Cnt Polymer

7/27/2019 Cnt Polymer

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Characterization of Carbon Nanotube

Polymer Composites

Characterization of Carbon Nanotube

Polymer Composites

Peter T. Lil lehei1, Jae-Woo Kim2, Cheol Park3,Kristopher E. Wise3, Emilie J. Siochi1, and

Joycelyn S. Harrison1

1Advanced Materials and Processing Branch

NASA Langley Research Center,

2Science Technology Co.,3National Institute of Aerospace

Peter T. Lillehei1, Jae-Woo Kim2, Cheol Park3,Kristopher E. Wise3, Emilie J. Siochi1, and

Joycelyn S. Harrison1

1Advanced Materials and Processing Branch

NASA Langley Research Center,

2Science Technology Co.,3National Institute of Aerospace


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AcknowledgementsAcknowledgements

NIA: C. Park, Z. Ounaies, K. E. Wise, J. Rouse

STC: J-W. Kim

Lockheed Martin: R. E. CrooksOak Ridge National Lab: N. Evans, E. Kenik, J. Bentley

NASA Langley Research Center: D. Working, C.

Topping, K. Pawlowski, S. E. Lowther, M.W. Smith,

J.S. Harrison, T.L. St.Clair

Georgia Institute of Technology: L.A. Bottomley, M.A.

Poggi

NIA: C. Park, Z. Ounaies, K. E. Wise, J. Rouse

STC: J-W. Kim

Lockheed Martin: R. E. CrooksOak Ridge National Lab: N. Evans, E. Kenik, J. Bentley

NASA Langley Research Center: D. Working, C.

Topping, K. Pawlowski, S. E. Lowther, M.W. Smith,

J.S. Harrison, T.L. St.Clair

Georgia Insti tute of Technology: L.A. Bottomley, M.A.

Poggi


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Earth, Moon, Mars & BeyondEarth, Moon, Mars & Beyond

Safe, sustained, affordable human and robotic

exploration of the Earth, Moon, Mars, and beyond

for less than one percent of the federal budget

Safe, sustained, affordable human and robotic

exploration of the Earth, Moon, Mars, and beyond

for less than one percent of the federal budget


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Long Term GoalsLong Term Goals

Create a virtual presence throughout our solar system andprobe deeper into the mysteries of the universe and life on

Earth and beyond

Conduct human and robotic missions to planets and other

bodies in our solar system to enable human expansion

Provide safe and affordable space access, orbital transfer and

interplanetary transportation capabili ties to enable research,

human exploration and commercial development of space

Develop cutting edge aeronautics and space systems

technologies to support highway in the sky, smart aircraft and

revolutionary space vehicles

Create a virtual presence throughout our solar system andprobe deeper into the mysteries of the universe and life on

Earth and beyond

Conduct human and robotic missions to planets and other

bodies in our solar system to enable human expansion

Provide safe and affordable space access, orbital transfer and

interplanetary transportation capabili ties to enable research,

human exploration and commercial development of space

Develop cutting edge aeronautics and space systems

technologies to support highway in the sky, smart aircraft and

revolutionary space vehicles


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Critical Technologies Required to

Achieve Goals

Critical Technologies Required to

Achieve Goals

Vehicle primary and secondary structures

Radiation protection Propulsion and power systems

Fuel storage Electronics and devices

Sensors and science instruments

Others

Vehicle primary and secondary structures

Radiation protection Propulsion and power systems

Fuel storage

Electronics and devices

Sensors and science instruments

Others


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Why Nano?Why Nano?

There is a need for new materials tomeet the challenging requirements ofnext-generation aircraft and spacecraft,

such as the hypersonic space planeand RLVs. Materials that have beenengineered from the "bottom up" offerexciting new possibilities for these

applications.

Within 5-10 years mature self-assembled, multifunctional

nanostructured materials from TRL 2 to5 for fabrication of spacecraft enablingNASA to safely and affordably explorethe Earth, Moon, Mars and beyond inthe second and third decades of this

century.

There is a need for new materials tomeet the challenging requirements ofnext-generation aircraft and spacecraft,

such as the hypersonic space planeand RLVs. Materials that have beenengineered from the "bottom up" offerexciting new possibilities for theseapplications.

