Lecture 10 AFM
Lecture 10 AFM
History and background of AFM; Basic component of an AFM; Tip-Sample interactions and feedback mechanism; Atomic force and different scanning modes; AFM tips and resolution.
Atomic force microscopy (AFM) was developed when people tried to extend STM technique to investigate the electrically non-conductive materials, like proteins.
In 1986, Binnig and Quate demonstrated for the first time the ideas of AFM, which used an ultra-small probe tip at the end of a cantilever (Phys. Rev. Letters, 1986, Vol. 56, p 930).
In 1987, Wickramsinghe et al. developed an AFM setup with a vibrating cantilever technique (J. Appl. Phys. 1987, Vol. 61, p 4723), which used the light-lever mechanism.
Cantilever Deflection Measured by Tunneling current. Disadvantages: Difficult alignment; Sensitivity of ~0.01 , but extremely sensitive to surface conditions, Thermal drifts, local changes in barrier height affect force measurements
The Cavendish Experiment: another example of light lever for precise spatial measurement
Since 1679, Sir Isaac Newton proposed the law of universal gravitation; In 1798, Sir Henry Cavendish determined, for the first time, the constant G.
The resolution of the 2D scanning depends on the step size and the number of scanning lines, as well as the tip sharpness as to be discussed below.
Optical and electron microscopes can easily generate two dimensional images of a sample surface, with a magnification as large as 1000X for an optical microscope, and a few hundreds thousands ~100,000X for an electron microscope. However, these microscopes cannot measure the vertical dimension (z-direction) of the sample, the height (e.g. particles) or depth (e.g. holes, pits) of the surface features. AFM, which uses a sharp tip to probe the surface features by raster scanning, can image the surface topography with extremely high magnifications, up to 1,000,000X, comparable or even better than electronic microscopes. The measurement of an AFM is made in three dimensions, the horizontal X-Y plane and the vertical Z dimension. Resolution (magnification) at Z-direction is normally higher than X-Y.
Carbon Nanotubes
Atomic interaction
Repulsion:
At very small tip-sample distances (a few angstroms) a very strong repulsive force appears between the tip and sample atoms. Its origin is the so-called exchange interactions due to the overlap of the electronic orbitals at atomic distances. When this repulsive force is predominant, the tip and sample are considered to be in contact.
Friction:
The SFM cantilever bends laterally due to a friction force between the tip and the sample surfaces --- lateral force microscope (LFM).
Adhesion:
Adhesion can be defined as the free energy change to separate unit areas of two media from contact to infinity in vacuum or in a third medium. In general, care has to be taken with the term adhesion, since it is also used to define a force - the adhesion force, as for example in force modulation microscope. In FMM at ambient conditions, in addition to the intrinsic adhesion between tip and sample, there is another one from the capillary neck condensing between the tip and water meniscus --- interference from the huminity. The pull-off force is considered as the adhesion force, which is in the range of a few nanonewton to tens of nanonewton.
The snap-in distance increases with the relative humidity, up to 10-15 nm.
Electrostatic interaction:
Caused by both the localized charges and the polarization of the substrate due to the potential difference between the tip and the sample. It has been used to study the electrostatic properties of samples such as microelectronic structures, charges on insulator surfaces, or ferroelectric domains.
Magnetic interaction:
Caused by magnetic dipoles both on the tip and the sample. This interaction is used for Magnetic Force Microscopy to study magnetic domains on the sample surface.
Contact mode (left): the deflection of cantilever is kept constant. Non-contact mode (right): the tip is oscillated at the resonance frequency and the amplitude of the oscillation is kept constant. Tapping mode: somewhere between the contact and non-contact mode.
Non-Contact
Contact
to the sample
Contact mode imaging (left) is heavily influenced by frictional and adhesive forces, and can damage samples and distort image data. Non-contact imaging (center) generally provides low resolution and can also be hampered by the contaminant (e.g., water) layer which can interfere with oscillation. Tapping Mode imaging (right) takes advantages of the two above. It eliminates frictional forces by intermittently contacting the surface and oscillating with sufficient amplitude to prevent the tip from being trapped by adhesive meniscus forces from the contaminant layer.
Contact,
Non-Contact,
Tapping
Nanografting
Contact-Mode scanning Lateral force microscope (LFM) --- surface friction. Force modulation microscope (FMM) --- detecting surface stiffness or elasticity; Tapping-Mode scanning Phase mode imaging --- detecting surface structure or elasticity property.
