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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
The wondrous world of carbon nanotubes
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
Overview• Introduction• Synthesis & Purification• Overview of applications• Single nanotube measurements• Energy storage• Molecular electronics• Conclusion and future outlook
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
• Discovered in 1991 by Iijima• Unique material properties• Nearly one-dimensional structures• Single- and multi-walled
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
What is a nanotube?
• Responsible bond:• Unit cell: honeycomb pattern• Wrapping these patterns back on top
of themselves and joining the edgesCarbon nanotube
2SP
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
Single and Multi-wall nanotube • Single wall nanotube:
– SWNT– single atomic layer wall,
diameter of 1-5 nm – excellent mechanical
property– hot topic now
• Multi wall nanotube:– MWNT– Inner diameter: 1.5 – 15 nm– Outer diameter: 2.5 – 30 nm– ~ 50 layers – containing more structure
defects
(http://www.lbl.gov)
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
Basis contains two atoms
nmdda 14.0,3 ==
2D graphite sheet
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
Orientation defined by Hamada vector (n,m) r = n a + m b
Common orientations:
• armchair (5,5)
• zigzag (9,0)
• chiral (10,5)
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
The Electrical Properties of nanotube• Can be either Metal or semiconductor
– Controlled by Rolling DirectionCh (rolling vector)= na + mb (unit vector)
Rule: = integer metallic
non-integer semiconductor
• Electrical Conductivity– Four Point Probe Method to determine sheet resistance and conductivity
3mn +
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
History Buckyball ( )
• The discovery of Buckyball is by accident, from Radio-astronomy
• Around 1970s
• The discovery of nanotubes comes from Buckyball
60C
(http://www.slb.com )
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
The first computer circuit composed of only one single carbon nanotube
IBM2001
Flat Panel display prototypeSamsung1999
Nobel Prize in Chemistry for the discovery of Buckyball
Robert F. Curl, Harry Kroto ,
Richard E. Smalley
1996
Synthesis of single wall carbon nanotubesS, Iijima and T, Ichihashi1993
Discovery of multi wall carbon nanotubes
Japanese Scientist, Sumio Iijima1991
Buckyball was synthesized and confirmed as C60
Scientists around the worldLate 1980s
Try to synthesize long carbon chainsHarry Kroto & Dave Walton1970s
EventsWhoWhen
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
Mechanical:Young Modulus ~ 1 TPa (SWNT) and 1.25 TPa (MWNT)
(Steel: 230 GPa)
High Aspect Ratio: 1000 – 10.000
Density: 1.3 – 1.4 g/cm3
Maximum Tensile Strength: 30 GPa
Thermal:Conductivity: 2000 W/mK (Copper has 400 W/mK)
Physical Properties
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
Special Properties
• Difference in chemical reactivity for end caps and side wall
• High axial mechanical strength• Special electrical properties:
– Metallic– Semi conducting
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
Methods of Fabrication
• Carbon Arc or Arc Discharge• Laser Ablation or Pulsed Laser Vaporization
(PLV)• Chemical Vapor Deposition (CVD)• High-pressure CO conversion (HiPCO)
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
Carbon Arc
• Carbon Atoms are evaporated by a plasma of Helium gas that is ignited by high currents passed through opposing carbon anode and cathode.
I
He
Arc-Discharge I
He
Arc-Discharge
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
• Excellent Method for the production of both MWNT and SWNT
• Carbon Nanotubes are obtained by controlling growth conditions– Pressure of gas in discharge chamber– Arcing Current
Carbon Arc
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
Pulsed Laser Vaporization
• Used for the production of SWNTs• Uses laser pulses to ablate (or evaporate) a carbon
target– Target contains 0.5 atomic percent nickel and/or
cobalt• The target is placed in a tube-furnace
– Flow tube is heated to ~1200°C
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
• A flow of inert gas is passed through the chamber to carry the nanotubes “downstream”– SWNTs condense from
the laser vaporization plume and are deposited on a collector outside the furnace zone
Pulsed Laser Vaporization
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
• MWNTs / SWNTs
• Yield <70%
• Catalyst / no catalyst
• Use of very strong laser
• Expensive (energy costs)
• Commonly applied
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
Chemical Vapor Deposition• Involves heating a catalyst material to high
temperatures in a tube furnace and flowing hydrocarbon gas through the tube reactor
• The materials are grown over the catalyst and are collected when the system is cooled to room temperature
• Key parameters are:– Hydrocarbons– Catalysts– Growth Temperature
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
Chemical Vapor Deposition- CVD process involves the dissociation of
hydrocarbon molecules catalyzed by the transition metal, and the dissolution and saturation of carbon atoms in the metal nanoparticle
- Both MWNT and SWNT can be grown byCVD methods
- MWNTs use acetylene gas for the carbon source and a growth temperature between 600 – 800°C
- SWNTs use carbon monoxide or methane for a carbon source and a much higher growth temperature (900 – 1200°C)
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
Steps of CVD
• Deposit photoresist• Expose resist• Deposit catalyst• Etch resist• CVD growth of Carbon
Nanotube on catalyst
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
Synthesis: growth mechanism
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
• Gas phase deposition
• Large scale possible
• Relatively cheap
• SWNTs / MWNTs
• Aligned nanotubes
• Patterned substrates
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
High-pressure CO conversion (HiPCO)
• New method of growing SWNT• Primary carbon source is carbon monoxide• Catalytic particles are generated in-situ
– Thermal decomposition of iron pentacarbonyl in a reactor heated to 800 - 1200°C
• Process is done at a high pressure to speed up the growth (~10 atm)
• Promising method for bulk production of SWNTs
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
Fabrication HiPCO
2CO• Single wall nanotube in gas phase (1200oC, 10 atm)• CO+CO C+ catalyst: (25 mTorr)• Flow high pressure carbon monoxide past catalyst particles at high temperatures• Can now produce largely single-walled nanotubes in kilogram quantities• Purification steps are unnecessary due to use CO instead of hydrocarbons
5FeCO
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
Synthesized SWNTs
• A metal catalyst needs to be present to produce a SWNT– Catalysts include
cobalt, iron or nickel• SWNTs are usually
assembled in ropes but some single tubes can also be found
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
Purification• Contaminants:
– Catalyst particles– Carbon clusters– Smaller fullerenes: C60 / C70
• Impossibilities:– Completely retain nanotube structure– Single-step purification
• Only possible on very small scale:– Isolation of either semi-conducting SWNTs
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
Purification techniques• Removal of catalyst:
– Acidic treatment (+ sonication)– Thermal oxidation– Magnetic separation (Fe)
• Removal of small fullerenes– Micro filtration– Extraction with CS2
• Removal of other carbonaceous impurities– Thermal oxidation– Selective functionalisation of nanotubes– Annealing
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
Cees Dekker, Delft University
Nanotube transistor
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
IBM
Wind et. al, Appl. Phys. Lett., May 20, 2002http://www.research.ibm.com/resources/news/20020520_nanotubes.shtml
• Logic gates, oscillators, … using many nanotubeson a single wafer has been demonstrated.
