Atomic force microscope
Atomic force microscopy (AFM) or scanning force microscopy (SFM) is a very high-resolution type of scanning probe microscopy, with demonstrated resolution on the order of fractions of a nanometer, more than 1000 times better than the optical diffraction limit. The precursor to the AFM, the scanning tunneling microscope, was developed by Gerd Binnig and Heinrich Rohrer in the early 1980s at IBM Research - Zurich, a development that earned them the Nobel Prize for Physics in 1986. Binnig invented the atomic force microscope and the first experimental implementation was made by Binnig, Quate and Gerber in 1986. The first commercially available atomic force microscope was introduced in 1989. The AFM is one of the foremost tools for imaging, measuring, and manipulating matter at the nanoscale. The information is gathered by "feeling" the surface with a mechanical probe. Piezoelectric elements that facilitate tiny but accurate and precise movements on (electronic) command enable the very precise scanning. In some variations, electric potentials can also be scanned using conducting cantilevers. In more advanced versions, currentscan be passed through the tip to probe the electrical conductivity or transport of the underlying surface, but this is much more challenging with few research groups reporting consistent data (as of 2004)
Contents
Basic principles
The AFM consists of a cantilever with a sharp tip (probe) at its end that is used to scan the specimen surface. The cantilever is typically silicon or silicon nitridewith 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. Depending on the situation, forces that are measured in AFM include mechanical contact force, van der Waals forces, capillary forces, chemical bonding, electrostatic forces, magnetic forces (see magnetic force microscope, MFM), Casimir forces, solvation forces, etc. Along with force, additional quantities may simultaneously be measured through the use of specialized types of probes (see scanning thermal microscopy, scanning joule expansion microscopy, photothermal microspectroscopy, etc.). Typically, the deflection is measured using a laser spot reflected from the top surface of the cantilever into an array of photodiodes. Other methods that are used include optical interferometry, capacitive sensing or piezoresistive AFM cantilevers. These cantilevers are fabricated with piezoresistive elements that act as a strain gauge. Using a Wheatstone bridge, strain in the AFM cantilever due to deflection can be measured, but this method is not as sensitive as laser deflection or interferometry
Atomic force microscope topographical scan of a glass surface. The micro and nano-scale features of the glass can be observed, portraying the roughness of the material. The image space is (x,y,z) = (20 µm × 20 µm × 420 nm). If the tip was scanned at a constant height, a risk would exist that the tip collides with the surface, causing damage. Hence, in most cases a feedbackmechanism is employed to adjust the tip-to-sample distance to maintain a constant force between the tip and the sample. Traditionally the tip or sample is mounted on a 'tripod' of three piezo crystals, with each responsible for scanning in the x,y and z directions. In 1986, the same year as the AFM was invented, a new piezoelectric scanner, the tube scanner, was developed for use in STM.[6] Later tube scanners were incorporated into AFMs. The tube scanner can move the sample in the x, y, and z directions using a single tube piezo with a single interior contact and four external contacts. An advantage of the tube scanner is better vibrational isolation, resulting from the higher resonant frequency of the single-crystal construction in combination with a low resonant frequency isolation stage. A disadvantage is that the x-y motion can cause unwanted z motion resulting in distortion. 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 (non-contact or "tapping") modes where the cantilever is vibrated.
Probe
An AFM probe has a sharp tip on the free-swinging end of a cantilever that is protruding from a holder plate. The dimensions of the cantilever are in the scale of micrometers. The radius of the tip is usually on the scale of a few nanometers to a few tens of nanometers. (Specialized probes exist with much larger end radii, for example probes for indentation of soft materials.) The holder plate, also called holder chip, - often 1.6 mm by 3.4 mm in size - allows the operator to hold the AFM probe with tweezers and fit it into the corresponding holder clips on the scanning head of the Atomic force microscope. This device is most commonly called an "AFM probe", but other names include "AFM tip" and "cantilever" (employing the name of a single part as the name of the whole device). An AFM probe is a particular type of SPM (Scanning probe microscopy) probe. AFM probes are manufactured with MEMS technology. Most AFM probes used are made from silicon (Si), but borosilicate glass and silicon nitride are also in use. AFM probes are considered consummables as they are often replaced when the tip apex becomes dull or contaminated or when the cantilever is broken. Just the tip is brought very close to the surface of the object under investigation, the cantilever is deflected by the interaction between the tip and the surface, which is what the AFM is designed to measure. A spatial map of the interaction can be made by measuring the deflection at many points of a 2D surface. Several types of interaction can be detected. Depending on the interaction under investigation, the surface of the tip of the AFM probe needs to be modified with a coating. Among the coatings used are gold - for covalent bonding of biological molecules and the detection of their interaction with a surface, diamond for increased wear resistance and magnetic coatings for detecting the magnetic properties of the investigated surface. The surface of the cantilevers can also be modified. These coatings are mostly applied in order to increase the reflectance of the cantilever and to improve the deflection signal.
