Atomic Force Microscope Related terms:
iction, Scanning
Tunneling Microscope,
Deflection, Scanning
Electron Microscope,
Nanoscale,
Characterisation, Electron
Microscope, Microscope
Image
AFM uses the van der Waals molecular forces or contact forces between a tip
and the sample to measure the sample topography or mechanical properties.
From: Fundamentals and Applications of Nano Silicon in Plasmonics and
Fullerines, 2018
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Characterization of electrospun nanofibers
Ramazan Asmatulu, Waseem S. Khan, in Synthesis and Applications of Electrospun Nanofibers, 2019
13.2 AFM Characterization
‘AFM is a high-resolution scanning probe microscope with a resolution of fractions of Angstrom, which has more
than 1000 times higher resolution when compared to the classical optical microscope. AFM contains a micro- and
nanoscale cantilever with a silicon or silicon nitrite sharp tip (probe) at its end that is used to scan the specimen
surface at the nanoscale level. CNTs can be attached to the tip of the cantilever to make a sharper tip to increase
the image resolution of the surfaces at the angstrom level. However, the CNT-based AFM tip is highly fragile, and
the operator must be extra careful during the mounting and surface scanning, Depending on the requirements,
applied forces between the tip and surface can be measured for the detection of mechanical contact force,
magnetic, van der Waals interaction, electrostatic, capillary, chemical, and steric forces (17]. Usually, three different
AFM modes can be employed in an AFM unit, including contact mode, noncontact mode, and tapping mode. Fig.
138 shows the different modes of AFM, including contact mode, noncontact mode, and tapping mode [25].
The contact mode in which the tip of the cantilever scans the sample in close contact with the surface is the most
‘commonly used method for surface force measurements. In the noncontact mode, the tip usually hovers about
5-15 nm above the surface of the substrate. There are some difficulties with the contact mode AFM because of the
higher wear rate and failure ofthe tips during scanning. On the other hand, tapping mode AFM deals with the
problems associated with friction, tip tackling with the rough surfaces, electrostatic forces, adhesion, and other
difficulties by the tapping process. Fig. 13.9 shows photographs and an AFM image of electrospun Estane
nanofibers incorporated with 26 wt.9% MnZnFe/Ni magnetic nanoparticles obtained at 18 kV voltage, 3 mL. h-!
pump speed, and 15 cm separation distance (13,17].Silicon nanoneedles for drug delivery
. Chiappini, C. Almeida, in Semiconducting Silicon Nanowires for Biomedical Applications, 2014
8.6.1 Atomic force microscope (AFM)-operated nanoneedles
[AFM actuation isthe first strategy implemented for the use of silicon nanoneedies for drug delivery (Fig. 8.2). The
force measurements with an AFM instrument can be used to study cellular events in individual cells with great
sensitivity (Lamontagne et al, 2008). Among the applications is the injection at the nanoscale of specific molecular
entities in individual living cells. Solid silicon nanoneedles optimised for harmless cell penetration (Obataya et al.
2005b) are developed with 6 um length and 200 nm width by FIB from Si AFM tips (Han et al, 20052). Subsequent
treatment of the surface of the newly formed nanoneedles with 3-mercaptopropyitrimethoxysilane (MPTS)
followed by incubation with N-{6-maleimidocaproylony)succinimide (EMCS) provides the means for further
functionalisation. DNA is bound to the needle by first soaking the succinimidyl nanoneedle in an avidin solution
and then incubating with a solution of biotinylated green fluorescent protein (GFP) DNA fragment. Force
distance measurements indicate that the nanoneedles can penetrate human embryonic kidney cells with a
reproducible profile that outlines the different stages of the needle penetration. The penetration force profile does
depend on DNA immobilisation on the nanoneedle's surface, suggesting that the DNA molecules and cell
components do not interact. Furthermore, calculations of friction force applied to one molecule of DNA in the
penetration process indicate that the DNA does not detach from the surface of the nanoneedle during insertion.
The cells manipulated by AFM can proliferate after repeated penetrations with a DNA-functionalised nanoneedle
(Han et al, 20052).
