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Scanning probe microscopies (SPM)
Principle: A nano-sized probe is brought close to a sample surface and scanned along the surface while some physical property is recorded
Techniques:
• STM (Scanning Tunneling Microscopy)
• AFM (Atomic Force Microscopy)
• SFM (Scanning Force Microscopy)
• DFM (Differential Force Microscopy)
• SNOM (Scanning Near-field Optical Microscopy)
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STM (Scanning Tunneling Microscopy)Scanning microscopy:• 1970’s: Young developed the first non-contact “feeler” microscope• 1980’s: Binnig and Rohrer developed the first stable STM. They earned the Noble price in 1986
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In classical physics an electron cannot penetrate into or across a potential barrier if its energy E is smaller than the potential Φ within the barrier
• A quantum mechanic treatment predicts an exponential decaying solution for the electron wave function in the barrier. And for a rectangular barrier we get:
• The probability of finding an electron behind the barrier of width s is now:
• And the transition probability T can be expressed:
( )( ) ( ) ( ) ( ) ( )
2
2 2
2 0 0 2 /zd z m E z z e where m Edz
−κΨ− Φ− Ψ = → Ψ = Ψ κ= Φ−
zs
( ) ( ) ( )2 2 20 sP s s e− κ= Ψ = Ψ
( ) ( )22 2
16 2 with the approximation s 1 and sE V E m V E
T eV
− κ− −= κ κ=
Φ is the workfunction, often approximated to Φ = ½ (Φsample + Φtip)
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• The current is proportional to the probability of electrons to tunnel through the barrier:
• With 5 eV as a typical example for a workfunction value, a change in 1 Å in distance between tip and sample (s increases by 1 Å) causes a change of nearly one order of magnitude in current! This high sensitivity facilitates a high vertical resolution!
( )2 20
F
n F
Es
nE E eV
I e− κ
= −
∝ Ψ∑
Iron on cupper
STM can only be used to study conducting materials
(and to some degree semiconductors)
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Modes of operation
Constant-Current Mode Constant-Height Mode
• The distance between tip and sample is constant and a x-y-scan gives a topographic image of the surface
• Better vertical resolution
• Slower scanning can give drift in the x-y-scan
• Used for surfaces that aren’t atomically flat
• The tip height is kept constant and tunneling current is monitored
• Lower vertical resolution
• Very fast scans minimal image distortion due to drift
• Allows studies of dynamical processes
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Bardeen Approach• Another way of describing electron tunneling comes from Bardeen’s approach which makes use of the time dependent perturbation theory. The probability of an electron in the state Ψ at EΨ to tunnel into a state χ at Eχ is given by Fermis’s Golden Rule:
• The tunneling matrix element is given by an integral over a surface in the barrier region laying between the tip and the sample:
• δ(EΨ - Eχ) means that an electron can only tunnel if there is an unoccupied state with the same energy in the other electrode (thus inelastic tunneling is not treated).
• In case of a negative potential on the sample the occupied states generate the current, whereas in case of a positive bias the unoccupied states of the sample are of importance. Therefore, by altering the voltage, a complete different image can be detected as other states contribute to the tunneling current. This is used in tunneling spectroscopy.
( )22P M E EΨ χ
π= δ −
2d dM dS
m dz dz
∗∗
⎛ ⎞Ψ χ ⎟⎜ ⎟= χ −Ψ⎜ ⎟⎜ ⎟⎜⎝ ⎠∫∫
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The occupied states of (00-1) SiC
The unoccupied states of (00-1) SiC
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AFM (Atomic Force Microscopy)
A feedback system to control the vertical position of the tip
A computer system that drives the scanner, measures data and converts the data into an image
A piezoelectric scanner which moves the sample under the tip (or the tip over the sample) in a raster pattern
Means of sensing the vertical position of the tip
A coarse positioning system to bring the tip into the general vicinity of the sample
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A computer system that drives the scanner, measures data and converts the data into an image
A piezoelectric scanner which moves the sample under the tip (or the tip over the sample) in a raster pattern
Definition of a piezoelectric material: A material that generates an electric charge when mechanically deformed. Conversely, when an external electric field is applied to piezoelectric materials they mechanically deform
Photodiode
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The cantilever/tip system
The tip is usually a non-conductingmaterial like Si3N4, SiO2 or Si
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AFM monitors interfacial forcesF α (1/d)x
F = interfacial forced = tip-sample separation
Interfacial forces include:• repulsive forces (contact AFM)• van der Waals forces (non-contact AFM)• electrostatic forces (EFM)• magnetic forces (MFM)• chemical forces (CFM)
The interfacial forces are typically in the range pN - nN
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The Force-Distance curve
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Modes of operation:
• Contact mode• Non-contact mode• Tapping mode
Non-contact mode
Contact mode
Contact mode:
• Tip in contact with sample surface
• Monitor cantilever deflection
• Monitor lateral forces
Non-contact mode:
• Tip oscillates just above sample surface
• Monitor Van der Waals forces between tip and sample
• Lower resolution than contact mode
• Lateral forces on the sample are reduced
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Contact and Lateral force AFM
Langmuir-Blodgett film (1 µm scan). (a) Topography image and (b) LFM image.
