM do not.

A schematic of an atomic force microscope is shown in the diagram below. The sample is mounted on a piezo ceramic which can be moved extremely accurately in the x, y and z directions. The sample is then rastered in the x and y directions under a sharp tip. This tip is mounted at the free end of a cantilever (as shown) onto which a laser beam is focussed. The beam is reflected from the back of the cantilever to a set of four photosensitive diodes. These act to detect any deflection of the laser beam arising from the cantilever moving as the sample is rastered. A feedback loop then acts to move the piezo in the z direction taking the laser beam back to its original position. In this way the sample is scanned with a constant force and the resulting z piezo motion produce a How the AFM works. topographical map of the region scanned with a vertical resolution much smaller than 1A; in favorable cases. The AFM can be used in a variety of environments, in air,in UHV or under liquids.

THE TECHNICAL STUFF

The Tip :
It is usually made of silicon or silicon nitride. The end of this tip is often slightly rounded being around 10 nm in radius. Silicon nitride tip is found better than silicon tip.

 The Cantilever :

The AFM tip is held at the end of a thin cantilever. Cantilevers are made by microlithography processes similar to those used in the fabrication of computer chips. Sample can be

The Scanner :

moved under the AFM tip in two ways, 1) In first we move the sample and keep the tip at fixed place (shown blue). 2) In second we move the tip over the stationary sample.

 The Height Transducer : In AFM the height

changes of the tip as it passes over the sample are usually monitored using a laser beam which is reflected by the cantilever as shown.This reflected beam gives information about the movement of the cantilever and tip.

 Feed Back Operation : AFM can be operated

in two principle modes to control the tip and its response 1) With Feed Back Control, this is also called high gain or constant force /varing height mode. 2) With out Feed Back Control, this is also called no gain or varing force /constant height mode. Here tip height is allowed to fluctuate (as shown).

TIP SAMPLE INTERACTION

As the distance between the tip and the sample surface is reduced by moving the sample with a

piezoelectric actuator towards the tip, one can easily detect the effect of repulsive /attractive forces.

Tip sample interaction is one of the ways by which image contrast is obtained. The three main classes of interaction are 1) Contact mode 2) Tapping mode (intermittent contact mode) 3) Non contact mode

 Contact Mode :
1-In this method of AFM operation tip
and the sample remain in close contact as the scanning proceeds. 2- By contact we mean the repulsive regime of the intermolecular force curve. 3-A feed back loop maintains a constant deflection between the cantilever & the sample by vertically moving the scanner at each (X,Y) data point. 4-The force constant range from 0.01 to 1.0 N/m. 5-Operation can occur in ambient air and liquid environment.

 Tapping mode :
1-In this method of AFM operation the cantilever oscillates at fix resonance frequency (~hundreds of kilo hertz) & positioned above the surface so that it only taps the surface for a very small friction of its oscillation period. 2-This reduces the lateral forces quickly as the tip scans over the surface for a little time 3-So a tapping AFM image is produced by imaging the force of the oscillating contacts of the tip with the sample surface.

 Non Contact Mode :

1-Here cantilever oscillates slightly above its resonance frequency (amplitude of ~10 nm) 2-Tip does not contact the sample surface, but oscillates above the adsorbed surface fluid layer during scanning. 3-The cantilevers resonant frequency is decreased by the van der waals forces, which extend for 1 to 10 nm above the adsorbed fluid layer & by other long range forces. 4-Feed back loop maintains constant oscillation amplitude or frequency.

AFM IMAGING MODE COMPARISON

CONTACT MODE TIPS/ CANTILEVERS

TAPPING MODE TIPS/ CANTILEVERS

APPLICATIONS OF AFM
1) It can measure the friction between tip and the sample:
In AFM topographic imaging uses the up & down deflection of the cantilever while friction imaging uses torsional deflection (as shown).

Simultaneous friction & topography image of graphite atom in which topography image as a 3D projection coloured by the friction data is shown. Each bump represents one carbon atom. As the tip moves from right to left, it bumps in to an atom and gets stuck behind it. The scanner continues to move & lateral force builds up until the tip slips past the atom and sticks behind the next one. This stick-slip behaviour creates a characteristic saw-tooth wave form in the friction image .

2) AFM can measure sample elasticity :

It can image sample elasticity by pressing the tip in to the sample & measuring the resulting cantilever deflection. The harder the sample, the more the cantilever deflection.

3) It can identify individual surface atoms:

The atom at the apex of the tip senses individual atoms on the underlying surfaces when it forms incipient chemical bonds with each atom. Because these chemical interactions alter the tip vibration frequency, they can be detected and mapped.

4) It can image non conducting surfaces :

Because of this property AFM is widely used in the biological systems such as analyzing the crystals of amino acids.

5) In force distance measurement :

The AFM tip is approached towards & retracted from the surface & the static deflection of the cantilever is monitored as a function of the piezodisplacement. These measurements have been used to measure nanoscale contacts, atomic bonding, van der waals & hydration /solvation forces in liquids. Forces of the order of a few pN can be measured with a vertical distance resolution of better than 0.1 nm.

AFM Images

COMPARISON OF AFM WITH OTHER IMAGING TECHNIQUES

In some cases, the resolution of STM is better than AFM because of the exponential dependence of the tunneling current on distance. The force -distance dependence in AFM is much more complex when characteristics such as tip shape and contact force are considered. STM is generally applicable only to conducting samples while AFM is applied to both conductors and insulators. Furthermore, the AFM offers the advantage that the writing voltage and tip-to-substrate spacing can be controlled independently, whereas with STM the two parameters are integrally linked. Compared with Scanning Electron Microscope, AFM provides extraordinary topographic contrast direct height measurements and unobscured views of surface features (no coating is necessary). Compared with Transmission Electron Microscopes, three dimensional AFM images are obtained without expensive sample preparation and yield far more complete information than the two dimensional profiles available from cross-sectioned samples.

AFM versus STM:

AFM versus SEM:

AFM versus TEM: