Pacific Nanotechnology Inc.

An introduction to Atomic Force Microscopy Modes

Paul West and Arthur Ross

Principles and Components

Core elementsAs originally conceived, the AFM (see Figure 2-1) was a surface profiling device. A nanometer- scale probe, mounted at the end of a tiny cantilever, is held in contact with the surface using piezoelectric positioning. Deflection of the cantilever, easily measured optically, indicates force between probe and surface. That force is held nominally constant by a feedback control system while the probe is scanned raster- fashion across the surface. The control voltage indicates elevation as a function of transverse position. The elevation can be displayed or recorded in various ways, providing a topogram of the surface. The resolution, limited by the probe tip radius, is of the order of a few tens of nanometers, with fields-of-view of the order of a few tens of microns.
Subsequent to those original demonstrations, many variations on this basic design have been developed. Oscillatory sensing was introduced for improved performance and for field gradient sensitivity. While all of them measure cantilever deflection as a positioning aid, the feedback control error signal can be derived in several ways. And exactly what constitutes a surface "profile" can be defined variously, depending upon ones objectives.

This chapter described the basic AFM instrument and some of its possible variations.

Coordinate system. We adopt the convention that the X and Y coordinate axes are nominally parallel to the surface under test (SUT), and the Z axis completes a right handed Cartesian coordinate system, as shown in Figure 2-1. The Z axis positioner thus moves the probe perpendicular to the SUT, while the X and Y positioner move the probe in a nominal object image plane.
Topography by quasi-static probe contact
In contact mode, the cantilever is scanned over a surface at nominally constant force. The Z axis PZT feedback loop, if properly implemented, ensures near constancy of cantilever deflection, which corresponds to constant force.

Contact mode is typically used for scanning hard samples and when a resolution of greater than 20 nanometers is required. The cantilevers used for contact mode are usually silicon or silicon nitride. Typical resonant frequencies are about 50 KHz and force constants are below 1 N/m.
contact mode images
Probes
AFM probe-cantilevers assemblies are readily available from commercial vendors. They are generally made of silicon or silicon nitride, taking advantage of the highly-developed techniques of micro lithographic for fabrication. Figure 2-3 shows SEM images of some representative tips.

The sharpness of the probe is a primary determinant of the resolution of the AFM. Probe tips are approximately spherical, and are characterized by an effective radius. A typical probe radius is in the neighborhood of 10-20 nm. Special "supersharp" tips of even smaller radii, approaching 1 nm, are offered, these being more suitable for probing narrow structures.

probe tips
Probe coatings. Probes are often used with various coatings for sensing particular phenomena. For use with the light lever detection system, the cantilever backside is aluminized for high optical reflectivity. Available probe coatings include:

Figure 2-4 shows some SEM images of probe tips at very high magnification.
diamond
Cantilever stiffness
For small deflections of the probe relative to its equilibrium (non-contact) position, the force versus distance characteristic is, to a good approximation, linear. The force can thus be approximated by Hooke's law:
Hook's Law
Because of the strong analogy to the simple mass-spring oscillator so familiar from elementary physics classes, we will often call k the cantilever "spring constant", tho the terminology is not rigorously appropriate.
k can be calculated if the dimensions and composition of the cantilever are known. Most commercially available cantilevers are supplied with a value for k , but these are often unreliable. For best results, Sader's method is recommended. The length and width of the cantilever are measured with an optical microscope and an approximate mechanical Q is measured by scanning the excitation frequency while observing the mechanical response. From those the effective spring constant can be calculated.

Lateral compliance
Lateral forceAs illustrated in Figure 2-5 the cantilever in an AFM can bend, and twist as it is scanned across a surface. The horizontal forces are dependent upon the so-called "asperity" of the surface (its abrasive nature) relative to the probe, that is, the sliding friction between probe and surface. Typically the compliance for twisting is much less than the compliance for bending. The twisting sensitivity, of course, is to the forces that exert a moment around the cantilever's major axis, that is, forces perpendicular to the axis of the cantilever and parallel to the SUT.