(a) (a)(b) (b)
Mica surface (3 nm scan). (a) Topography image and (b) LFM image.
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Tapping mode AFM• Tip oscillates while scanning across the sample surface
• Resolution similar to contact mode
• Lateral forces on the sample are reduced because of the tapping motion
The cantilever amplitude is monitored
(Light colors are higher)
(Light color correspond to higher surface
modulus/stiffness)
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Magnetic Force Microscopy (MFM)• Tip cantilever tip is now coated with a soft-magnet material
• The cantilever deflects when is scans over the magnetized domains
• MFM images locally magnetized domains
• Magnitude of deflection (up/down) is proportional to sample magnetization
• MFM is used to determine the local magnetization variation
MFM image showing the bits of a hard drive (30 x 30 µm)
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Electrostatic Force Microscopy (EFM)• Voltage is applied between tip and sample while cantilever hovers above sample
• The cantilever deflects when is scans over static charges
• EFM plots locally charged domains similar to MFM plots of magnetic domains
• Magnitude of deflection is proportional to the charge density
• EFM is used to determine the local charge density variation
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Parameter SEM AFM
Operating environment
Depth of field
Resolution (x,y)
Resolution (z)
Magnification range
Sample preparation
Vacuum
Large
~ 5 nm
10 - 106
Soft materials: Freeze
drying, coating
Ambient, liquid, vacuum
Medium
0.1 – 0.3 nm
0.01 nm
5·102 - 108
None
Comparison between SEM and AFM:
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Scanning Near-field Optical Microprobe
(SNOM)or
Near-field ScanningOptical Microprobe
(NSOM)• Diffraction imposes a natural limit to available resolution with conventional optics. The best confocal microscopes can obtain ~ 250 nm resolution.
• The idea of SNOM is to use an optic fiber, tapered at the exit end and having an exit diameter only a few fractions of the wavelength of the light in the beam
• The distance between the radiation source (tapered exit) and the sample surface must then also be short compared to the radiation wavelength
Two fundamental differences between near-field (NF) and far-field (FF) (conventional) optical microscopy:
1. In NF microscopy the NF interaction region is much smaller than the FF interaction area for conventional microscopy
2. NF microscopy has a sub-wavelength distance between the radiation source and the sample while FF microscopy has much larger distance
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SNOM/NSOM today is very similar to standard scanning probe microscopy, but with an optical channel
Mechanical:
• Translation stage, piezoelectric scanner
• Feedback control (z-distance)
• Anti-vibration optical table
Electrical:
• Scanning drivers for piezoelectric scanner
• Z-distance control
• Amplifiers, signal processors
• Software and computer
Optical:
• Light source (lasers), fiber, mirrors, lenses, objectives
• Photon detectors (photon multiplier tupe, charge coupled devices (CCD)
• Probe to give the window to the near-field
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Commercial NSOM:
Nanonics MultiView 2000
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Two different probe types are being used:
1. Aperture type• Taped fiber, multiple-taped fibre
• Cantilevered AFM/NSOM tips (Si3N4, SiO2)
• Other kinds, such as tetrahedral tip, fluorescent tip
• Metal coating optional
2. Apertureless type• Dielectrics, semiconductors or metals
• Other kinds, such as nano-particle attached tip
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What can we do with NSOM/SNOM?1. Ultrahigh resolution OPTICAL Imaging/Plasmonic studies
2. Spectroscopy
• Near-field Surface Enhanced Raman Spectroscopy
• Local Spectroscopy of Semiconductor Devices
• Near-field Broadband Spectroscopy
3. Modification of surfaces
• Sub-wavelength photolithography (write patterns into a photoresist)
• Ultra High Density data storage (write and read data on magneto-optical materials)
• Laser Ablation (nano-lithography, photo mask repair)
4. Near-field femtosecond studies
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High resolution:
A resolution of 25 nm (or one-twentieth of the 488 nm radiation wavelength) have been demonstrated by the IBM group by utilizing a test specimen consisting of a fine metal line grating
Limitations of near-field optical microscopy:
• Practically zero working distance and an extremely small depth of field
• Extremely long scan times for high resolution images or large specimen areas.
• Very low transmissivity of apertures smaller than the incident light wavelength.
• Only features at the surface of specimens can be studied