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Presented by:-
DHRUBAJYOTI SADHUKHAN
CUJ/I/2015/INT/04
Content
 Introduction
 Advantage and disadvantage of AFM
 Experimental setup
 Imaging methods
 Force vs Distance curve
 Mode of AFM
 Contact mode
 Tapping Mode
 Non-contact mode
 Components of NC-AFM
 Mode of Operation
 Comparison between Modes of AFM
 Application
Invention
 Gerd Binning in 1986 invented
the AFM
 1st Experimental implementation
made by Gerd Binning,
Christoph Gerber and Calvin
Quate (1986)
 The first Non-Contact AFM
(NC-AFM) was developed by
Martin et al in 1987.
Introduction
 The STM measures the tunneling
current (conducting surface).
 The AFM measures the forces
acting between a fine tip and a
sample.
 The tip attached to the free
end of a cantilever and
brought very close to a
surface.
 Attractive or repulsive forces
resulting interactions between
the tip
▪ High resolution type of scanning
probe microscopy.
▪ Measures surface structure in length
scale 10nm-100μm.
▪ Provides height information of the
sample
▪ Can be imaged, very hard (ceramic
material) or very soft (human cells,
individual molecules of DNA)
▪ Used in all fields of science
Introduction
Atomic force microscope
ADVANTAGES AND DISADVANTAGES
OF AFM
ADVANTAGES
 Does not require a conductive
sample
 Ability to magnify in the X,Y,Z axes
 Works in ambient air or in a liquid
environment
 Cheap
 Small size advantage.
DISADVANTAGES
• Cannot be used for size
greater than 100μm
• Limited scanning speed
• Possibility of image variation
▪ Image does not reflect the
true sample topography,
Experimental setup of AFM
Working of AFM
Imaging methods
Contact mode
 Tip is in contact with the substrate
 High resolution
 Can damage surfaces
Non-contact mode (NCM)
▫ Tip is oscillating and not touching the
sample
Tapping mode
 Tip is oscillating and taps the surface
Lateral force microscopy (LFM)
 Tip is scanned sideways
 used to measure friction forces on the
nanoscale
Force Modulation Microscopy
 Rapidly moving the tip up and down
while pressing it into the sample.
 Possible to measure the hardness of
the surface and characterize it
mechanically
Forces versus distance curve
 The force measured by AFM can
be classified into long-range forces
and short-range forces.
 When scan at large distances from
the surface
 Van der Waals force,
capillary forces (due to the
water layer often present in an
ambient environment).
 When the scanning is in contact
with the surface the short range
forces
 quantum mechanical forces
or repulsive vander waal force
(Pauli Exclusion Principle
forces).
Modes of AFM
Contact mode
 (< 0.5 nm probe
surface separation
Tapping mode
 (0.5-2 nm probe-
surface separation)
Non contact Mode
 (0.1-10 nm probe-
surface separation)
Contact Mode
 Tip is dragged over the surface of the
sample.
 Cantilever bends, as the spring
constant of cantilever is less than
surface.
 Repulsive force on the tip
 The force between the probe and the
sample remains constant by
maintaining a constant deflection and
an image of the surface is obtained.
 The deflection of the cantilever Dx is
proportional to the force acting on the
tip,
▫ via Hook’s law, F=-k. x,
Tapping mode
 Cantilever oscillates close to
its resonance frequency.
 feedback loop ensures the
constant oscillation amplitude.
 Forces cause a change in the
 oscillation amplitude,
 resonant frequency
 phase of the cantilever.
Non-Contact Mode AFM
▪ To avoid problems caused by
capillary forces, the sample is
immersed in a liquid.
▪ This procedure is especially
beneficial for biological
samples.
▪ The probe operates in the
attractive force region and the
tip sample interaction is
minimized.
 Allowed scanning without influencing the shape of the sample by
the tip-sample forces.