Probe position sensing
Light lever. High sensitivity in the force transducer of an AFM can be achieved by a simple geometric optical device known as the light lever (see Figure 2-6). A low-power laser beam is reflected from the top of the cantilever to a distant photo detector. Small displacements of the cantilever result in large displacements of the laser beam at the location of the detector due simply to the large "lever arm" of the light path.
Force Sensor
Deflection and TorsionPosition sensitive detector. Cantilever torsion is measured by an enhancement of the light lever. A four-quadrant position sensitive detector (PSD) is used with the signals added and subtracted as shown in Figure 2-7 to give equivalent vertical and horizontal displacements. Because the vertical and lateral deflections are substantially independent of one another, it is possible to measure topography and lateral friction force independently (see §). Because the physical dimensions of commercially available cantilevers are not well characterized, the elasticity coefficients must be calculated individually for each cantilever from measured dimensions and material properties.
Optical interferometry. Some practitioners have used optical interferometry on the cantilever for extreme sensitivity to Angstrom-scale deflection (see, for example, Martin et al, (1987) for a heterodyne technique, Erlandsson et al, (1988) for non-heterodyne). While the potential sensitivity of interferometry is higher (sub-A) than that of the light lever, its cost and complexity discourage its use for all but the most demanding applications.

Probe-surface interactions

While it might be thought that the force between an AFM probe and a hard surface might have an abrupt brick wall character, this is an over-simplification at the nanoscopic scale. Not only are fundamental interatomic forces finite in extent, there is also the problem of surface contamination. AFMs are usually operated in ambient environmental conditions (room temperature, atmospheric pressure, ambient air). As a result, there is invariably a surface layer comprised of water and miscellaneous hydrocarbons. This layer is thick enough relative to the nominal probe operating height that the probe tip is almost always immersed in it (see Figure 2-8), forming a meniscus that complicates near-surface operation.
In ambient air the AFM probe must pass through surface contamination
The forces between probe and surface, to the extent that they are position-dependent only, i.e. are lossless, can be represented by an effective potential energy (see Figure 2-9).
energy diagram
There are three basic regions of interaction between the probe and surface:


Piezoelectric transducer (PZT) positioning The X-Y resolution of the measurements possible in an AFM are of the order of the tip radius, which is typically are a few tens of nm, and can be as small as just a few nm. If one postulates an image area of 1000 x 1000 pixels (a rather high resolution digital image), at, say, 20 nm per pixel, then the actual imaged area is 20 µ m by 20 µ m. This is far too small for simple mechanical positioning. A far better solution is the use of piezoelectric ceramic positioners.

Piezoelectrics are materials that expand or contract in the presence of internal voltage gradients (that is, bulk electric fields). The magnitude of the piezoelectric phenomenon makes these devices quite appropriate as nanometer-scale actuators (see, for example, Gallégo-Juarez (1989)). Piezoelectric actuators can produce, under electronic control, extremely fine position control down to the nanometer scale required by an AFM. The motion is smooth, with no thresholds or "stickiness" characteristic of electromechanical devices. The are non-magnetic, making them suitable for applications that are magnetic-field sensitive. They are also capable of extremely high accelerations, as much as thousands of g 's, in combination with high forces, upwards of thousands of newtons. There is no observable mechanical wear, in most applications.

Traditionally the PZT positioning in AFMs is done by a one-piece tubular actuator. Four electrodes in a quadrant configuration cover the outside, while a full-circumference electrode covers the inside. Voltages applied to opposite quadrant pairs causes tilt along the axis of symmetry. Simultaneous voltage on all four quadrants causes elongation or contraction. The major virtue of this design is its mechanical simplicity: one instrument provides motion in all three coordinate axes. It does, however, have some drawbacks:

Of these, the most objectionable is perhaps the scan rate limitation. Achievable rates in typical units are so slow that a full frame scan can take many minutes. Various speedup schemes, such as the dual feedback controller scheme of Egawa et al (1999) have been tried, with mixed success. This particular scheme used, as have others, a supplementary PZT actuator on the cantilever, in addition to the principal tube-style 3D actuator. This sort of dual actuator configuration is especially applicable to vibrating cantilever mode (VCM). The PZT tube actuator provides coarse Zaxis positioning, but with slow dynamics, while the cantilever actuator provides fast, fine-grained dynamics for both Z-axis positioning and cantilever drive.

