AFM Probes and AFM Cantilevers
An AFM cantilever with an AFM tip on its end is the main sensing component ultimately responsible for the quality of AFM imaging. The most common and at the same time very sensible scheme of data acquisition is an optical one based on registration of a laser beam reflected from the backside of the AFM cantilever with a sectioned (position sensitive) photodiode. For better reflection the backside of AFM cantilevers is often covered with aluminium or gold. There are a number of other deflection registration techniques and related peculiarities of AFM cantilever construction among which piezo cantilevers are worth of particular consideration [160, 161, 210, 211, 390, 921, 922, 1382]. However, this report is limited to the description of AFM cantilevers for the optical registration scheme.
AFM cantilever parameters
- Material of the AFM cantilever
The most popular materials are monocrystalline silicon and Si3N4. Silicon nitride AFM cantilevers offer an advantage over silicon ones in the sense that they may be produced thinner and, hence, more flexible (having lower stiffness). However, Si3N4 does not possess perfect manufacturability for AFM tips machining, therefore Si3N4 AFM tips are usually inferior to those made of silicon. The merits of both materials have been coupled together in hybrid AFM probe construction, which features the flexibility of a silicon nitride AFM cantilever and the sharpness of a silicon AFM tip [1442].
AFM cantilevers made of tungsten, nickel and another materials are in occasionally used [157, 581, 602, 870, 921, 922, 943, 1022, 1065, 1328]. The material through its inherent mechanical properties (elasticity module or Young's module E, module of rigidity G) and density defines the stiffness, resonance frequency and Q-factor (see below) of the AFM cantilever. In addition, the material properties of the coating should also be taken into consideration if it covers over the entire AFM cantilever surface.
Using AFM cantilevers made of low resistance materials such as metals or highly doped silicon ensures that no electrostatic charges collect at the AFM tip apex. Gathering electrostatic charges results in distortion of the images and is especially crucial in Scanning Tunneling and Electrical Force Microscopy studies.
- Geometry of the AFM cantilever
A number of AFM cantilever geometries have been proposed since the invention of AFM and even earlier when Scanning Tunneling Microscopy was the only SPM technique of comparable principle of operation. The most preferable among researchers are the rectangular (diving board) and the triangular lever shapes. Triangular AFM cantilevers are often used in such contact mode experiments where twisting a tip along the only symmetry axis of the lever is undesirable. The range of geometries of the AFM cantilevers manufactured by MikroMasch is wide:
AFM Cantilever Property |
Range for MikroMasch AFM cantilevers |
Range of AFM cantilevers from reviewed publications |
Length (l) | 90µm - 450µm | > 10µm |
Width (w) | 13.5µm - 50µm | > 3µm |
Thickness (s) | 500nm - 7µm | > 0.1µm |
Force constant (k) | 0.03N/m - 45N/m | 0.001N/m - 400N/m |
Resonance frequency (fo) | 10kHz - 450kHz | 3kHz ~ 10Mhz |
- Stiffness of the AFM cantilever
Stiffness is defined by the force constant k measured in N/m (or sometimes nN/nm). The commonly used AFM cantilevers have force constants in the range 0.01-100N/m. The "soft" AFM cantilevers with k<0.1N/m are chosen mainly when using contact mode in order to affect the sample to minimal extent. The rigid ones with k>1N/m are often used in non-contact or dynamic modes since they exhibit high resonance frequencies and small oscillation amplitudes of about several tens Angström. This ensured wide dynamic frequency range and substantially raises sensitivity.
Fig. 1.1 Schematic of vertical deflection | Fig. 1.2 Schematic of lateral deflection |
By default the term "force constant" refers to the force constant with respect to vertical deflection of the AFM cantilever (Fig.1.1). The theoretical expression for estimation of this force constant in the case of the simplest rectangular AFM cantilever is given by following formula:
In a number of SPM techniques especially in Lateral Force Microscopy (LFM) the tip is moved in touch with the surface of the sample and twisting of the AFM cantilever apart from vertical deflection also takes place as depicted in Fig 1.2. The stiffness of the AFM cantilever from such kind of applied external force is determined by the lateral force constant, which can differ from that of "normal" k to a great extent. The formula for klat has the same structure except for an additional parameter h defining AFM tip height:
By additional processing of commercial AFM cantilevers Kageshima et al. [1437] enhance the lateral force sensitivity of Atomic Force Microscopy for detection of molecular scale interactions. Sensors of two types are fabricated by this group. As a result, the lateral force constants are reduced about 10-fold and 180-fold for both types respectivelly which allows for improvement of lateral force resolution up to 1nN.