Within 5-10 years mature self-assembled, mult ifunctional

nanostructured materials from TRL 2 to5 for fabrication of spacecraft enablingNASA to safely and affordably explorethe Earth, Moon, Mars and beyond inthe second and third decades of this

century.


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Requirements for NanomaterialsRequirements for Nanomaterials

Lightweight

Actuation

Radiation Protection

Electrical Conductivity

Thermal Conductivity

Sensing, health monitoring

Self healing Energy generation

Energy storage

Lightweight

Actuation

Radiation Protection

Electrical Conductivity

Thermal Conductivity

Sensing, health monitoring

Self healing Energy generation

Energy storage


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What Materials Will Get Us

There?

What Materials Will Get Us

There?

Carbon nanotubes towards multifunctionalstructures

Boron nitride nanotubes for hightemperature multifunctional structures

Nanoporous materials for thermoelectriccooling

Solid electrolytes to enable self-repair,

energy generation and storage

Amorphous metals

Carbon nanotubes towards multifunctionalstructures

Boron nitride nanotubes for hightemperature multifunctional structures

Nanoporous materials for thermoelectriccooling

Solid electrolytes to enable self-repair,

energy generation and storage

Amorphous metals


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Challenges of Carbon NanotubesChallenges of Carbon Nanotubes

Translating excellent combination of CNTproperties on the nanoscale to structural,

multifunctional properties on themacroscale

Dispersion of carbon nanotubes

Characterization of carbon nanotubenanocomposites

Inconsistent quality of carbon nanotubesupply

Scaling down processing equipment towork around low CNT supply

Translating excellent combination of CNTproperties on the nanoscale to structural,

multifunctional properties on themacroscale

Dispersion of carbon nanotubes

Characterization of carbon nanotubenanocomposites

Inconsistent quality of carbon nanotubesupply

Scaling down processing equipment towork around low CNT supply


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Nanocomposite CharacterizationNanocomposite Characterization

Develop through the use of optical,electron and probe microscopies:

techniques, methodologies and tools tocharacterize nanostructured composite

materials.

Determine the factors that contribute to, orinhibit, the translation of the nano-physical

properties to macroscale composites. Aid in the synthesis and design of the next

generation of nanocomposites.

Develop through the use of optical,electron and probe microscopies:

techniques, methodologies and tools tocharacterize nanostructured composite

materials.

Determine the factors that contribute to, orinhibit, the translation of the nano-physical

properties to macroscale composites. Aid in the synthesis and design of the next

generation of nanocomposites.


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Computationally Guided Materials DevelopmentComputationally Guided Materials Development

ON N

O

O

(O

O

O O )CN

CNT

Extruded CNT Nanocomposite

Injection Molded CNT NanocompTensile Test Specimen

Design

Processing

Characterization

Modeling


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The ProblemThe Problem

Kinetically

stable, weeks

Kinetically

stable, weeks

Thermodynamically

stable, years

Thermodynamically

stable, years

0.02%SWNT-CP20.02%SWNT-CP2 0.02%SWNT-(-CN)A/O0.02%SWNT-(-CN)A/O

Both samples are indistinguishable by

conventional optical characterization techniques

Both samples are indistinguishable by

conventional optical characterization techniques

Composite preparation


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p p p

Optical microscopy

Is the dispersion

acceptable?

Is the lack of dispersion due to:

1. Nanotube quality

2. Fabrication process

3. Polymer composition

No

Correct issue(s) causing poor dispersion

Yes

Determine reason for lack of dispersion.

Use microscopy, spectroscopy, and other

necessary test methods.

No or Unknown

Is the reason for lack

of dispersion now

known?

Is additional microscopy

needed to determine reason

for lack of dispersion?

Yes

No

No

Electron and probe microscopy

on surface and cross-section

Yes, optically dispersed

Does the application

require a further

assessment of the

dispersion?

Yes

Process improvement / optimization

No

YesAssess the bundle size, presence of

agglomerates, and local concentration

gradients to fully characterize the

dispersion

Is the level of

dispersion

sufficient for the

application?

