1

Applied NanoStructured Solutions LLC

Dr. Tushar Shah – Chief Technology Officer

2011
2

Carbon Nanostructure (CNS) Infusion

2

What’s Different: CNS grown directly (infused) on surfaces 

... a continuous, in-line, production scalable process for glass, carbon ,ceramic , metals
3

CNS General Appearance

SEM Images – CNS Infused on Fiber Substrate

Filaments 

Covered with 

CNS after 

Growth Individual Fiber 

Filament with CNS 

Coating

CNS Radial and 

Longitudinal Coverage

~180μm 

tot. OD

Fiber 

Substrate
4

CNS Sizing Characterization 

SEM Images – Diameter Measurements
5

CNS Definition

Overall Structure Model

Branched Carbon 

Nano-Structures

Anchoring/Infusion 

into substrate

Entanglement 

and Branching

Zoomed in 

on next slide

Base 

Growth

Tip 

Growth

Intermediate 

Growth

Unreacted 

Catalyst
6

CNS Definition

Structure Model – High Resolution

Branched 

CNS

Anchoring/

Infusion 

into 

substrate

Base Growth

Tip 

Growth

Intermediate 

Growth

Individual Catalyst 

Particle Atoms

CNS Graphene 

Structure

Unreacted 

Catalyst
7

Fiber Substrate

Capping Layer 

(necessary for 

analysis Catalyst 

Presence Here 

 Tip Growth

Catalyst 

Presence Here 

 Intermediate

Growth

Catalyst 

Presence Here 

 Base Growth

Anchoring/Infusion 

into substrate

Entanglement and 

Branching

Growth 

Mechanism

CNS Structural Overview

High Resolution Cross-Section SEM Images
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CNS Branching and Anchorage 

High Resolution Cross-Section SEM Images

Branched Carbon Nano-Structures

CNS anchored to 

filament surface

Sample 

D01735

Glass Fiber Substrate
9

CNS Branching and Entanglement 

High Resolution TEM Images

CNS Walls 

(parallel 

lines)

Intermediate 

Catalyst 

Particle 

(Dark Spot)

CNS 

Agglomeration 

even after high 

energy 

sonication –

evidence of 

entanglement

CNS 

Branching

Sample 

163+6B+CNS
10

• CNS remained highly entangled 

after aggressive grid preparation 

(high energy sonication)

Sample B02382

TEM images confirm 

entanglement of CNS

Catalyst 

Particle 

(Dark 

Spots)

Lacey 

Carbon 

Grid 

Film

CNS Branching and Entanglement 

High Resolution TEM Images

Branching
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CNS Branching and Entanglement 

High Resolution TEM Images

CNS 

CNS Branching

Branching
12

Raman Spectrums

Thermogravimetric & Raman Analysis Of 

Infused CNSs

636.67°C

69.40%

677.39°C

36.18%

686.70°C

46.01%

675.06°C

37.31%

699.78°C

84.81%

0

5

10

15 Deriv. Weight (%/min)

0 200 400 600 800 1000 Temperature (°C)

021609_zyvex_7119_800C20r_2.002

021609_zyvex_7156_800C20r.001

021609_zyvex_8197_800C20r.001

021609_zyvex_Arkema_C-100_800C20.001

020409_S2_CNT_B83_800C20r.001

Universal V4.5A TA Instruments

Vendor 1

Vendor 2

Vendor 3

Vendor 4

ANS CNS

Commercially Available MWCNS’s

CNS Infused On Fiber Equal In Quality To Commercially Available CNS 

D-Band

ANS CNS G-Band

Vendor 2

Vendor 1

Vendor 3

Vendor 4

Thermogravimetric (TGA) Analysis 
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Carbon Enhanced Reinforcements (CER) 

Product Forms with Multifunctional Properties

Product Forms

CER Fiber Tow Prepregs

CER Post Coated Tow For Fabrics

CER Fabric Prepregs

CER Thermoplastic Pellets

“Tunable” Properties

Physical 

Density, thickness 

Mechanical

Toughness, isotropy 

Thermal

Control heat stability and 

conductivity

Electrical

Shielding, storing, directing, 

absorbing 

Durability

Corrosion, wear, fatigue resistance

Product Forms provided per Stewardship and Customer Requirements
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CNS Material Forms

CNS infusion demonstrated on multiple material forms for broad range of 

composite manufacturing processes and product applications: bodies 

of rotation, multi-material flat panels, complex geometries

– Fabrics

– Prepreg

– Wet layup

– VARTM

– Resin film infusion

– Tow/roving

– Wet filament winding

– Towpreg

– Unidirectional tapes

– Chopped

– Sheet, bulk and injection molding compounds

Demonstrating Standard Material Forms and Manufacturing Processes for 

Rapid Technology Transition
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Substrate Materials and Architectures