The expressions for determination of the force constants of triangular levers are more complicated [1308]. See also a useful paper of Newmeister and Ducker [1218].
It is commonly adopted that triangular AFM cantilevers withstand much better lateral forces in comparison to rectangular ones of identical normal stiffness. Rigorous calculations performed by Sader [2622] show that the reality is quite the contrary. This unexpected theoretical result is to be verified experimentally.
It is a nontrivial task however to measure exactly the force constant of a particular AFM cantilever mainly due to the fact that geometrical parameters of every AFM cantilever cannot be exactly controlled and determined individually in mass production. Therefore, the theoretically calculated stiffness may substantially differ from the actual one. This concerns particularly the thickness control during the etching process of AFM cantilever micromachining. A simple calculation shows that the variation of thickness in ± 20 % results in variation of k value in the range of about -50%~+70%. To cope with this unsertainty a number of empiric and semiempiric techniques of force constant measuring and calibration are developed [E008, 859, 1300, 1205, 1206, 1621, 2626].
Determining the mechanical properties of materials at the micro and nanoscale needed for microprocessor design and development of micro-elecrtomechanical systems (MEMS) is a challenge due to the inadequate testing equipment since it must be capable of applying loads in the order of 10-6 to 10-9 Newtons. AFM with well-calibrated silicon AFM cantilevers is quite promising technique for such measurements. Comella and Scanlon [756] report on the development of AFM cantilever based technique for mesuring the elasticity of thin films. In their simple and reliable approach microcantilevers of the investigated material are formed by an ordinary lithographical method, then a silicon AFM cantilever with a well-calibrated force response is used to measure microbeams deflection under defined loadings. The authors claim that the method developed is applicable to beams of thickness ranging from Angströms to microns. Vice versa, using calibrated loading (for example, with an indenter) the unknown force constant of the AFM cantilever can be measured [E011].
Visit also the Materials Research section and subsections within for numerous examples of materials characterization.
- Resonance frequency of the AFM cantilever
Resonance frequency fo varies from several kHz up to several Mhz [163] and analytically is expressed as:
where m and mtip are masses of an AFM cantilever and an AFM tip respectively. In the simplest case of a rectangular AFM cantilever neglecting the AFM tip mass it is derived that:
It can be easily seen that the decisive factor to increase the resonance frequency is to shorten the length of an AFM cantilever. At the same time the AFM cantilever can be produced relatively "soft" by means of width or thickness adjustments compensating the increase of the force constant due to appearance of l in the denominator of the expression for k. The AFM cantilevers with high resonance frequencies fo and low k are the better choice for tapping mode investigations since the AFM tip taps the surface gently while at the same time oscillates at several hundred kilohertz [519, 1578].
The eigenfrequency of the AFM cantilever can vary significantly if the latter is coated with a rather thick coating like, for instance, DLC. Salvadori at al [85] investigate the dependence of fo from the thickness of DLC coating deposited on the AFM cantilevers of 3.5 - 5 µm thicknesses using a specially derived formula for a thin and uniform coating with thickness s. This dependence is found to be almost linear. A 0.3 µm coating raises the eigenfrequency of the AFM cantilever by 50%. However, deposition of thick DLC films results in severe bending of the AFM cantilever as shown in photographs presented by Lemoine at al [82]. This bending originates from the intrinsic stress in DLC films. It can be released substantially by incorporating silicon atoms (~ 15 %) in a-C:H film. The authors note that stress-induced AFM cantilever deflections are too large for direct use of the AFM cantilevers in an AFM microscope. The bending gives rise to works on stress measurements in thin films grown on silicon cantilever beams ([1649]).
Fritz et al. [1211] report on the successful deposition of a thin copper film onto conductive silicon AFM cantilevers by MikroMasch produced by means of a galvanic displacement technique. This procedure does not lead to bending of the lever and keeps the resonance frequency almost unchanged. To demonstrate the effectiveness of this approach for tribological studies, the coated AFM cantilevers are chemically functionalized with alkanethiol monolayers. The effect of the changed surface energy is detected with adhesion measurements in water and ethanol.