Yes

Design experiments to determine reason for

lack of dispersion

No


14/41

Optical MicroscopyOptical Microscopy

OM images assessing the

dispersion quality of SWNT in

polymer composites. (a) Direct

mixing of 1 % SWNT/CP2, (b) in-

situ polymerization of 1 %

SWNT/CP2 with sonication, (c)

poor dispersion quality from 0.5

% SWNT/-CN, and (d) gooddispersion quality from 0.5 %

SWNT/ -CN. (a) and (b): aredifferent fabrication methods;results in different dispersion

quality. (c) and (d): same

procedure but different dispersion

results (different CNT quality).Samples with no visible

aggregates are labeled as

optically dispersed.

OM images assessing thedispersion quality of SWNT in

polymer composites. (a) Direct

mixing of 1 % SWNT/CP2, (b) in-

situ polymerization of 1 %

SWNT/CP2 with sonication, (c)

poor dispersion quality from 0.5

% SWNT/-CN, and (d) gooddispersion quality from 0.5 %

SWNT/ -CN. (a) and (b): aredifferent fabrication methods;

results in different dispersion

quality. (c) and (d): same

procedure but different dispersion

results (different CNT quality).Samples with no visible

aggregates are labeled as

optically dispersed .

(a) (b)

(d)(c)

(a) (b)


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Electron MicroscopyElectron Microscopy

HR-FESEM images on the dispersionquality of samples 1-4. (a) Surface

and (b) cross-section of sample 1

showing poor dispersion quality.

Optical microscopy already showed

this sample had a poor dispersion;

shown here for comparison. (c)

Surface and (d) cross-section of

sample 2 showing improved

dispersion over the direct mixingtechnique. (e) Surface and (f) cross-

section of sample 3 showing an

improved dispersion from using the

-CN polymer. Dispersion is still notideal due to poor quality of SWNT. (g)

Surface and (h) cross-section of

sample 4 showing nearly 100%

dispersion, no visible aggregates,

very small bundles, no resin r ich

areas, etc.

HR-FESEM images on the dispersionquality of samples 1-4. (a) Surface

and (b) cross-section of sample 1

showing poor dispersion quality.

Optical microscopy already showed

this sample had a poor dispersion;

shown here for comparison. (c)

Surface and (d) cross-section of

sample 2 showing improved

dispersion over the direct mixingtechnique. (e) Surface and (f) cross-

section of sample 3 showing an

improved dispersion from using the

-CN polymer. Dispersion is still notideal due to poor quality of SWNT. (g)Surface and (h) cross-section of

sample 4 showing nearly 100%

dispersion, no visible aggregates,

very small bundles, no resin richareas, etc.

(c) (d)

(h)(g)

(e) (f)

( ) ( )



16/41


QuickTime and aTIFF (LZW) decompressor

are needed to see this picture.

Film Surface


are needed to see this picture.

Film Surface

Direct mixing SWNT/CP2

Cross-section

In situ polymerization SWNT/(-CN)APB/ODPA

Cross-section

Siochi et al, Soc. Exp. Mech. (2003).


17/41


(a)The Field Emission Scanning ElectronMicroscope (FE-SEM) is capable ofimaging SWNT with the secondaryelectron detector (SE) (a) directly or (b)indirectly in composites. Indirect

imaging is done by using the electricfield arti fact to map the disturbance onthe beam induced electric field causedby the SWNT (dark contrast). With (c) in-situ mechanical testing, visualization of

crack propagation and other failuremechanisms are possible.

The Field Emission Scanning ElectronMicroscope (FE-SEM) is capable ofimaging SWNT with the secondaryelectron detector (SE) (a) directly or (b)indirectly in composites. Indirect

imaging is done by using the electricfield arti fact to map the disturbance onthe beam induced electric field causedby the SWNT (dark contrast). With (c) in-situ mechanical testing, visualization of

crack propagation and other failuremechanisms are possible.

(b) (c)


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FE-SEM: (a) SE image of purif ied SWNT, (b) STEM image of same locationas a) showing additional detail (c) STEM image of ropes and catalyst

particles (d) STEM image of an individual SWNT.

FE-SEM: (a) SE image of purified SWNT, (b) STEM image of same locationas a) showing additional detail (c) STEM image of ropes and catalyst

particles (d) STEM image of an individual SWNT.