The silicon AFM-based nanoneedle system can also mediate intracellular presentation proteins, allowing insertion
of two different His-tagged, fluorescently labelled proteins into HeLa cells. The nanoneedle surface is chemically
modified with nitrilotriceticacid (NTA) groups, and then chelated with NiCI, to conjugate poly-histidine-modified
proteins. The protein-nanoneedle hybrid inserted into HeLa cells shows constant fluarescence intensity at the
surface of the device while kept inside the cell, to indicate a stable conjugation of the protein to the needle
(Obataya et a, 2005a).
Although neitheir of these examples demonstrate drug delivery, they indicate an avenue to use silicon
nanoneedies for manipulation of ving cells and intracellular access, without inflicting critical cell damage. Indeed
an AFM nanoneedle can successfully transport electrostatically bound GFP plasmid DNA into cells. The
transfection efficiency of over 50% is sufficient to prove molecular delivery through AFM-operated nanoneedles
(Han et al, 20052). Similarly AFM nanoneedles mediate efficient (above 70%) transfection of GFP plasmid DNA
into the nucleus of mesenchymal stem cells, known hard-to-transfect cells using microinjection because of their
flat shape (Han et al, 2008). When the plasmid DNA is only non-specfically bound to the surface of the
nanoneedle, the system releases its load inside the target cell but also in the surrounding media. Ifthe cell
penetration is not rapid enough, the delivery fails.
Using 2 nanoneedle actuated by AFM surmounts the limitation of whole-cell population studies of typical cell
biology methods by being able to manipulate single cells (Lamontagne et al, 2008) with minimal invasiveness.
Moreover, these nanoneedles can also access specific regions (e.g, nuclei) inside living cells and deliver to target
areas, a feature not available with conventional delivery methods. However, itis a time-consuming technique
because of the need to manipulate each cell individually, limited by the availability of the nanoneedles, and
requires a highly specialised setup, trained operators and costly consumables.
———|
Size Analysis and Identification of Particles
Roger W. Welker, in Developments in Surface Contamination and Cleaning: Detection, Characterization, and
Analysis of Contaminants, 2012
2.3 Atomic Force Microscopy
The atomic force microscope (AFM) is not like other microscopic analysis methods; microscopes generally
produce an image using light or electrons. Its better to think of the AFM as a stylus gauge, rather than an optical
or electron optical imaging system (Fig. 4.24). In the AFM (Fig. 4.25), a tiny stylus is moved up and down over a
surface. The surface is moved in a precise x-y pattern under the moving stylus. The interaction of the stylus with
the surface is measured as the deflection of a cantilever beam. The measurement is made by observing the
deflection ofa laser beam reflected off the back of the cantilever. This combination of motions, back and forth for
the sample and up and down forthe stylus, produces a 3D image of the surface. The AFM is capable of nanometer
resolution. Various probes are available to perform magnetic force microscopy and some chemical analysis.
Surface-enhanced Raman spectroscopy is claimed to be able to produce spectra from single molecules.
a
Characterization and Simulation Technologies of
Nanomaterial
In Fundamentals and Applications of Nano Silicon in Plasmonics and Fullerines, 2008
7.1.2 Atomic Force Microscope
The ator
conducting surfaces. Its basic principle is based on measuring mechanical forces between the needle and the
surface, from which size is deduced, What is measured is deflection of the tip, which can be recorded and convert
to-a height (see Chapters 4 and 5). The deflections caused by this force allow the AFM to record topographic
features of the surface. The device measures vertical as well as lateral sizes of nanostructures. The vertical
dimension of the feature approach the real height; however the lateral dimensions are actually convolution of the
dimension of the feature with the diameter of the tip. It should be noted that unlike STM, AFM profiling is not
sensitive enough to image individual atoms. Because the tip may damage the surface, two modes of operation are
force microscope (AFM) generally uses a non-metallic needle placed over nanostructures on a non-
used:
+ Contact mode (repulsive mode): the probe is held a few nanometers above the sample. Due to the hard
contact, the sample and tip interact in this mode via a repulsive force+ Non-contact mode (attractive mode): the probe is held a few tens of nanometers above the sample and set to
vibrate above its natural frequency. In this mode, the tip and sample interact via an attractive molecular force.