 The cantilever of spring constant of 20- 100 n/m
 Non-contact mode: amplitude set as ~ 100% of “free” amplitude; •
Non-Contact Mode AFM
Tapping vs NC AFM Contact vs NC AFM
Non-Contact Mode AFM
Components Of The Microscope
▪ Piezocrystals
▫ ceramic materials
▫ develop an electrical potential in
response to mechanical
pressure.
▪ Probe
▫ The probe represents a micro-
machined cantilever with a sharp
tip at one end, which is brought
into interaction with the sample
surface.
▪ Beam Deflection Detection
▫ To detect the displacement of
the cantilever, a laser is
reflected off the back of the
cantilever and collected in a
photodiode.
▪ Cantilever
▫ V-shaped cantilever-
▫ Providing low mechanical
resistance to vertical
deflection, and high resistance
to lateral torsion.
Components Of The Microscope
Sensors
Silicon micro cantilever
▪ Produced from etching small (~100×10×1 μm) rectangular,
triangular, or V-shaped cantilevers from silicon nitride.
▪ Tend to have a higher stiffness, ~40 N/m, and resonant frequency,
~200 kHz, than contact AFM cantilevers (with stiffness's ~0.2 N/m
and resonant frequencies ~15 kHz).
▪ The reason for the higher stiffness to stop the probe snapping to
contact with the surface due to Van der Waals forces.
▪ Tips can be coated for specific purposes, such as a ferromagnetic
coatings for use as a magnetic force microscope.
▪ By doping the silicon, the sensor can be made conductive.
qPlus sensor
▪ Used in many ultra-high vacuum NC-AFMs.
▪ The sensor was originally made from a quartz tuning fork from a
wristwatch, consists of two coupled lines that oscillate opposed
to each other,
▪ qPlus sensor has only one tine that oscillates.
▪ Invented in 1996 by physicist Franz J. Giessibl.
▪ Can be used for combined STM/NC-AFM operation.
▪ The tip can either be electrically connected to one of tuning fork
electrodes, or to a separate thin (~30μm diameter) gold wire.
▪ The sensor stiffness, ~1800 N/m
▪ The resonant frequency, ~25 kHz
Modes of operation
Frequency modulation
▪ Introduced by Albrecht, Gretter, Horne and Rugar in 1991,
▪ To maintain excitation on resonance it must keep a
90° phase difference between the excitation and response of
the sensor.
▪ This is done by driving the sensor with the deflection signal
phase shifted by 90°.
▪ The change in resonant frequency ( f) can be used, either
in feedback mode, or in constant height mode.
Amplitude modulation
 Introduced by binnig and quate in their seminal 1986
 The sensor is excited just off resonance to detect forces
which change the resonant frequency.
 Advantage is that there is one feedback loop (the
topography feedback loop)
▪ Measures surface
topography by the
attractive inter-atomic force
between the tip and a
sample surface (Figure 1).
▪ Piezoelectric modulator is
used to vibrate the
cantilever near its resonant
frequency (Figure 2) as it
passes over a surface, and
correlate changes in the
cantilever’s vibrations to
topographical features.
Working Non-Contact Mode AFM
Figure 1
Figure 2
▪ Tip approaches a sample,
the van der Waals attractive
force between the tip and
the sample causes changes
in both the amplitude and
the phase of the cantilever
vibration (see Figure 3).
▪ These changes are
monitored by a Z-servo
system feedback loop to
control the tip sample
distance (see Figure 4).
Working Non-Contact Mode AFM
Figure 3
Figure 4
Advantages of Non Contact AFM Modes over
Contact and Tapping Mode
 Contact Mode AFM
 Lateral forces can distort the image.
 deformation
 Capillary forces from a fluid layer can cause large forces
normal to the tip sample interaction.
 Combination of these forces reduces spatial resolution
and can cause damage to soft samples.