(a) (b)

(d)(c)


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Electron Energy Loss Elemental Map: Nitrogen K edge

SWNT coated with polyimide: Adhesion and wetting Assessment

DE

-100

0

100

200300

400

500

600

0 10 20 30 40 50 60

Pixel

DE

Surface Plot of Nitrogen Map

Park et al.,Nanotechnology, 14 L11 (2003)Kenik et al, Proceeding of Microscopy and Microanalysis (2002)


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Probe MicroscopyProbe Microscopy(a) (b) (c)

Scanning Probe images on the dispersion quality of CNT in SWNT/polymer composites. (a)

topography, (b) current and (c) MFM image from 0.5 % SWNT/-CN. (d) topography, (e)current and (f) MFM image from 2 % SWNT/-CN.Scanning Probe images on the dispersion quality of CNT in SWNT/polymer composites. (a)

topography, (b) current and (c) MFM image from 0.5 % SWNT/-CN. (d) topography, (e)current and (f) MFM image from 2 % SWNT/-CN.

(d) (e) (f)


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Probe MicroscopyProbe Microscopy

Z Z

S SExperiment

Modeling

Modeling

1.92 pN

2.98 pN


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Microscopy SummaryMicroscopy Summary

Optical microscopy is sufficient to characterize dispersionon a >1 mm scale. Optically Dispersed

Scanning electron microscopy is able to map the electric

field in SWNT composites to asses dispersion from100s of mm down to 10s of nm.

(Scanning) Transmission electron microscopy can directlyvisualize single tubes, bundles and catalyst particles.

In-situ mechanical testing allows for visualization ofnanocomposite failure mechanisms.

Probe microscopy allows for the direct measurement of

interaction forces between SWNT and molecules orfunctional groups.

Optical microscopy is sufficient to characterize dispersionon a >1 mm scale. Optically Dispersed

Scanning electron microscopy is able to map the electric

field in SWNT composites to asses dispersion from100s of mm down to 10s of nm.

(Scanning) Transmission electron microscopy can directlyvisualize single tubes, bundles and catalyst particles.

In-situ mechanical testing allows for visualization ofnanocomposite failure mechanisms.

Probe microscopy allows for the direct measurement of

interaction forces between SWNT and molecules orfunctional groups.


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SpectroscopySpectroscopyRaman FTIR

Downshift

Upshift

Raman and FTIR Spectroscopy show that charge transfer isoccurring between the polymer and the SWNT, supported by

DFT calculations.

polymer= -5.1eV SWNT = -4.8 to -5.0eVWise, K. E.; Park, C.; Siochi , E. J.; Harrison, J. S. Donor-AcceptorStabil ization of Polymer-Carbon Nanotube Composites Chemical

Physics Letters, 391, 207, 2004.

Raman and FTIR Spectroscopy show that charge transfer isoccurring between the polymer and the SWNT, supported by

DFT calculations.

polymer= -5.1eV SWNT = -4.8 to -5.0eV

Wise, K. E.; Park, C.; Siochi, E. J.; Harrison, J. S. Donor-AcceptorStabil ization of Polymer-Carbon Nanotube Composites Chemical

Physics Letters, 391, 207, 2004.


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Polarized Raman SpectroscopyPolarized Raman Spectroscopy

4000

6000

8000

10000

12000

14000

16000

18000

20000

22000

24000

26000

28000

30000

32000

34000

36000

38000

Int

155015601570158015901600161016201630

Raman shift (cm-1)

0

90

0

90


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Percolation CharacterizationPercolation Characterization

Best Fit

LCH 2.684

LCL -16.22

t 3.102

s 0.3002

PHIc 0.0006

2-parameter phenomenological percolation equation, McLachlan et al,J. Phys. C20 865 (1987), PRB 56 1236 (1998)

(1)(i1/s

m1/s

)/(i1/s

+Am1/s

) + (c1/t

m1/t

)/(c1/t

+Am1/t

) = 0A = (1) /c

=10-6 (v-vc)1.5

REQUIREMENT

FOR ANTI-STATIC

Park et al., Chem. Phys. Lett., accepted


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Volume Fraction

0.000

0.005

0.010

0.015

0.020

0.025

0.000 0.200 0.400 0.600 0.800 1.000

0.7nm

2.1nm

3.5nm

-18

-16

-14

-12

-10

-8

-6

-4

0 0.05 0.1 0.15 0.2

Transverse

Log10

DC

(S/cm)

SWNT concentration (wt%)

r=0.7nm

r=2.1nm r=3.5nm

Higher orientation

Analytical Modeling of PercolationAnalytical Modeling of Percolation

Ounaies et al., Composites Sci. and Technol.ASAP (2003)