This mode is well-suited for studying biological and some polymeric specimens. However this mode provides
poorer lateral resolution than the contact mode.
Nanoscale Drug-Delivery Systems
‘Anthony Singer, .. Shyam S. Mohapatra, in Nanocarriers for Drug Delivery, 2019
2.3.4 Atomic Force Microscopy
The atomic force microscope is a type of scanning probe microscope. Atomic force microscopy (AFM) allows for
three:
imensional characterization with a subnanometer resolution [31]. This technique can characterize NPs as
small as 0.5 nm, which makes it advantageous over other traditional techniques like DLS microscopy. Another
advantage of AFM is its ability to characterize different geometries of NPs. Other than measuring the size of the
NPs, AFM can be used to obtain other physical characteristics of the particles in the sample, such as the magnetic
properties, thermal conductivity, and electrical properties.
Scanning Probe and Particle Beam Microscopy
Alexandre Cuenat, Richard Leach, in Fundamental Principles of Engineering Nanometrology (Second Edition),
2014
7.3.2.2 Contaminated tips
‘An ideal AFM tip ends in a single point at its apex. However, manufacturing anomalies and/or contamination may
lead to double or even multiple tip ends. When this occurs, the tips can map features on the sample surface more
than once. For example, a double tip will result ina regular doubling of features. Such artefacts lead to what are
commonly termed double- or multiple-tip images. Contaminants on a tip can also interact with a sample surface,
leading to repeated patterns of the contaminants scattered across the surface. Cleaning of AFM tips and
cantilevers is highly recommended [22].Recommended
publications:
Carbon
Journal
Diamond and
Related Materials
Journal
Sensors and
Actuators A:
Physical
Journal
Nano Energy
Journal
Atomic Force Microscope-Based Nanorobotic System for
Nanoassembly
Lianging Liu, ... Heping Chen, in Nano Optoelectronic Sensors and Devices, 2012
4.1.3 AFM-Based Nanomanipulation
The AFM probe used for collecting image data can also work as an end effector to modify the sample surface
through the manioulation of oulling. scratching. pushing. and so on. In the last two decades. AFM has beenproven to be a powerful manipulation tool, with users taking advantage of its high precision and high resolution.
The pioneering work of AFM-based nanomanipulation can be tracked back to 1992 when Kim and Lieber
demonstrated the rearrangement of thin oxide structures on the underlying surface by increasing the applied load
during scanning with AFM (1). In 1995, Junno et al. assembled GaAs particles with diameters of 30nm into
arbitrary nanostructures by controlled pushing under ambient conditions (2). Schaefer et al. manipulated gold
nanoparticles in HOPG surface into two-dimensional arrays of nanometer-sized clusters [3] In 1998, Martin etal
assembled silver particle (with diameter 15nm) into an “LTL" pattern with AFM in noncontact mode [4]. In 2003,
Decossas et al. demonstrated they could straighten, bend, translate, reorient, and cut carbon nanotubes on glass
substrate using contact AFM [5]. Yang and Sacher reported their research on the influence of set point in Cu
particle manipulation with AFM (6). In 2004, Muller etal. performed a 3-nm width lithography in mica surface
with AFM [7] In 2005, for the first time, Sugimoto et al. achieved Sn atom manipulation on the surface of Ge in
normal temperature (8). Although all the above research progress has proved the powerful ability of AFM as a
‘manipulation tool, because AFM collects data for image by “feeling” rather than “looking,” there is no real-time
visual feedback available during manipulation due to the slow speed of AFM scan. Thus, all the above work is
carried out in the dark, and the operation result has to be verified by a new image scan after each step of the
manipulation. Obviously, this scan-designmanipulation-scan cycle is very time-consuming and has low
effectiveness.