 High contact pressure
 Tapping Mode AFM
 Slower scan speed than in contact mode.
 contamination of the tip is possible
 tip is damaged after several scans
Advantages of Non Contact AFM Modes over
Contact and Tapping Mode
Advantage of Non-contact Mode AFM
 Low force is exerted on the sample surface and
 no damage is caused to soft samples
 No contamination of tip
 no limitation in tip’s sharpness
Disadvantages of NC-AFM
- Lower lateral resolution, limited by tip-sample
separation.
- Slower scan speed
- Usually only applicable in extremely hydrophobic
samples with a minimal fluid layer.
Applications of NC-AFM
Some possible application are:
- Substrate roughness analysis.
- Step formation in thin film epitaxial deposition.
- Pin-holes formation.
- Grain size analysis.
- Phase mode is very sensitive to variations in material
properties, including surface stiffness, elasticity and
adhesion.
- Comparing the tip-samples forces curves for materials to
study the ratio of Young´s Modulus (graphite as a
reference for measure of the indentation).
- Obtaining information of what happening under indentation
at very small loads.
Reference
▪ https://www.azonano.com/article.aspx?ArticleID=3010
▪ https://en.wikipedia.org/wiki/Non-contact_atomic_force_microscopy
▪ http://www.parksystems.com/index.php/park-spm-modes/91-standard-imaging-mode/217-true-non-
contact-mode
▪ http://www.parksystems.com/index.php/park-spm-modes/91-standard-imaging-mode/217-true-non-
contact-mode
▪ Principles of Atomic Force Microscopy (AFM) Arantxa Vilalta-Clemente Aristotle
University,Kathrin Gloystein Aristotle University
▪ Y. Martin, C.C. Williams, H.K. Wickramasinghe, J. Appl. Phys. 61, 4723 (1987).
▪ Q. Zhong, D. Innis, K. Kjoller, V.B. Elings, Surf. Sci. Lett. 290, L688 (1993).
▪ Heyde, M.; Kulawik, M.; Rust, H.-P.; Freund, H.-J. (2004). "Double quartz tuning fork sensor for
low temperature atomic force and scanning tunneling microscopy". Review of Scientific
Instruments. 75 (7): 2446
Thank You

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Non contact mode (AFM)

  • 2.
  • 3. Content  Introduction  Advantage and disadvantage of AFM  Experimental setup  Imaging methods  Force vs Distance curve  Mode of AFM  Contact mode  Tapping Mode  Non-contact mode  Components of NC-AFM  Mode of Operation  Comparison between Modes of AFM  Application
  • 4. Invention  Gerd Binning in 1986 invented the AFM  1st Experimental implementation made by Gerd Binning, Christoph Gerber and Calvin Quate (1986)  The first Non-Contact AFM (NC-AFM) was developed by Martin et al in 1987.
  • 5. Introduction  The STM measures the tunneling current (conducting surface).  The AFM measures the forces acting between a fine tip and a sample.  The tip attached to the free end of a cantilever and brought very close to a surface.  Attractive or repulsive forces resulting interactions between the tip
  • 6. ▪ High resolution type of scanning probe microscopy. ▪ Measures surface structure in length scale 10nm-100μm. ▪ Provides height information of the sample ▪ Can be imaged, very hard (ceramic material) or very soft (human cells, individual molecules of DNA) ▪ Used in all fields of science Introduction Atomic force microscope
  • 7.