2-D Resistivity Contour Mapping2-D Resistivity Contour Mapping


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Aluminum 3.45 x 105 S/cm (STD: 2.8%)

y pp g

Front & Back Sides: Uniform Conductivity &

Dispersion

y pp g

Front & Back Sides: Uniform Conductivity &

Dispersion

5% SWNT/LF

Front side5% SWNT/LF

Back side

1.38 x 10-2 S/cm

STD: 2.9%1.42 x 10-2 S/cm

STD: 0.9%

5% SWNT

(-CN)PolyimideFront side

5% SWNT

(-CN)PolyimideBack side

5.74 x 10-2 S/cmSTD: 6.6%

5.90 x 10-2 S/cmSTD: 4.9%

Effects of volume fractions of the SWNTs inEffects of volume fractions of the SWNTs in


28/41

10-3

10-2

10-1

100

101

102

103

104

105

106

107

108

10-1710

-1610

-1510

-1410

-1310

-1210

-1110

-1010

-910

-810-710

-610

-510

-410

-310-2

HiPCo+bCN, various volume fractions

'(cm)

-1

Frequency(Hz)

0.000% HiPCo+bCN (PC455-32-10)

0.020% HiPCo+bCN (PC427-46-13)

0.035% HiPCo+bCN (PC427-71-09)

0.050% HiPCo+bCN (PC455-24-30)

0.075% HiPCo+bCN (PC455-44-09)

0.100% HiPCo+bCN (PC379-96)0.200% HiPCo+bCN (PC455-34-11)

0.500% HiPCo+bCN (PC427-49-13)1.000% HiPCo+bCN (PC427-48-13)

2.000% HiPCo+bCN (PC427-34-11)

5.000% HiPCo+bCN (PC427-31-10)

10.00% HiPCo+bCN (PC455-37-19)

20.00% HiPCo+bCN (PC455-51-18)

Below a critical volume C, the composite materials are insulating. Some wherebetween 0.035 and 0.05%, there is an abrupt change in the conductivity, apercolation transition.

matrixmatrix

Impedance Cole Cole Plot of SWNT PolyimideImpedance Cole Cole Plot of SWNT Polyimide


29/41

0

5 1010

1 1011

1.5 1011

2 1011

0 2 109

4 109

6 109

8 109

1 1010

Imagina

ryimpedance(Z")

Real impedance (Z')

Cole-Cole plot for (-CN)APB/ODPA

Imaginaryimpe

dance(Z")

Cole-Cole plot for 0.035% Hipco

Real impedance (Z')

Two Resonance Freq?

Impedance Cole-Cole Plot of SWNT-Polyimide

Nanocomposites

Impedance Cole-Cole Plot of SWNT-Polyimide

Nanocomposites

ec s o rea men s c reaF ti l ti )

ec s o rea men s c reaF ti l ti )


30/41

10-3

10-2

10-1

100

101

102

103

104

105

106

107

108

10-11

10-10

10-9

10-8

10-7

10-6

0.5% SWNT+CP2

'(cm)-1

Frequency (Hz)

0.5% SWNT(P2)+CP2 (PC455-98-05)0.5% SWNT(P3)+CP2 (LB430-71-P3)0.5% SWNT(P5)+CP2 (PC455-98-11)

The conductivity of a polymer with the same loading of SWNTs subjected to different acidtreatments (P2&3) and functionalization (P5), and therefore with different conductivities. Theshapes of the curves (presence of a flat region) indicate that all samples are conductors andtherefore above their percolation thresholds but the different SWNT properties lead to clearlydifferent conductivities.

Functionalzation)Functionalzation)


31/41

Small Angle Neutron Scattering: SWNT/PolymerSmall Angle Neutron Scattering: SWNT/Polymer

Q-1

QuickTime andaTIFF (LZW) decompressor

areneeded to seethis picture.


areneededto see thispicture.

Well-dispersed SWNTs in surfactant solutions behave like rigid rods, as reflected in the characteristicQ-1 power law in small angle neutron scattering spectrum.