To obtain the real-time feedback, some researchers tried to use a haptic technique and virtual reality interface to
facilitate AFM-based nanomanipulation. In addition to providing a virtual reality interface for the operator, Sitti
and Hashimoto linked a 1-DOF haptic device to the AFM system through which the operator can sense the
vertical force acting on the probe during manipulation [9]. However, the 1-DOF force feedback may provide
spurious force feeling because the manipulation force is mainly in the lateral direction instead of normal
direction. Guthold et a. 10] connected the AFM to a Phantom™ stylus (a haptic device from Sensable Inc.) with
the function of 3D force feedback. In imaging mode, the topography data from AFM are sent to the Phantom™,
and the operator can “feel” the topography of the sample. in manipulation mode, the Phantom™ can be used to
‘move the tip over the surface while keeping the internal normal force feedback on. However, its still not clear
whether the mapping from topography information to force information is helpful to the operation. Furthermore,
although a virtual reality interface can display a static virtual environment and a dynamic tip position, it does not
display the environment changes during manipulation. The operator is still “blind” because the environment
changes are not updated in real time. Thus, any method that can show the real-time changes of manipulation
result and provide more vivid 3D force feedback to the operator will significantly improve the efficiency and
effectiveness of AFM-based nanomanipulation. The followed AFM-based nanorobotic system is a feasible way to
approach this goal
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Seeing Atoms and Clusters on Surfaces
In Fundamentals and Applications of Nano Silicon in Plasmonics and Fullerines, 2018
4.6.5 Metal-Coated Silicon AFM Tips [28]
AFM tips are made either of pure silicon or of silicon nitride. Conventional photolithography is used to synthesizete tips. Une starts witn a tem x em piece ofa silicon water Yor example. Arter stanaara cleaning @ 4 jim thick
SiO; layer is grown by wet oxidation. The pattern for the tip is defined using standard photolithography with a
Mask aligner. This is followed by removal of the exposed silicon oxide (using BHF solution). The unexposed
photoresist is stripped by immersing the samples in acetone. KOH solution is now used to perform bulk
‘micromachining of silicon. This step results in making the AFM tip structure. The tip is imaged by SEM to record
the tip diameter and sharpness. Fig. 4.24 is an example of tips made.
For use in a harsh environment the tips can be coated with either platinum, iridium or gold. AFM probes can be
made with different force constants and resonant frequencies for the three modes of imaging: contact mode,
NC/tapping mode, and force modulation mode measurements. Harsh environment include applications in a
variety of wet as well as radiation intensive environments, The gold-coated tip is especially interesting for
applications in the fields of biology and life sciences.
[_| [Pures book
Sliding wear performance of epoxy-based nanocomposites
‘Ming Qiu Zhang, ... Ying Luo, in Tribology of Polymeric Nanocomposites (Second Edition), 2013
List of Abbreviations
ARM
atomic force microscope
AlOs
aluminum oxide
c
carbon
casiog
calcium silicate
CNTs
carbon nanotubes
CuO
copper oxide
pps
4
| 4-diaminodiphenysulfone
DMA
dynamic mechanical analyzer (or analysis)
psc
differential scanning calorimeter (or calorimetry)
EDs
X-ray energy dispersive spectroscopy
Ep
epoxyFeO,
trliron tetraoxide
FTIR
Fourier transform infrared
GMA
alycidyl methacrylate
Pc
gel permeation chromatograph
MWNTs
multiwalled carbon nanotubes
°
oxide
omMMT
organomodified montmorillonite
PGMA
polyglycidyl methacrylate
Pst
polystyrene
PTFE
polytetrafluoroethylene
scr
short carbon fiber
sos
sodium dodecyl sulfonate
sem
scanning electron microscope
si
silicon
sic
silicon carbide
SiC-g-PGMA
polyglycidyl methacrylate grafted silicon carbide nanoparticles
SiC-g-P(GMA-co-St)
copolymer of glycidyl methacrylate and styrene grafted silicon carbide nanoparticles
SisNe
silicon nitride
SiOz
silicon dioxide
SiO,-g-SMA
poly(styrene-co-maleic anhydride) grafted silicon dioxide nanopa-rticles
SMA
polystyrene-co-maleic anhydride)
st
stvreneTGA
thermogravimetric analyzer (or analysis)
TiO,
titanium dioxide
XPS
X-ray photoelectron spectroscopy
ZnO
zine oxide
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The Short-period (Si14/Ge1)20 and (Si28/Ge2)10
superlattices as Buffer Layers for the Growth of
Si0.75Ge0.25 Alloy Layers
M.M. Rahman, ...C. Tatsuyama, in Rapid Thermal Processing for Future Semiconductor Devices, 2003
3. Result and discussion X-ray diffraction (XRD) observation
X-ray diffraction data of all the samples showed very clear Si(004) and Sig7sGeo.s(004) alloy peaks (data is not
shown). We have chosen the alloy layer thickness above the critical thickness according to some well-known
reports [1,2]. Residual strain €,, perpendicular to the growth plane in the alloy layers was estimated from XRD
data using procedure discussed in [14]. Estimated residual strain is plotted in Fig. 2 as a function of the growth
‘temperature of the buffer layers. In A-type samples with Ge-1-monolayer mode SSL, itis seen that the residual
strain decreases monotonically with decreasing of the growth temperature of the buffer layers and reached a value
of about ~0.08% at 300°C. Lower growth temperature of buffer layers may have better layered structures, because
Ge segregation is lower for lower growth temperature. In our previous study, we have observed that substantial
intermixing occurs at the interface of the Si-Ge SSL prepared at S00°C[17]. But Ge surface segregation at 500°C
has been found to be suppressed with an increase of the Si deposition rate [18,19].
