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

Non contact mode (AFM)

  • 1.
  • 3.
    Content  Introduction  Advantageand 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 Binningin 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 STMmeasures 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 resolutiontype 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
  • 8.
    ADVANTAGES AND DISADVANTAGES OFAFM 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,
  • 9.
  • 10.
  • 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 distancecurve  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 Contactmode  (< 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  Tipis 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  Cantileveroscillates 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 scanningwithout 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
  • 18.
  • 19.
    Components Of TheMicroscope ▪ 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 DeflectionDetection ▫ 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 ▪ Usedin 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 Frequencymodulation ▪ 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  Introducedby 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 topographyby 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 approachesa 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 NonContact 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 NonContact 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 Somepossible 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
  • 32.