H. Wang (Michigan Tech, NIST)

Effect of CNT Reinforcement on NanocompositeEffect of CNT Reinforcement on Nanocomposite


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Effect of CNT Reinforcement on Nanocomposite

Fiber Strength

Effect of CNT Reinforcement on Nanocomposite

Fiber Strength

UltemUltem & 1% SWCNTLaRC-8515LaRC- 8515 & 1% SWCNT

UltimateStrength

YieldStrength

0

50

100

150

200

MPa

Designed to adapt for differentDesigned to adapt for different


33/41

Designed to adapt for different

material needs

Designed to adapt for different

material needs

Wet spinning

Dry-jet spinning

Mini melt extrusion

Pultrusion

Calendering

Melt mixing

Brabender

Capillary rheometer Melt moldingDog bone

Fabrication of Building Blocks forFabrication of Building Blocks for


34/41

CNT

Extruded CNT Nanocomposite

Injection Molded CNT NanocompositeTensile Test Specimen Molded Matrix Resin

Molded CNTNanocomposite

Not conductive Highly Conductive

Melt extrusion/injection molding provides aroute to fabricating CNT nanocomposites withcomplex shapes. Demonstrated with in-house

processing capabilities.

Demonstratedconductivityenhancements onresin transfermoldednanocomposites.Work performed in

collaboration withM&P Technologies.

Coextruded Rods

SLMFSTTechnical Status POC: Emilie J . Siochi, LaRC, Emilie.J [email protected]

Coextrusion provides a route toproducing nanocompositeswith hierarchical morphologies.

Work performed incollaboration with AdvancedCeramics Research.

Resin

CNT Nanocomposite

HierachicalHierachical structurestructure Generate > 3km fiber/hr

Wet spun ribbon (Slit die)

Multifunctional Nanocomposites - BIOSANTMultifunctional Nanocomposites - BIOSANT

Dynamic Mechanical AnalysisDynamic Mechanical Analysis


35/41

Dynamic Mechanical Analysis

SWNT/CP2 Composite

Dynamic Mechanical Analysis

SWNT/CP2 Composite

CP-2

1.0vol% SWNT-CP2

0 50 100 150 200 250

Tan

(1Hz)

1.0% SWNT Inclusion

65% increase in stiffness

20% increase in hardness

Park et al., CPL, 364 (2002) 303-308

Mechanical properties ofMechanical properties of


36/41

Mechanical properties of

extruded fibers

Mechanical properties of

extruded fibers

SWCNT TensileModulus UltimateStrength YieldStress

(Wt%) (Gpa) (Mpa) (Mpa)

0.0 2.2 0.3 105 7 74 5

0.1 2.6 0.3 105 10 86 6

0.3 2.8 0.2 105 7 94 5

1.0 3.2 0.2 105 5 100 5

Reference: Submitted to Composites B: Engineering

SS


37/41

SummarySummary

Spectroscopic results suggest that amphoteric doping

of carbon nanotubes by two related polyimides.

Electrical conductivity increased by a 10 orders ofmagnitude at 0.1wt% SWNT loading.

Percolation of electrical conductivity was achieved

between 0.035 and 0.050 vol%.Percolation studies allow for a rapid assessment of the

dispersion without the need for laborious microscopy

procedures.Significant increases in stiffness (65%) and hardness

(20%) were achieved at 1% SWNT reinforcement.

Spectroscopic results suggest that amphoteric doping

of carbon nanotubes by two related polyimides.

Electrical conductivity increased by a 10 orders ofmagnitude at 0.1wt% SWNT loading.

Percolation of electrical conductivity was achieved

between 0.035 and 0.050 vol%.Percolation studies allow for a rapid assessment of the

dispersion without the need for laborious microscopy

procedures.

Significant increases in stiffness (65%) and hardness

(20%) were achieved at 1% SWNT reinforcement.

S IIS II


38/41

Summary IISummary II

Optical microscopy is a screening tool for probe and electronmicroscopy.

Both SEM and HR-SEM can visualize the CNT in a polymer

matrix and give details about the dispersion. TEM is able to visualize individual nanotubes and bundles in a

polymer matrix. Advanced techniques like EDS and EELSmapping provide additional information on nanotube polymer

interactions. Scanning probe microscopy gives complimentary data to

electron and optical microscopy. Force measurements madeby the scanning probe and give insights to polymer nanotubeinteractions.

Raman and FTIR spectroscopy give insights to polymernanotube interactions.

Physical and electronic properties of CNT polymer

composites are strongly influenced by the CNT dispersion andorientation.