The Proportional-Integral-Differential (PID) Feedback Controller.
Most AFM schemes for generating topography images make use of some sort of feedback control system in conjunction with their error measurement and Z-axis actuator. The design and implementation of such a feedback control system is non-trivial. The design is driven by unavoidable trade-offs between tracking accuracy, speed, and stability. The simple, naive design will almost always result in instability, entailing not only failure to track properly, but also damage or destroy) the probe and sometimes damage the SUT. While a simple solution is possible, optimized solutions require considerable sophistication in both analysis and implementation.

The AFM, when tracing SUT topography, might be regarded as a special case of the age-old generic process control model shown in Figure 2-10 (upper).

The traditional industrial process control mechanism for a poorly-defined and/or inherently nonlinear process is the so-called proportional-integral-differential (PID) controller. With reference to Figure 2-10, the process drive y ( t ) is generated as a sum
process control mechanism
Feedback controller
Such a control mechanism is easily analyzed using LaPlace transforms and well-known techniques if the overall system, that is the "plant" plus feedback amplifier, is linear and time invariant. In the case of the AFM, however, the probe plus cantilever plus PZT actuator system is only approximately linear. Moreover, even the dynamics in the linear approximation are not easily characterized. Cantilever resonances are usually at tens of kHz and unimportant in topography following. The typical tubular PZT actuator, however, has resonances in the neighborhood of a few kHz. These are significant and do affect topography tracking.

The goals of the feedback controller design are straightforward:


The first and second of these are generally trade-offs against one another. Arbitrarily tight following can be accomplished at the expense of extremely slow transient response, that is, of low closed loop bandwidth. Rapid scanning can be achieved at the expense of large tracking error. The tradeoff is, of course, a consequence of the stability requirement, which is absolute. A loop is either stable or unstable, the latter being intolerable.

The usual solution in the practice of AF microscopy is to tune the PID coefficients semi-heuristically. Such techniques are well-established in the literature of industrial process control. While they do result in a stable system, its bandwidth is not large, thus limiting the usable scan speed. Scanning speed is an especially important issue. AFMs using a simple PID style of feedback controller can take many minutes to complete an image.

As noted above, the limiting factor in the loop design is usually the PZT actuator, which usually has internal mechanical resonances in the neighborhood of a few khz. This is orders of magnitude slower than the cantilever resonances. The cantilever itself thus is generally not significant in limiting the closed loop bandwidth.

Schitter et al. (2001), recognizing the importance of the PZT in limiting system performance, carefully characterized their PZT actuator dynamics through the mathematical tool known as system identification. System identification is the creation of a linear system model using only observations of input and output, rather that physical modelling. This is especially useful for the PZT, physical modelling of which would be a very complex mathematical problem. System identification, on the other hand, is relatively simple, producing directly a useful pole-zero model.

model Schitter et al.Using that model Schitter et al. then generated a controller using the H control system criterion (see, for example, Skogestad and Postlethwaite (1996)). This design was implemented, and displayed significant improvement in transient response (Figure 2-11).

Details of this sort of analysis and design are beyond the scope of this paper, but they are well-known and are documented in modern control theory textbooks (e.g. references found in the Schitter et al. (2001) paper).

Subsequent sections of this paper show a simple "feedback amplifier." These should always be understood as the classic PID controller, with the proviso that more sophisticated designs may yield substantial performance improvements.

Observing the Elevation. Note in Figure 2-10 the presence of an elevation estimator whose inputs are the PZT control voltage and the cantilever deflection. This is a correction that is required of all AFM feedback schemes, though we may, for simplicity, omit it in system diagrams. The reason is simple. Even if we assume that we know the actuator position with complete precision, the actual position of the probe tip is the sum of that actuator position and the cantilever deflection. That is to say, the actuator sets the equilibrium position of the probe, while the surface interaction deflects the probe away from that equilibrium position. One must add (or subtract, depending on mechanical design details) the two to obtain the true probe tip position. In more sophisticated designs, that is, ones that account for the PZT dynamics, one must also account for the fact that the actuator position lags its control voltage because of the mechanical resonances. While we will, in subsequent sections, show the amplifier output as an analog of position, suitable for recording, this is an over-simplification if one is trying to do precision work.
Quasi-static (QS) operation
"Quasi-static" here denotes operation where the relationship between applied force and displacement is not significantly affected by inertia (mass) of the probe; the probe position thus represents only a static force balance. "Quasi" is prefixed to show that probe motion is possible, tho scanning is slow. Such operation is primarily applicable to surface following.