LFM measures lateral deflections (twisting) of the cantilever that arise from forces on the cantilever parallel to the plane of the sample surface. LFM images variations in surface friction, arising from inhomogeneity in surface material. LFM imaging is also enhanced by edge deflection (slope variations) of surface feature. This differentiates from the imaging of different materials by two sharp changes (up/down) at both sides.
Topography
Friction image
2m x 2m section on a Ni CD-stamper matrix. The friction image presents a more detailed surface structure then the topography image. Bright areas correspond to higher friction.
T.Gddenhenrich, S.Mller and C.Heiden, Rev. Sci. Instrum. 65, (1994) 2870
technique
topography
Elasticity by FMM
The elasticity image reveals that each of the bumps is soft relative to the silicon substrate, a reasonable result for protein molecules.
FMM
FMM gives more detailed information about the composition and distribution of the two components --- soft polymer (dark area) and hard carbon fiber.
topography
FMM
Contact mode topography (left) and force modulation image (right) of carbon black deposit in automobile tire rubber. 15m scan. Veeco.
topography
FMM
Contact mode topography (left) and force modulation image (right) of a twophase block copolymer. The softer, more compliant component of the polymer maps in black. 900nm scans. Veeco.
Phase imaging monitors the phase lag between the signal that drives the cantilever to oscillate and the cantilever oscillation output signal. In TappingMode AFM, the cantilever is excited into resonance oscillation with a piezoelectric driver. Phase imaging is used to map variations in surface properties such as elasticity, adhesion and friction, which all may cause the phase lag. Phase detection images can be produced while an instrument is operating in any vibrating cantilever mode, such as tapping mode AFM, MFM, EFM. The phase lag is monitored while the topographic image is being taken so that images of topography and material properties can be collected simultaneously ---- direct correlation between surface properties and topographies.
Identification of contaminants; Mapping of different components in composite materials; Differentiating regions of high and low surface adhesion or hardness; Mapping of electrical and magnetic properties with wide-ranging implications in data storage and semiconductor industries. In many cases, phase imaging complements lateral force microscopy (LFM), and force modulation microscopy (FMM), often providing additional information more rapidly and with higher resolution. Phase imaging is as fast and easy to use as Tapping-Mode AFM with all its benefits for imaging soft, adhesive, easily damaged or loosely bound samples.
Non-contact AFM
Phase image
Non-contact AFM
Phase image
Phase imaging tells the homogeneity of the coating regardless the roughness of the original alumina surface. This cannot be seen from the height imaging (left).
Non-contact AFM
Phase image
Phase (top) and Tapping-Mode (bottom) images of wood pulp fiber. The phase image highlights cellulose microfibrils. In addition, a lignin component appears as light areas in the phase image, but is not apparent in the topography image. 3m scan. Veeco.
Measured width: distance between the 1st and last tip/sample contact; The smaller the tip (Rtip), the smaller the measured width; When Rtip ~ Rsample, measured width = 2Rsample; For a 5 nm feature (say a particle), the tip apex size must be ~ 1 nm to get a reliable lateral measurement --- quite challenging! Normal tip size, ~ 20 nm or larger. Another challenge for lateral imaging: to differentiate two adjacent features.
Large tip measures a feature apparently larger than the real size; Larger tip cannot discern two or more adjacent features. Higher resolution demands sharper tips.
AFM Tips
Normal Tip
Supertip
Ultralever
AFM Tips
Diamond-coated tip
FIB-sharpened tip
15 nm
Obtained by, EnviroScope AFM, Veeco. Imaging in fluid requires long tips
Imaging small features and scanning small area at high resolution require ultra-sharp tips. JOURNAL OF BIOLOGICAL CHEMISTRY, Vol. 278, No. 24, Issue of June 13, pp. 2165521662, 2003
Common commercial cantilever: Si3N4 and SiO2 Resonance frequency of the cantilever,
1 k 0.5 f0 = ( ) 2 m0
Ewt 3 k= 4l 3
The softer the lever (smaller k), the better for sensing the deflection, but requires smaller mass to keep the high frequency. Why high f needed?
k: the spring constant, E: Young module; t: thickness; l: length; w: width, m0 the effective mass of the lever.
V-shape cantilever
Common commercial cantilever: Si3N4 and SiO2 Resonance frequency of the cantilever,
1 k 0.5 f0 = ( ) 2 m0
Ewt 3 k= 4l 3
The softer the lever (smaller k), the better for sensing the deflection, but requires smaller mass to keep the high frequency.
k: the spring constant, E: Young module; t: thickness; l: length; w: width, m0 the effective mass of the lever.
Pit etching in Si
Si3N4 coating
Si underetching