It is known there are upper limits on the number of strained-layer regions, which can be accommodated
elastically on a given substrate [20]. For Ge grown epitaxially on Si, the maximum number of Ge Mls can be
deposited is six [21]. But in the present experiment we have used only one ML and two MLs mode deposition.
‘Another point is worth noticeable; when
is deposited at lower temperature it introduces a large number of
point defects. The strain in the SSL layers can deflect the dislocations and point defects can capture threading
dislocations. As a result the upper layers not only become relaxed but also become smooth. The residual strain in
B-type samples with Ge-2-monolayer mode in SSL layers seems to show decreasing trend, but it is higher than
that of A-type samples. The reason of higher residual strain of this type of samples is not clear at this time.
Atomic Force Microscopy (AFM) Observation
AFM images of some samples of both types of samples are shown in Fig. 3, where 2(a-b) are samples (A-type) with
SSL buffers grown at 450 and 300 °C, respectively, 2(¢-d) are the samples (B-type) with buffers grown at 450 and
300°C, respectively All the images show the cross hatch patterns, which is related to the underlying grid of misfitdislocations. From the figure, itis seen that the height of troughs and crests of cross hatches is low.
Root-mean-squared (rms) surface roughness of all the samples is shown in Fig. 4 as a function of growth
temperature of the buffer layers. Without SSL buffer layer, the rms roughness of 2000-A-Sip7sGeo.s alloy is high
{about 40 A, data is not shown here), whereas samples with SSL buffer layer show dramatic reduction in
roughness. From Fig. 4, it is seen that the roughness of type-A samples is independent of the growth temperature
of SSL buffer layers and gives about a constant value (~12 A). As the strain energy increases with decreasing of the
growth temperature, which can effectively deflect the threading dislocation, may be the cause of the constant rms
roughness and smooth surface ofthe alloy layers. In the case of type-B samples rms roughness pattern is as like
type-A samples but its roughness value is higher that that of type-A samples. Two-monolayer mode Ge deposition
‘may cause island like pattern in the SSL structure. As a result, it may go to partial relaxation and ultimately can
not deflect threading dislocations. So roughness increases. Some spots on the type -B samples is the evidence of
the unfiltered threading dislocations.
Cross-sectional Transmission Electron Microscopy (XTEM) Observation
Some cross-sectional transmission electron microscopy (XTEM) images of type-A samples are shown in Fig. 5,
where 2000 A Sip.7sGeo,2s alloy layer with (a) 500°C-grown, (b) 450°C-grown and (c) 400°C-grown SSL buffer
layers. From the figure, itis seen that the upper alloy layers of all the samples are clear and free from dislocations.
A clear upper alloy is seen here, which is consistent with the lower roughness of AFM images. Different types of
dislocations are seen in the images with different temperature growth buffers. In Fig. 5(a), dislocation half loops
are seen in the substrate region. Dislocations are deflected from the strained layer superlattices. Pinning of
dislocations in Si substrate has been explained by LaGoues et al. [22]. V-shaped dislocations (Fig. Se) also shows
the filtering of dislocation.
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