- Q-factor
The Q-factor shows what part of the entire vibration energy that system loses during a full cycle of oscillation. In other words, it defines the minimal external vibration force within a given range of frequencies needed to maintain the oscillation of the system. Ideally, no external force is needed since it contributes to the overall noise thus reducing sensitivity. In highly damping ambients such as liquids substantial external forces are needed and therefore the Q-factor is smaller by 2 - 3 orders of magnitude than that in ultrahigh vacuum. In mechanical systems it is approximated as:
where b is the damping factor. Thus the Q-factor depends on the mechanical characteristics of the AFM cantilever and the damping properties of the ambient. The higher the Q-factor, the higher the sensitivity. See a publication on this topic by Yasumura et al. [1210].
AFM tip parameters
-
Material of the AFM tip
The choice of material depends on the purposes the AFM probe is intended for. When the highest possible hardness is necessary, for example in nanoscratching experiments or Scanning Spreading Resistance Microscopy (SSRM), a diamond AFM tip is glued to the AFM cantilever [602, 1606, 1609]. Another approach is to use a conventional silicon AFM tip with a diamond-like coating (DLC) [1336].
Resistance of the AFM tip and the entire AFM cantilever against aggressive ambients especially in the case of fluids is of primary importance as well. This problem is often solved using protective coatings such as Cr-Au or Pt.
The protective coatings at the same time can serve as conductive coatings. TiN, W2C, TiO, doped DLC and many others are occasionally used. AFM cantilevers with such tips are suitable for Scanning Tunneling Microscopy (STM), Electric Force Microscopy (EFM) and other conductance sensitive techniques. In principle, the silicon AFM tip itself can be used for such purposes if made of highly doped silicon. However, it is easily damaged in contact mode techniques such as the above mentioned SSRM where very high contact forces of 10-5 N are applied to the specimen [157].
Another class of coatings includes magnetic ones such as Co, Ni, Fe and a number of special alloys for use in Magnetic Force Microscopy (MFM) and Scanning Tunneling Microscopy investigations [642, 873, 1111, 1117, 1122, 1123, 1126, 1176, 1441]. The magnetic AFM probes by MikroMasch are listed here.
Since the mid 1990's a novel approach for functionalization of the AFM tip apex with other molecules in order to build specific AFM probes and sensors is developing intensively. Until now different micro-, macromolecules and functionalization addenda have been proposed and investigated as candidates for supertips: carbon nanotubes [30, 78, 818, 1325, 1380, 1381, 1456, 1464, 1610], W2C nanotubes [1445], proteins [974], adamantane [270], caltrop shaped molecules based on a differentially substituted tetrahedral silicon atom [E009] and many others [451, 1211, 1622]. Besides inherent extrasharpness the functionalized AFM tips possess selectivity with respect to the features on the sample surface having different chemical nature and are ideally suited to mapping their distribution and performing single-molecule force spectroscopy studies. Of course, to measure such tiny forces down to 10-12 N and gradients of 10-5 N/m very sensitive and intelligent registration and feedback systems are necessary.
Functionalization of the AFM tip apex with various agents allows for preferential imaging of different atoms at the sample surface. Ke et al. [13] investigate theoretically the effect of tip morphology on the image contrast for a GaAs(110) surface for the three atomically different AFM tip apexes of a Si tip: (1) Si apex with a half-filled dangling bond; (2) Ga apex with an empty dangling bond; and (3) As apex with a fully filled dangling bond. The study reveals a great impact of the dangling-bond states of different atoms at the tip apex on the image contrast. Calculation reveals that the Ga apex images the As sublattice, and the As apex images the Ga sublattice, and in the case of the Si apex, it is possible to image only the As sublattice or both the As and Ga sublattices, depending on the tip-sample separation.
- Geometrical parameters of the AFM tip
These are the height, profile, opening angle at the tip apex and apex curvature radius.
The overwhelming majority of former commercial AFM tips have triangular or square pyramid shape with an opening angle up to 70° (Fig. 2, a). They are produced by lithography and do not actually exhibit sufficient sharpness.
Using the (electro)chemical etching technique sharper AFM tips can be produced from monocrystalline silicon. The bulk shape of this AFM tip is still pyramidal and not so sharp (< 40°, Fig. 2, b) but the very end of the tip tends to become increasingly thinner approaching the apex. The opening angle near the apex is about 20°. Nevertheless, the pyramidal profile of the AFM tip does not still allow imaging of high aspect ratio structures.