  • 8. ADVANTAGES AND DISADVANTAGES OF AFM ADVANTAGES  Does not require a conductive sample  Ability to magnify in the X,Y,Z axes  Works in ambient air or in a liquid environment  Cheap  Small size advantage. DISADVANTAGES • Cannot be used for size greater than 100μm • Limited scanning speed • Possibility of image variation ▪ Image does not reflect the true sample topography,
  • 11. Imaging methods Contact mode  Tip is in contact with the substrate  High resolution  Can damage surfaces Non-contact mode (NCM) ▫ Tip is oscillating and not touching the sample Tapping mode  Tip is oscillating and taps the surface Lateral force microscopy (LFM)  Tip is scanned sideways  used to measure friction forces on the nanoscale Force Modulation Microscopy  Rapidly moving the tip up and down while pressing it into the sample.  Possible to measure the hardness of the surface and characterize it mechanically
  • 12. Forces versus distance curve  The force measured by AFM can be classified into long-range forces and short-range forces.  When scan at large distances from the surface  Van der Waals force, capillary forces (due to the water layer often present in an ambient environment).  When the scanning is in contact with the surface the short range forces  quantum mechanical forces or repulsive vander waal force (Pauli Exclusion Principle forces).
  • 13. Modes of AFM Contact mode  (< 0.5 nm probe surface separation Tapping mode  (0.5-2 nm probe- surface separation) Non contact Mode  (0.1-10 nm probe- surface separation)
  • 14. Contact Mode  Tip is dragged over the surface of the sample.  Cantilever bends, as the spring constant of cantilever is less than surface.  Repulsive force on the tip  The force between the probe and the sample remains constant by maintaining a constant deflection and an image of the surface is obtained.  The deflection of the cantilever Dx is proportional to the force acting on the tip, ▫ via Hook’s law, F=-k. x,
  • 15. Tapping mode  Cantilever oscillates close to its resonance frequency.  feedback loop ensures the constant oscillation amplitude.  Forces cause a change in the  oscillation amplitude,  resonant frequency  phase of the cantilever.
  • 16. Non-Contact Mode AFM ▪ To avoid problems caused by capillary forces, the sample is immersed in a liquid. ▪ This procedure is especially beneficial for biological samples. ▪ The probe operates in the attractive force region and the tip sample interaction is minimized.
  • 17.  Allowed scanning without influencing the shape of the sample by the tip-sample forces.  The cantilever of spring constant of 20- 100 n/m  Non-contact mode: amplitude set as ~ 100% of “free” amplitude; • Non-Contact Mode AFM Tapping vs NC AFM Contact vs NC AFM
  • 19. Components Of The Microscope ▪ Piezocrystals ▫ ceramic materials ▫ develop an electrical potential in response to mechanical pressure. ▪ Probe ▫ The probe represents a micro- machined cantilever with a sharp tip at one end, which is brought into interaction with the sample surface.
  • 20. ▪ Beam Deflection Detection ▫ To detect the displacement of the cantilever, a laser is reflected off the back of the cantilever and collected in a photodiode. ▪ Cantilever ▫ V-shaped cantilever- ▫ Providing low mechanical resistance to vertical deflection, and high resistance to lateral torsion. Components Of The Microscope
  • 21. Sensors Silicon micro cantilever ▪ Produced from etching small (~100×10×1 μm) rectangular, triangular, or V-shaped cantilevers from silicon nitride. ▪ Tend to have a higher stiffness, ~40 N/m, and resonant frequency, ~200 kHz, than contact AFM cantilevers (with stiffness's ~0.2 N/m and resonant frequencies ~15 kHz). ▪ The reason for the higher stiffness to stop the probe snapping to contact with the surface due to Van der Waals forces. ▪ Tips can be coated for specific purposes, such as a ferromagnetic coatings for use as a magnetic force microscope. ▪ By doping the silicon, the sensor can be made conductive.
  • 22. qPlus sensor ▪ Used in many ultra-high vacuum NC-AFMs. ▪ The sensor was originally made from a quartz tuning fork from a wristwatch, consists of two coupled lines that oscillate opposed to each other, ▪ qPlus sensor has only one tine that oscillates. ▪ Invented in 1996 by physicist Franz J. Giessibl. ▪ Can be used for combined STM/NC-AFM operation. ▪ The tip can either be electrically connected to one of tuning fork electrodes, or to a separate thin (~30μm diameter) gold wire. ▪ The sensor stiffness, ~1800 N/m ▪ The resonant frequency, ~25 kHz
  • 23. Modes of operation Frequency modulation ▪ Introduced by Albrecht, Gretter, Horne and Rugar in 1991, ▪ To maintain excitation on resonance it must keep a 90° phase difference between the excitation and response of the sensor. ▪ This is done by driving the sensor with the deflection signal phase shifted by 90°. ▪ The change in resonant frequency ( f) can be used, either in feedback mode, or in constant height mode.
