Introduction to Atomic Force Microscopy

Dr. Janelle Gunther March 10, 1998

ACS Group and MENs, Beckman Institute

adapted from the world wide web page at http://www.di.com Digital Instruments, Santa Barbara, CA

Scanning Probe Microscopy (SPM)

A family of microscopy forms where a sharp probe is scanned across a surface and some tip/sample interactions are monitored Scanning tunneling Microscopy (STM) Atomic Force Microscopy (AFM) contact mode non-contact mode TappingMode Other forms of SPM Lateral force Force modulation Magnetic or electric force surface potential scanning thermal phase imaging

Multimode SPM

General AFM Beam Deflection Detection

A B Solid State Laser Diode

Cantilever and Tip

Used for Contact Mode, Non-contact and TappingMode AFM Laser light from a solid state diode is reflected off the back of the cantilever and collected by a position sensitive detector (PSD). This consists of two closely spaced photodiodes. The output is then collected by a differential amplifier Angular displacement of the cantilever results in one photodiode collecting more light than the other. The resulting output signal is proportional to the deflection of the cantilever. Detects cantilever deflection <1A

Piezoelectric Scanners
SPM scanners are made from a piezoelectric material that expands and contracts proportionally to an applied voltage. Whether they expand or contract depends upon the polarity of the applied voltage. Digital Instruments scanners have AC voltage ranges of +220 to -220V. 0V

+V
-V

No applied voltage

Extended

Contracted

In some versions, the piezo tube moves the sample relative to the tip. In other models, the sample is stationary while the scanner moves the tip. AC signals applied to conductive areas of the tube create piezo movement along the three major axes.

Contact Mode AFM

A tip is scanned across the sample while a feedback loop maintains a constant cantilever deflection (and force) The tip contacts the surface through the adsorbed fluid layer. Forces range from nano to micro N in ambient conditions and even lower (0.1 nN or less) in liquids.

Tapping Mode AFM

A cantilever with attached tip is oscillated at its resonant frequency and scanned across the sample surface. A constant oscillation amplitude (and thus a constant tip-sample interaction) are maintained during scanning. Typical amplitudes are 20-100nm. Forces can be 200 pN or less The amplitude of the oscillations changes when the tip scans over bumps or depressions on a surface.

Non-contact Mode AFM

The cantilever is oscillated slightly above its resonant frequency. Oscillations <10nm The tip does not touch the sample. Instead, it oscillates above the adsorbed fluid layer. A constant oscillation amplitude is maintained. The resonant frequency of the cantilever is decreased by the van der Waals forces which extend from 1-10nm above the adsorbed fluid layer. This in turn changes the amplitude of oscillation.

Advantages and Disadvantages of the 3 main types of AFM

Contact Mode

Advantages:
High scan speeds The only mode that can obtain atomic resolution images Rough samples with extreme changes in topography can sometimes be scanned more easily

Disadvantages:
Lateral (shear) forces can distort features in the image The forces normal to the tip-sample interaction can be high in air due to capillary forces from the adsorbed fluid layer on the sample surface. The combination of lateral forces and high normal forces can result in reduced spatial resolution and may damage soft samples (i.e. biological samples, polymers, silicon) due to scraping

Lateral Force Microscopy

The probe is scanned sideways. The degree of torsion of the cantilever is used as a relative measure of surface friction caused by the lateral force exerted on the probe.

Identify transitions between different components in a polymer blend, in

Lateral Force Microscopy

Images/photo taken with NanoScope SPM, courtesy Digital Instruments, Santa Barbara ,CA

Natural rubber/ EDPM blend 20 micron scan

Polished polycrystalle silicon carbide film. Grain structures 30 micron scan Magnetic recording head Al oxide grains and contamination 800nm scan

Phase Imaging
Accessible via TappingMode Oscillate the cantilever at its resonant frequency. The amplitude is used as a feedback signal. The phase lag is dependent on several things, including composition, adhesion, friction and viscoelastic properties.

Identify two-phase structure of polymer blends Identify surface contaminants that are not seen in height images Less damaging to soft samples than lateral force microscopy

Phase Imaging
Image/photo taken with NanoScope SPM, courtesy Digital Instruments, Santa Barbara ,CA

Compositepolymer imbedded in a matrix 1 micron scan

Bond pad on an integrated circuit Contamination 1.5 micron scan

MoO3 crystallites on a MoS2 substrate 6 micron scan

Magnetic Force Microscopy

Special probes are used for MFM. These are magnetically sensitized by sputter coating with a ferromagnetic material. The cantilever is oscillated near its resonant frequency (around 100 kHz). The tip is oscillated 10s to 100s of nm above the surface Gradients in the magnetic forces on the tip shift the resonant frequency of the cantilever . Monitoring this shift, or related changes in oscillation amplitude or phase, produces a magnetic force image. Many applications for data storage technology

Magnetic Force Microscopy

Image/photo taken with NanoScope SPM, courtesy Digital Instruments, Santa Barbara ,CA

Overwritten tracks on a textured hard disk, 25 micron scan

Domains in a 80 micron garnet film

LiftMode

Two passes are made over the sample. The first measures topography while the second measures a material property (magnetic, electric, etc.) Eliminates cross-contamination of the images.

Force Modulation Imaging

Oscillate the cantilever vertically at a rate that is significantly faster than the scan rate. The amplitude of the oscillations changes in response to the sample stiffness. Used in conjunction with LiftMode to separate topography and elasticity data.

Force Modulation Imaging

Other Techniques
Image/photo taken with NanoScope SPM, courtesy Digital Instruments, Santa Barbara ,CA

Scanning capacitance microscopy Apply a constant amplitude sine wave voltage to the sample. The image is then reconstructed from the changes in the amplitude of the capacitance oscillations. Location of defects in wafers (pinning of electrical carriers) Image carrier concentration Scanning thermal microscopy Uses a temperature sensitive probe with a special holder. Location of hot-spot defects in semiconductor wafers
90 micron scan size

Other Techniques
Nanoindenting and scratching A diamond tip is mounted on a metal cantilever and scanned either with contact or TappingMode. Indenting mode presses the tip into the sample Scratch mode drags the tip across the sample at a specific rate and with a specified force. The use of TappingMode makes it possible to simultaneously image soft samples.

Imaging of biological samples cells, DNA (TappingMode in solution)