If high aspect ratio samples with steep and deep walls are to be investigated, long and thin AFM tips resembling a bee sting (Fig. 2, c) are used. Such AFM tips are grown on the apexes of the conventional AFM tips using Electron Beam Deposition (EBD). Other techniques such as Focused Ion Beam (FIB) machining [2594] or oriented growth of whisker-like silicon needles [1281] are also developed. The latest advances in technology of carbon nanotubes allow attachment or direct growth of carbon nanotubes as an extratip at the AFM tip apex of commercial AFM cantilevers (Fig. 2, e).
The resolution of Scanning Probe Microscopy depends substantially on the sharpness of the imaging AFM tip. Curvature radius of conventional AFM tips is about 8 - 15 nm. Very high resolution is achievable with Hi'Res-C AFM tips specially developed by MikroMasch (Fig. 2, d). Curvature radii of these AFM tips are in the order of 1 nm and with their help fine molecular or even atomic structure can be resolved.
In some studies very specific AFM probe tips are required, for example AFM tips with a flat apex (Fig. 2, f). Such AFM tips are used in tribological, indentation and other studies.
a | b | c |
d | e | f |
Fig. 2 AFM tip variety. (a) AFM probe with pyramidal AFM tip. (b) AFM probe with conventional silicon AFM tip. (c) AFM probe with EBD grown AFM tip. (d) SEM image of an old Hi'Res-C AFM tip. (e) AFM probe with Carbon Nanotube AFM tip. Image taken from [1612] with permission of Dr. R. Schlaf. (f) AFM probe with flat AFM tip apex. |
Sometimes there is no apparent dependence between AFM tip characteristics and imaging parameters. For example, Sedin and Rowlen [21] observe two different trends for measured surface roughness as a function of AFM tip size. Root mean squared (RMS) roughness is one of the most commonly reported measures of surface roughness from AFM images. It is found that at small lateral scan sizes (<500nm) the image root mean square roughness decreased as AFM tip size increased, but at larger scan sizes (e.g. 5000nm), the roughness increases with increasing AFM tip size. The authors also emphasize that there is a great variation of AFM tip shapes within a single lot of commercial AFM cantilevers. Frost et al. [27] show that AFM tip quality has a strong influence on the surface roughness parameters extracted from the AFM images particularly for surfaces with low surface roughness (~1nm) as generally obtained by means of thin film technologies. For evaluation of the influence of the actual AFM tip quality on the measured surface topography they propose nanometer-sized sputtered InP-structures whose sizes are well-controllable with a set of parameters of the sputtering process.
There are also attempts to estimate the effect of AFM tip apex size on the AFM image using various simulation approaches [132, 698]. The material of the next paragraph is devoted to AFM tip shape determination methods and related problems.
Ideally, the AFM tip apex should be round shaped and terminate with the single atom. Deviations from this ideal situation cause so-called AFM tip artifacts in the scanned images. A collection of AFM tip induced artifacts is gathered by Xu and Arnsdorf [1605]. 10 suggestions to minimize artifacts in SPM images are proposed in [1010]. Artifacts may also be caused either by the AFM system design and operation mode or by external environmental conditions, i.e. by factors not related to AFM tip imperfectness [1376]. Thorough description of commonly observed artifacts in SPM as well as procedures for AFM tip shape characterization are developed and published by The American Society for Testing and Materials (ASTM) [2800, 2801].
There are a number of AFM tip defects, which cause artifacts. The most common of them are:
1) Multiple peaks at the apex comprising atomic scale protrusions. Every peak during scanning contributes in the tip-sample interaction. In the simplest case of a double peak apex the features on the sample surface look double in the scans (Fig. 3, d). Absence of this defect is especially crucial when measuring single macromolecules.
2) Blunt apex. This results in lowering of resolution power. The sharpness of the apex tends to decrease during consecutive contact mode scans of the sample surface (Fig. 3, a,b,c).
3) Non-spherical apex. Results in geometry distortion of sample features.
(a) 700 x 700 x 20 nm | (b) 700 x 700 x 16 nm |
(c) 800 x 800 x 12 nm | (d) 400 x 400 x 16 nm |
Fig. 3. Imaging of sharp edges of CdF2 films grown in <111> orientation. a, b, c) Decreasing of AFM tip sharpness in the set. d) Double tip artifact. Image courtesy of Prof. Sergey Gastev, St. Petersburg |
As a matter of fact, the yield of AFM cantilevers with "good" AFM tips is occasionally not very close to 100% due to defects of one type or another including the most common mentioned above. Thus, development of a simple AFM tip shape characterization technique is quite desirable. Moreover, scanning probe techniques are utilized as the means of choice for critical dimension metrology (CDM) applications [837, 1608, 1612] increasingly in recent years, and the AFM tip shape geometry becomes a crucial factor of success.