Optical microscopy is a screening tool for probe and electronmicroscopy.

Both SEM and HR-SEM can visualize the CNT in a polymer

matrix and give details about the dispersion. TEM is able to visualize individual nanotubes and bundles in a

polymer matrix. Advanced techniques like EDS and EELSmapping provide additional information on nanotube polymer

interactions. Scanning probe microscopy gives complimentary data toelectron and optical microscopy. Force measurements madeby the scanning probe and give insights to polymer nanotubeinteractions.

Raman and FTIR spectroscopy give insights to polymernanotube interactions.

Physical and electronic properties of CNT polymercomposites are strongly influenced by the CNT dispersion andorientation.

Th k YTh k Y


39/41

Thank YouThank You

R f 2002 2003References 2002 2003


40/41

References 2002-2003References 2002-2003

Lil lehei et al., Nano Lett, 2, 827-829 (2002)

Park et al., Chem Phys Lett, 364, 303-308 (2002)

Park et al., Nanotechnology, 14, L1-L4 (2003)

Kumar et al., Macromolecues 35, 9039-9043 (2002)

Ounaies et al., Compos Sci Technol, 63, 1637-1646 (2003)Eklund et al., Nano Lett, 2, 561-566 (2002)

Odegard et al., Compos Sci Technol, 63, 1671-1687 (2003)

Rouse, Lillehei, Nano Lett, 3, 59-62 (2003)

Park et al., 5th BCC Conference Proc. (Oct 2002)

Park et al., Microscopy and Microanalysis Proc. (Aug 2002)

Park et al., ICCE/9 Proc. (2002)

Siochi et al., SEM Annual Conference Proc., MEMS/NEMS (2003)

Poggi et al., Proc. Electrochemical Soc., Fullerenes (2003)

Ounaies et al., IMECE Proc. (2003)NASA Tech Reports:

- 2002-211940 - 2002-211760 - 2002-212137

- 2003-12577 - 2003-4ismn-ejs

Lil lehei et al., Nano Lett, 2, 827-829 (2002)Park et al., Chem Phys Lett, 364, 303-308 (2002)

Park et al., Nanotechnology, 14, L1-L4 (2003)

Kumar et al., Macromolecues 35, 9039-9043 (2002)

Ounaies et al., Compos Sci Technol, 63, 1637-1646 (2003)Eklund et al., Nano Lett, 2, 561-566 (2002)

Odegard et al., Compos Sci Technol, 63, 1671-1687 (2003)

Rouse, Li llehei, Nano Lett, 3, 59-62 (2003)

Park et al., 5th BCC Conference Proc. (Oct 2002)

Park et al., Microscopy and Microanalysis Proc. (Aug 2002)

Park et al., ICCE/9 Proc. (2002)

Siochi et al., SEM Annual Conference Proc., MEMS/NEMS (2003)

Poggi et al., Proc. Electrochemical Soc., Fullerenes (2003)

Ounaies et al., IMECE Proc. (2003)NASA Tech Reports:

- 2002-211940 - 2002-211760 - 2002-212137

- 2003-12577 - 2003-4ismn-ejs

http://www.aerospace.nasa.gov/aero_blueprint/index.html

http://aero-space.nasa.gov/blueprint/library.htm

Optical & Electrical Properties: SWNT/CP2 CompositesUV/Vis (500 nm)
http://www.aerospace.nasa.gov/aero_blueprint/index.htmlhttp://aero-space.nasa.gov/blueprint/library.htmhttp://aero-space.nasa.gov/blueprint/library.htmhttp://www.aerospace.nasa.gov/aero_blueprint/index.html


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CP2 (no film)

85%

68%

100%

54%

62%

32%

UV/Vis (500 nm)

TransmissionScanned film

1 x 10-8

6.3 x 10-18

2 x 10-7

< 10-5

V (S/cm)

5 x 10-8

(1.0wt%) < 1% < 10-5Direct mixing

In situ

polymerization

under sonication

CP2: colorless polyimideV (S/cm): volume conductivityS: Siemens = ohm-1

Transmission: normalized at 34 m

0

0.1

0.2

0.3

0.4

0.5

0 10 20 30 40 50 60

y = 0.030728 + 0.0079404x R= 0.99275

Absorbance

Thickness (um)

Beers law

Cnt Polymer

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