  • 24. Amplitude modulation  Introduced by binnig and quate in their seminal 1986  The sensor is excited just off resonance to detect forces which change the resonant frequency.  Advantage is that there is one feedback loop (the topography feedback loop)
  • 25. ▪ Measures surface topography by the attractive inter-atomic force between the tip and a sample surface (Figure 1). ▪ Piezoelectric modulator is used to vibrate the cantilever near its resonant frequency (Figure 2) as it passes over a surface, and correlate changes in the cantilever’s vibrations to topographical features. Working Non-Contact Mode AFM Figure 1 Figure 2
  • 26. ▪ Tip approaches a sample, the van der Waals attractive force between the tip and the sample causes changes in both the amplitude and the phase of the cantilever vibration (see Figure 3). ▪ These changes are monitored by a Z-servo system feedback loop to control the tip sample distance (see Figure 4). Working Non-Contact Mode AFM Figure 3 Figure 4
  • 27. Advantages of Non Contact AFM Modes over Contact and Tapping Mode  Contact Mode AFM  Lateral forces can distort the image.  deformation  Capillary forces from a fluid layer can cause large forces normal to the tip sample interaction.  Combination of these forces reduces spatial resolution and can cause damage to soft samples.  High contact pressure  Tapping Mode AFM  Slower scan speed than in contact mode.  contamination of the tip is possible  tip is damaged after several scans
  • 28. Advantages of Non Contact AFM Modes over Contact and Tapping Mode Advantage of Non-contact Mode AFM  Low force is exerted on the sample surface and  no damage is caused to soft samples  No contamination of tip  no limitation in tip’s sharpness
  • 29. Disadvantages of NC-AFM - Lower lateral resolution, limited by tip-sample separation. - Slower scan speed - Usually only applicable in extremely hydrophobic samples with a minimal fluid layer.
  • 30. Applications of NC-AFM Some possible application are: - Substrate roughness analysis. - Step formation in thin film epitaxial deposition. - Pin-holes formation. - Grain size analysis. - Phase mode is very sensitive to variations in material properties, including surface stiffness, elasticity and adhesion. - Comparing the tip-samples forces curves for materials to study the ratio of Young´s Modulus (graphite as a reference for measure of the indentation). - Obtaining information of what happening under indentation at very small loads.
  • 31. Reference ▪ https://www.azonano.com/article.aspx?ArticleID=3010 ▪ https://en.wikipedia.org/wiki/Non-contact_atomic_force_microscopy ▪ http://www.parksystems.com/index.php/park-spm-modes/91-standard-imaging-mode/217-true-non- contact-mode ▪ http://www.parksystems.com/index.php/park-spm-modes/91-standard-imaging-mode/217-true-non- contact-mode ▪ Principles of Atomic Force Microscopy (AFM) Arantxa Vilalta-Clemente Aristotle University,Kathrin Gloystein Aristotle University ▪ Y. Martin, C.C. Williams, H.K. Wickramasinghe, J. Appl. Phys. 61, 4723 (1987). ▪ Q. Zhong, D. Innis, K. Kjoller, V.B. Elings, Surf. Sci. Lett. 290, L688 (1993). ▪ Heyde, M.; Kulawik, M.; Rust, H.-P.; Freund, H.-J. (2004). "Double quartz tuning fork sensor for low temperature atomic force and scanning tunneling microscopy". Review of Scientific Instruments. 75 (7): 2446