an ultimate tool for nanoscience and nanotech · scanning probe microscopy an ultimate tool for...
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Scanning Probe MicroscopyAn Ultimate Tool for Nanoscience and Nanotech
Lin Huang, PhD
Digital Instruments
Veeco Metrology Group
Invited Presentation at AVS Thin Film Division Meeting, July 17, 2002, Sunnyvale
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Basic Components Diagram of an SPM
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What SPM Can Do in NanoWorld?
• Visualize atoms, molecules and nanostructures
• Manipulate materials down to atom by atom
• Probe other sample characteristics at nanoscale
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Observing Atoms with STM
Au(111) reconstruction in air Si(111)7x7 in UHV
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Visualization of Single Macromolecules with AFM
Annealing of Jacketed
Polystyrene on HOPG
40°C
30°CCooperation w/ B.Tartsch and M. Moeller (Ulm Uni)
2.85 µm
1.4 µm
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Nanotube on Si with Electrodes Sample courtesy of Prof. Park (Harvard Univ.)
20 µm scan 400 nm scan with Z-range of 8 nm
Fe clusters on GaAs
Nanostructures Imaged with AFM
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Problems with SPM Imaging
One of the Solutions
Tapping Mode Fast Scanning Scan Speed improved by factor of 10
•NSIV Controller•Micro-actuated Probe
•Slow scan speed
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Problems with Speeding up TappingModeProblems with Speeding up TappingModeTMTM
•• Slow, asymmetric error growth rateSlow, asymmetric error growth rate•• Fast scan increases amp. errorFast scan increases amp. error•• High setpoint �����������High setpoint �����������•• Low setpoint ����� ���������������Low setpoint ����� ���������������
AmpAmp. . Error Error
ScanScan
StandardStandard
Response speed of elements in feedback loop
Frequency (Hz)
1 10 100 10001 10 100 1000 1000010000
• Low bandwidth of tube Z• Resonant F 0.7 kHz ~ 5 kHz • Low gains ��������������• High gains ����������
OPTIMIZE SYSTEMOPTIMIZE SYSTEM MINIMIZE ERRORMINIMIZE ERROR
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Improvements in the NSIV Controller
ImprovedImprovedMicroMicro--actuatedactuated
CantileverCantilever
Standard Silicon Probe
• Large cantilever with ZnO
actuator.
• Resonant frequency ~ 50 kHz
• Actuator provides both oscillation
and fast deflection in Z
• Z-range about 700 nm
T. Sulchek et al. Appl. Phys. Lett. 76, 1473 (2000).
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High Speed with Resolution
1.5 Hz Fast Tapping 15 Hz
340 s340 s 34 s34 s
5.5 µm
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TappingMode+ Fast Scanning
Fe nanoparticles on GaAs. Individual nanoparticles and atomic terraces typical of epitaxial growth, along with other surface detail, are visible in both images.
2µm
< 30 secondsTappingMode+> 5 minutes
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High Speed with Molecular Resolution
Height 2 nm Phase 30o
Scan rate 8 H z
500 nm
V3V3
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High Speed with Accuracy
SLZ only @ 1 HzDepth=115.8 nm
FSZ only @ 11 HzDepth=113.4 nm
*SLZ and FSZ are calibrated separately with a VLSI 180 nm standard.
5 µm
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What SPM Can Do in NanoWorld?
• Visualize atoms, molecules and nanostructures
• Manipulate materials down to atom by atom
• Probe other sample characteristics at nanoscale
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Manipulating A&M with STM
CO on Pt(111)
P. Zeppenfeld & D. EiglerLutz & Eigler
Fe on Cu(111)
Kanji characters for "atom."
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Manipulating Nanocrystals with STM
APL, Chey, Huang and Weaver
Ag Nanocrystals on Si(111)7x7
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Problems with SPM Manipulations
One of the Solutions
NanoMan Platform for Nano-scale Manipulation and Lithography
•Hardware: Dimension Closed Loop Head•Software: NanoMan Interface
•Piezo problem in open loop scanners•Control of actuate positioning
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Hardware: Dimension “CL” SPM Head
� Most advanced scanning and nanoscale positioning
� Closed loop with lateral noise < 2 nm RMS, 6 nm p-p
� <1% nonlinearity with Max. scan size 100 µm
CL
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Dimension “CL” SPM Performance
VLSI certified STS3 pitch 3.00+/- 0.02µmMean=3.00µm, integral non-linearity ~ 0.04%, differential non-linearity ~ 0.45%.