Problem of tip-sample convolution. Methods of AFM tip characterization.
Achieving the best possible resolution will always remain the outmost goal for many SPM studies. There are, though, some technical challenges to be overcome as well as fundamental limitations on the way to high resolution.
One of the technical issues that has to be considered is the imperfect geometry and finite size of the AFM tip. The best approximation to the ideal AFM tip geometry (omitting various natural disturbing factors like thermal noise) is believed to be a carbon nanotube of several nanometers in diameter, several micrometers long and with a single atom at the sharp conical apex. Most of the commercial AFM probes are too far from this ideal case. In general, a conventional AFM tip is unable to penetrate high aspect ratio structures, to touch every point on the sample surface and to profile exactly surfaces with complex topography. In this way, the finite size of the AFM tip and its imperfectness contribute significantly to distortion of images.
There are also some physical restrictions in achieving subnanometer resolution besides technical issues. Due to the long-range nature of van der Waals forces acting between AFM tip and sample, resulting force is determined by the mean interaction of a large number of atoms from both the AFM tip and the sample surface especially when the features are comparable in size with AFM tip apex. Therefore, the features of the sample surface become diluted by this interaction of collective nature.
Thus, actually the image is a complex convolution of the AFM tip and the surface shapes. This convolution is unavoidable but there are ways to reconstruct a rather accurate image from the diluted one using special mathematical methods.
The earliest attempts to formulate the task mathematically date from papers of Reiss et al. [1633] and Keller [1634]. Their works have become the basis for several similar methods of deconvolution where some simple particular geometries, e.g. spheres or parabolas are considered. These methods require intensive computation and evaluation of numerical derivatives and, therefore are comlicated enough for practical implementation.
Another approach to solve the problem of deconvolution relies on mathematical morphology. This approach has been proposed and developed by many authors [1637] beginning from works of Gallarda and Jain [1635] and Pingali and Jain [1636]. It is applicable to general shapes (any AFM tip and sample which can be expressed as an array of heights in the usual fashion), and does not require numerical derivatives.
These methods have one point in common - it is necessary beforehand to estimate the AFM tip geometry in order to perform proper deconvolution procedure thereafter. One of the most popular methods for AFM tip shape and size determination is based on the so-called AFM tip characterizers, which are the features of well-defined geometry at the nanoscale. Characterizers may be highly ordered edges of crystal facets (SrTiO3 [1603], MgO and NaCl [1604]), nanoparticles of well-defined spherical form [1605, 1607], sputtered cones [51] or nanoparticles [27] of InP, spike-like features in hydrothermally deposited ZnO films [268], macromolecules [788, 1455] and many others [E010]. Additionally, specially designed calibration standards can also serve as AFM tip characterizers. A computer analysis of the obtained scans can help restore the AFM tip shape and at the same time deduce what kind of defect the AFM tip contains.
An alternative widely used approach for AFM tip shape determination has come to be known as "blind reconstruction". The term "blind" means that there is no need of a priory knowledge of the exact characterizer's actual geometry. Since the publication of the principles of general blind reconstruction by Villarrubia [1639] equivalent or similar methods independently are discovered later [1643, 1644]. The algorithms of blind reconstruction are published in [1645] and a speedier version is described and tested in [1646]. It is experimentally verified to work in a comparison between blind reconstruction of an AFM tip and an independent method [1647]. In other work Todd and Eppell report on the improvement of this method in respect to spatially anisotropic noise which generally takes place at the nanoscale and introduces an error in the AFM tip geometry determination [801]. The latest advances in evaluation of AFM tip performance in the blind reconstruction method can be found in the papers of Nie et al. [1654, 1656].
Another modern technique developed by S. Xu et al. [23] is called nanografting. It is based on subsequent imaging of a thiol self-assembled monolayer. The authors state that this method features simplicity, high speed and the ability to characterize the very top portion of the AFM tip. Moreover, AFM tips with multiple asperities, which are difficult to investigate using other approaches, can be easily identified and characterized via nanografting.
We would like to express special thanks to John Villarrubia from the National Institute of Standards and Technology (Gaithersburg, MD, USA) for the constructive discussion on the content of this paragraph.
Please, send all comments and suggestions concerning these pages to info@mikromasch.com.
ID | Reference list |
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