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
Nanotube transistor
• Field Effect transistor– Similar to MOSFET– Formation of p-type– Annealing or doping with
K to form n-type– Use both n and p to
make CMOS typecircuits
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
Directed Growth of SWNTs
• SWNT can be grown as suspended networks
• Grown from silicon pillars that have been patterned with a catalyst material
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
< Energy storage:
• Li-intercalation
• Hydrogen storage
> FED devices:
• Displays
< AFM Tip
> Molecular electronics
• Transistor
< Others
• Composites
• Biomedical
• Catalyst support
• Conductive materials
• ???
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
Super CapacitorElectrochemical double layer
Electrode (+) Electrode (-)
Separator
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
Field Emitting Devices
Single Emitter
Film Emitter
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
Patterned Film Field Emitters
• Etching and lithography• Conventional CVD• Soft lithography
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
Field Emission Display Device• Take advantage of the properties
of high current containing and high aspect ratio
• Useful as the electron source for Flat Panel Display with lower power consuming and high voltage circuit is unneeded
• Samsung has shown the prototype of 9” full color display with 576 X 242 pixels
• The first nanotube flat screen TV is expected to be manufactured by the end of 2003
The Samsung 4.5” full-color nanotube display
Schematic structure of nanotube flat panel display.(Choi et al.)
(Cathode)
(Anode)
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
Upon deformation
sp2 to sp3
Stretching of bonds
Opens bandgap in most nanotubes[Phys. Rev. B, vol. 60 (1999)]
Electromechanical Switch?
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
Resonator, Nanobalance• Deflection of MWNT ∝ Vs
2
• If Vs is alternating: resonance occurs (same as elastic theory of beams)
• Nanobalance: can measure picogram – femtogram masses.– Picture shows v = 968 KHz,
m = 22±6 fg
Poncharal et al., Science (1999)
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
Nanotweezers
• Separation between tweezer arms depends on applied potential
• Measure electrical properties of nanoparticles (SiC), nanowires (GaAs)
Kim and Lieber, Science (1999)
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
Atomic Force Microscopy
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
Atomic Force Microscopy
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
Chemical Sensor• Advantages
– High adsorption surface area
– Changing electrical properties at room temp.
– Detect very small concentrations (ppm) of O2, NO2, NH3
• Semiconducting nanotube • Depletion or accumulation of
carriers depending on species
Change of electrical resistance of SWNT with exposure to O2
V-I curves for NH3 and NO2exposure
Collins et al., Science (2000); Kong et al., Science (2000)
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
Conclusions
• Mass production is nowadays too expensive• Many different techniques can be applied for
investigation• Large scale purification is possible• FEDs and CNTFETs have proven to work• Positioning of molecular electronics is difficult• Energy storage is still doubtful, fundamental
investigations are needed
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Zentrum für Mikro- und Nanotechnologien
Technische Universität Ilmenau, FG Nanotechnologie
ReferencesDresselhaus, et al. “Carbon Nanotubes: Synthesis, Structure, Properties and Applications, 2001
K. Tanaka, et al. “The Science and Technology of Carbon Nanotubes,” 1999
H. Dai, et al. “Single-Wall Nanotubes Produced by Metal-Catalyzed Disproportionation of Carbon Monoxide,” Chemical Physical Letters 260 1996
N.R. Franklin, et al. “An enhanced CVD approach to extensive nanotube networks with directionality,” Advanced Materials, vol.12, June 2000
C. Journet, et al. “Large Scale Production of Single-wall Carbon Nanotubes by the Electric Arc Technique,” Nature 388 (1997).
P. Nikolaev, et al. "Gas-phase Catalytic Growth of Single-Walled Carbon Nanotubes from Carbon Monoxide,“Chemical Physics Letters 313 (1999).
C.D. Scott, et al. “Growth Mechanisms for Single-Wall Carbon Nanotubes in a Laser-Ablation Process” Applied Physics A 72 2001
The Nanotube Site: http://www.pa.msu.edu/cmp/csc/nanotube.htm
Institute of Theoretical Physics: http://www.itp.ucsb.edu