ASM 150-1D pitch 144.5nm +/- 0.5nm (Al/Glass)Mean=144.7nm,integral non-linearity < 0.1%,differential non-linearity < 2.5%.
Linear and Accurate
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• ~8nm wide parallel polymer lamellae. XY closed-loop feedback active.
Dimension “CL” SPM PerformanceLow-noise
300nm
Topography Phase
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Software: Dedicated User Interface
Interface for direct control of nanopositioning, scripting, and lithography
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Nudging the Nanotubes
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Manipulation of Single Macromolecules
•Manipulation of
jacketed polystyrene
molecules on HOPG;
500 nm scan
•Imaging Mode:
Tapping
•Manipulation Mode:
constant height
•Dotted lines indicate
the tip motion
1
43
2
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Pushing Au Particles on Mica
• Manipulation of 50 nm Au
balls on Mica; 3 um scan
• Imaging Mode: Tapping
• Manipulation Mode:
constant height
1
23
4
5
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Lithography: Anodic Oxidation of Si
“no job too small”
~15 nm line widths
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What SPM Can Do in NanoWorld?
• Visualize atoms, molecules and nanostructures
• Manipulate materials down to atom by atom
• Probe other sample characteristics at nanoscale
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•Magnetic Force Microscopy (MFM)•Electric Force Microscopy (EFM)•Current Measurements in Contact AFM
•TUNA•Conductive AFM
•Scanning Capacitance Microscopy (SCM)•Scanning Thermal Microscopy
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(60 µm, Z-scale = 2 de)120 OC100 OC80 OC
60 OC40 OC26 OC
MFM Phase Images of Garnet
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Height EFM Phase 3 m scan
EFM on Rubber Modified Polypropylene with 10% Carbon Black
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Application Modules
• Scanning Capacitance• Scanning Spreading
Resistance• Tunneling AFM• Conductive AFM• Scanning Thermal
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Scanning Capacitance Microscopy
• Measures capacitance variations between a conductive probe and semiconductor sample while scanning in contact mode
• Produces a 2D image of near surface variations in carrier concentration with a sensitivity range of 1015-1020 carriers/cm3 and a lateral resolution of 10 to 20 nm
500 nm
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SCM Sensor
Sample
Resonator
Detector
VCO
Gain & Filter
CTRL
Lock In Amp Oscillator
Ref
dC/dV
AC +DC Bias
Fly Lead
HzFMeasuredySensitivit 22103: −×
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Operation of Scanning Capacitance System
Courtesy: R. Klienman
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Capacitance of unexpected 8V avalanche breakdown
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SCM on Ferro-Electric PZT film
SCM dC/dV topography
domain imaging and manipulation
Courtesy: P DeWolf
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Current Measurements in Contact Mode
TUNA C-AFMGain 1 pA / V 1 nA / V Noise (RMS) 50 fA 1 pA Range 80 fA – 100 pA 2 pA – 1 A
DC bias voltage(-12V to +12V)
conductive AFM probe to ADC
pA-Amplifierextra gain+ filter
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TUNAFM on SiO2 with Embedded Defects
-2V -3V -4V
-5V -6V -6V
Scan size: 1x1 µm2
Si
SiO2
Nano-crystal Si
Courtesy: S Madhukar
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TUNA on MR Head (Data-Storage)
Topography Tunneling current
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TUNA on Conductive Polymer
Topography: 50µmCurrent: Bias voltage: -6V
RMS current: 190fA - 1.6pA
PPVon
PANI
PANI
low
highercurrent
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Standard Si3N4 tip/cantilever assembly
Metal film conductors on either side of the tip
High thermal coefficient of resistivity film along the side of tip.
TCR of the sensor ~ 2.3 x10-3/oC
Thermosensitive Probe
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Working principle
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Topography Temperature Map
MR Element
20 µm
SThM Measurement of MR Head
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Invar puck on heater with controlled ramping rate: 10 K/minute from 35°C to 45°C
Sensitivity:~ 7.5 K/V
Sensitivity Calibration
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Temperature Profile of Laser Diode
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A: center of the hot line; B: 25 µm from A to the right
Topography and Thermal Images
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•• Each probes calibrated individuallyEach probes calibrated individually
Measurement with 5 Probes