Imaging modes
AFM operation is usually described as one of three modes, according to the nature of the tip motion:
- contact mode, also called static mode (as opposed to the other two modes, which are called dynamic modes)
- tapping mode, also called intermittent contact, ACmode, or vibrating mode, or, after the detection mechanism, Amplitude Modulation AFM
- non-contact mode, or, again after the detection mechanism, Frequency Modulation AFM
Contact mode
In contact mode, the tip is "dragged" across the surface of the sample and the contours of the surface are measured either using the deflection of the cantilever directly or, more commonly, using the feedback signal required to keep the cantilever at a constant position. Because the measurement of a static signal is prone to noise and drift, low stiffness cantilevers are used to boost the deflection signal. Close to the surface of the sample, attractive forces can be quite strong, causing the tip to "snap-in" to the surface. Thus, contact mode AFM is almost always done at a depth where the overall force is repulsive, that is, in firm "contact" with the solid surface below any adsorbed layers.
Tapping mode
In ambient conditions, most samples develop a liquid meniscus layer. Because of this, keeping the probe tip close enough to the sample for short-range forces to become detectable while preventing the tip from sticking to the surface presents a major problem for non-contact dynamic mode in ambient conditions. Dynamic contact mode (also called intermittent contact, AC mode or tapping mode) was developed to bypass this problem. In tapping mode, the cantilever is driven to oscillate up and down at near its resonance frequency by a small piezoelectric element mounted in the AFM tip holder similar to non-contact mode. However, the amplitude of this oscillation is greater than 10 nm, typically 100 to 200 nm. The interaction of forces acting on the cantilever when the tip comes close to the surface, Van der Waals forces, dipole-dipole interactions, electrostatic forces, etc. cause the amplitude of this oscillation to decrease as the tip gets closer to the sample. An electronic servo uses the piezoelectric actuator to control the height of the cantilever above the sample. The servo adjusts the height to maintain a set cantilever oscillation amplitude as the cantilever is scanned over the sample. A tapping AFM image is therefore produced by imaging the force of the intermittent contacts of the tip with the sample surface. This method of "tapping" lessens the damage done to the surface and the tip compared to the amount done in contact mode. Tapping mode is gentle enough even for the visualization of supported lipid bilayers or adsorbed single polymer molecules (for instance, 0.4 nm thick chains of synthetic polyelectrolytes) under liquid medium. With proper scanning parameters, the conformation of single molecules can remain unchanged for hours.
Non-contact mode
In non-contact atomic force microscopy mode, the tip of the cantilever does not contact the sample surface. The cantilever is instead oscillated at either its resonant frequency (frequency modulation) or just above (amplitude modulation) where the amplitude of oscillation is typically a few nanometers (<10 nm) down to a few picometers. The van der Waals forces, which are strongest from 1 nm to 10 nm above the surface, or any other long-range force that extends above the surface acts to decrease the resonance frequency of the cantilever. This decrease in resonant frequency combined with the feedback loop system maintains a constant oscillation amplitude or frequency by adjusting the average tip-to-sample distance. Measuring the tip-to-sample distance at each (x,y) data point allows the scanning software to construct a topographic image of the sample surface. Non-contact mode AFM does not suffer from tip or sample degradation effects that are sometimes observed after taking numerous scans with contact AFM. This makes non-contact AFM preferable to contact AFM for measuring soft samples, e.g. biological samples and organic thin film. In the case of rigid samples, contact and non-contact images may look the same. However, if a few monolayers of adsorbed fluid are lying on the surface of a rigid sample, the images may look quite different. An AFM operating in contact mode will penetrate the liquid layer to image the underlying surface, whereas in non-contact mode an AFM will oscillate above the adsorbed fluid layer to image both the liquid and surface. Schemes for dynamic mode operation include frequency modulation where a phase-locked loop is used to track the cantilever's resonance frequency and the more common amplitude modulation with a servo loop in place to keep the cantilever excitation to a defined amplitude. In frequency modulation, changes in the oscillation frequency provide information about tip-sample interactions. Frequency can be measured with very high sensitivity and thus the frequency modulation mode allows for the use of very stiff cantilevers. Stiff cantilevers provide stability very close to the surface and, as a result, this technique was the first AFM technique to provide true atomic resolution in ultra-high vacuum conditions. In amplitude modulation, changes in the oscillation amplitude or phase provide the feedback signal for imaging. In amplitude modulation, changes in the phase of oscillation can be used to discriminate between different types of materials on the surface. Amplitude modulation can be operated either in the non-contact or in the intermittent contact regime. In dynamic contact mode, the cantilever is oscillated such that the separation distance between the cantilever tip and the sample surface is modulated. Amplitude modulation has also been used in the non-contact regime to image with atomic resolution by using very stiff cantilevers and small amplitudes in an ultra-high vacuum environment.
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