"Contact mode" might be considered to be simply a high-force form of quasi-static operation, though all QS operation is not necessarily contact mode. Care should be used in reading too much into the terminology, as it is often used loosely.

A typical quasi-static system architecture is shown in Figure 2-12. A feedback control loop adjusts the equilibrium probe position so that the deflection matches a setpoint, thus keeping the force constant. The actuator control voltage thus represents the surface profile as defined by constant static force. That profile may vary slightly, depending on the exact value of the setpoint and the steepness of the force profile.
Quasi static
A Q-S topogram may be generated simultaneously with measurements of specific physical surface properties, or it may be itself the primary objective.
Vibrating Cantilever Mode (VCM)

In order to make more sensitive measurements, requiring better signal/noise ratios, in scientific instruments it is common to modulate the signal being measured and use phase or amplitude detection circuits. Use of modulated techniques shifts the measurement to a higher frequency regime where there is less 1/f noise. Vibrating probes also can be sensitive to near-surface force gradients, such as arise from surface polarization or magnetization.

In the AFM, the probe is vibrated as it is scanned across a surface. As shown in Figure 2-13, the probe is vibrated in and out of surface potential. The modulated signal can then be processed with a phase or amplitude demodulator.

Probe motion
The cantilever oscillatory excitation is normally provided by a piezoelectric ceramic, similar to those used for X-Y positioning.

A typical vibrating system architecture is shown in Figure 2-14. The Z-axis position of the probe
Vibrating mode system architecture
is the sum of a fast oscillating drive component and a slowly-varying average position that is controlled by a feedback control system. The feedback system adjusts the Z position of the SUT in accordance with the error relative to a setpoint. The measurement which is compared to the setpoint is amplitude, frequency, or phase, depending on the particular mode of operation in use. Care is needed in the detailed design of the low pass filter and feedback control system, as there is a potential for instability. That instability, moreover, is sensitive to details of the probe-surface force relationship. A system that is stable for one value of setpoint can become unstable for a different value of the setpoint. (The mathematics of this design are beyond the scope of this paper.)
mass-spring oscillatorProbe-cantilever dynamics. Vibrating modes all make use of the natural mechanical resonance of the probe-cantilever system. For most purposes of AF microscopy, these dynamics can be adequately modelled by a simple damped massspring system (Figure 2-15). The mass and spring identify readily with the actual mass and stiffness, tho the physical source of the damping is not entirely obvious. Such a system displays the familiar Lorentzian resonance (Figure 2-16). The amplitude response is






Lorentzian resonance
mass-spring oscillator response
It is noteworthy that the amplitude at resonance omega can be written

equation

where eqn2 is the quasi-static amplitude response, that is, the amplitude that would result if the force acted only against the spring. The amplitude on-resonance is thus enhanced by a factor of eqn3. This is, of course, the low frequency limit of (2-4). Also noteworthy is the exact 90° phase at resonance, that is, the displacement response lags the driving force by 90°.

Probe interaction with surface
. When the probe tip interacts with a surface, the resonance frequency generally shifts to a lower value, and there is a corresponding change in the phase. When scanning in the vibrating modes, a constant relationship is maintained by the feedback electronics, which keeps either the phase shift or amplitude constant at a given frequency, while scanning.

As discussed above, there is a contamination layer on surfaces in ambient air with a thickness between 1 and 50 nanometers. Capillary forces, which are attractive, strongly affect probe behavior near the contamination layer.

The probe may be used in three fashions as it is scanned across the surface (see Figure 2-17).
probe near a contamination
Regime 1 - The probe is vibrated across the surface of the contamination layer. The vibration amplitude must be very small and a very stiff probe must be used. Typically, the images of the surface contamination layer are very "cloudy" and appear to have low resolution. This is because the contamination fills in the nanostructures at the surface.

Regime 2 - "Near Contact Mode" - The probe is scanned inside the contamination layer. Very high resolution images can be produced by this technique, but great care is required. The cantilever must be stiff so that capillary forces do not snap the probe to the surface, and the amplitude must be very small.

Regime 3 - "Intermittent contact" or "tapping" mode - The probe is vibrated in and out of the contamination layer. The energy in the vibrating cantilever is much greater than the depth of the capillary attraction potential well. The probe thus moves easily in and out of the contamination layer. This mode is conceptually simple, and is the easiest to implement, but it often results in broken probes due to the surface crashes that occur on every cycle.

A side benefit of vibrating modes is that "stickiness" due to friction ("lateral") forces, if any, tends to be released on each cycle as the probe moves away from the surface.

Typically, vibrating methods are used when the highest resolution is required or if very soft samples are being scanned. The probes used for vibrating mode are often less than 10 nm in diameter.

Small amplitude VM topography. While both QS topography and VM topography use force feedback, VM can operate at a much smaller force than QS, and operates in a fundamentally different way.
force-displacementThough the interaction force vs. displacement relationship is fundamentally nonlinear, for sufficiently small displacements it can be considered approximately linear, as shown in Figure 2-18. Moreover, an approximate straight line force relationship, tangent to the actual force curve, is equivalent to a linear spring, whose stiffness

Δk = -ΔFA That equivalent spring adds to or subtracts from the basic cantilever elasticity, altering keff.and thus its resonant frequency. The shift is up in a repulsive regime (larger keff ), or down in an attractive regime (smaller keff ). Although the magnitude of the change can be quite small, it is readily detected due to the generally high Q of the resonance. Viscous losses in the SUT may also affect the parameters of the resonance, though the specific relationship is less obvious, and generally is quite small compared to the elastic force contribution.

Any of several techniques can be used to detect the resulting change in the resonant frequency, changes in amplitude and phase being most common.

When scanning in vibrating modes, a constant relationship is maintained by the feedback electronics, which keeps either the phase shift or amplitude constant at a given frequency, while scanning.

Typically, small amplitude vibrating methods are used when the highest resolution is required or if very soft samples are being scanned. Some examples are shown in.Figure 2-19

Representative vibrating mode images
2 x 2 tip-checkerThe probes used for vibrating mode are often less than 10 nm in diameter. As vibrating mode imperils the probe more than simple contact modes, it is prudent to periodically check its integrity with a resolution reference sample that contains fine-scale features, such as that shown in Figure 2-20.

Large amplitude VM topography. Large amplitude VM, often called "tapping", is conceptually simpler than small amplitude VM, and easier to implement. It has the advantage of being less affected by the surface contamination layer. The probe is detached from the surface meniscus on every cycle. As the effects of the surface on the probe motion is more dramatic than in small amplitude VM, it is more easily extracted from the deflection signal. It has disadvantages, however:


The system architecture for large amplitude VM is essentially the same as small amplitude VM. As before, care is needed in design of the feedback control amplifier that positions the SUT in the Z coordinate, as there is a hazard of instability. The design is complicated by the fact that the value of the coordinate setpoint can change the small-signal gain, thus altering the stability properties.

Force Gradient Modes

Nanoscopic-scale electrostatic and magnetostatic material properties are particularly accessible to AFM measurement. Any interaction force for which a suitable probe exists can be mapped. The mechanism of the mapping is the spatial gradient of the force. That spatial gradient adds or subtracts from the effective spring constant of the AFM cantilever, as discussed above. The resulting changes in resonant frequency are readily measured. The fields are sensed through the changes in probe-cantilever resonance as the probe is moved slowly above the SUT.

Principles. For very small displacements of the probe, the z-axis gradient of the force modifies the effective spring constant of the cantilever as discussed above. Assuming that the field, and thus the force, varies only with Z, then the resonance of the probe-cantilever system is approximately:

probe-cantilever system
and we have implicitly assumed that the force can be adequately modeled by the first term of its Taylor series expansion in ΔZ.
Taylor series

(The negative sign arises because F = -kZ for a simple mass-spring oscillator.)

The shift in resonant frequency is sensitive to the first spatial derivative of the spring constant, and thus to the second spatial derivative of the force, that is:

second spatial derivative of the Force

Measurements of the resonant frequency at two elevations thus yields an approximation to the second derivative of the surface field strength.

Force gradient instrumentation techniques. Several schemes are used for such measurements:



Separating topography

Application to permanently polarized materials. The force gradient technique is often applied to permanently polarized materials (called electrets when electric, or magnets when magnetic). It requires a probe that is either conductive or ferromagnetic. The coatings lead to several problems:


Application to more general forces. The nature of the forces sensed by the force gradient technique can be quite general. The only constraint is that the force be a function of height above surface. For example, a constant voltage bias between probe and surface produces a vertical force due to the distance-dependent capacitance between probe and surface (see §3.4, for example).