Process Can Be Tailored To A Variety of Substrates End Uses
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ANS – Pilot Scale Manufacturing 

Tows, 16” 40” moving to 60” Fabric Lines
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ANS – Product Development Center

Product Development Center for Prototype and Low Rate 

Manufacturing of Components
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Goal: No Respireable Durable Fiber

ANS Product Stewardship

• ANS / Government Progress to date:

• Air Monitoring 

• NIOSH Method 7400

• All tests to date have not yielded any respireable

durable fiber

• Next NIOSH Audit Activity begins 2/22/11

• A 3-part Pre-Manufacturing Notification (PMN) has been 

submitted to the EPA for review and approval

• 3 products designated by CNS length:

• Short: .01-15μ

• Medium: 15-50μ

• Long 50-100μ
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ANS Tunable Properties 

Material Characteristics
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CNS Infused To Glass Fiber Tow 

Infused Low and High Density CNS 

CNS Loading

1u

200 u
21 1.00E-12

1.00E-11

1.00E-10

1.00E-09

1.00E-08

1.00E-07

1.00E-06

1.00E-05

1.00E-04

1.00E-03

1.00E-02

1.00E-01

1.00E+00

1.00E+01

1.00E+02

1.00E+03

1.00E+04

1.00E+05

1.00E+06

1.00E+07

Log Scale Electrical Conductivity (1/Ω*m)

Material

Electrical Conductivity (Through Thickness) Comparison (Log Scale)

Electrical & Thermal Conductivity of 

Glass/Epoxy Composites

Conductive Composites

Improved Thermal Conductivity

Baseline Glass

CNS Glass Copper

1.81E-12

209.77

5.96E+07

0.19

0.51

2.99

0

0.5

1

1.5

2

2.5

3

3.5k[W/m*K]

CNS Infused S2 

Glass /Epoxy

Composite 

S2 Glass /Epoxy 

Composite

Neat resin
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-20

0

20

40

60

80

100

120

0 2 4 6 8 10 12 14 16 18 20

Shielding (dB)

Test Frequency (GHz)

Shielding Effectiveness

CNS Infused Gl/Ep Composites

0% (Baseline Gl/Ep)

1.67%

3.20%

4.37%

6.78%

Current CNS composite material 

capabilities for EMI shielding

EMI Shielding (2-18 GHz)

Increased Wt% CNS in Composite Improve EMI Shielding 

Characteristics
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EMI Shielding (100Mhz – 1GHz) 

Increased Wt% CNS in Composite Improves EMI Shielding 

Characteristics

0

10

20

30

40

50

60

70

80

90

100

110

120

100 1000 10000

Attenuation (dB)

Frequency (MHz)

EMI Shielding Effectiveness (dB)

Panel 218 - BL Glass

Panel 134 - CNS Glass/Epoxy

(4.37wt% CNS)

Panel 220 - CNS Glass/Epoxy

(6.57wt% CNT)

Panel 182 - CNS Carbon/Epoxy
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EMI Shielding

Bonding of CNS Composite Structures Not Critical

• Demonstrate EMI shielding for composite construction

– Evaluate effects of seams, gaps, gaskets

0

1 0

2 0

3 0

4 0

5 0

6 0

7 0

8 0

9 0

100

0 5 1 0 1 5 2 0

CNT Carbon Composite (dB)

Panel Cover With Gasket (dB)

Panel Cover, No Gasket (dB)

Test Frequency (GHz)

Attenuation (dB)
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Multifunctional Properties

Mechanical Strength

TRL-6; MRL-6 for CNS-infusion TRL-3/4 for composites

• Demonstrating mechanical performance through industry standard 

test methods

• Optimizing CNS processes to realize mechanical improvements 

in all properties and all material forms

• ANS Technical Data Sheets with design allowables will be 

published

(% Above/Below Baseline)

100%

110%

130%

Optimizing CNS Process Recipe and Composite Manufacturing Processes
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Composite Processes Development

CNS improve critical failure interfaces in composites
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Lightning Strike Test

TOP 

(Strike 

Surface)

BOTTOM 

Panel RFI 73 – CNS Glass/Epoxy

4 Plies Fabric, Surface Resistivity: 12 

ohms/sq

Panel RFI 472 – 1 Pliy Fabric

CNS Carbon/Epoxy on 3 base plies

30kA 200kA
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Lightning Test – High Current Test

Baseline Glass/Epoxy Panel Vs. CNS Glass/Epoxy Panel

BL Glass/Epoxy is Punctured and Delaminates,

CNS Panel Strike Surface has surface abrasion
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Future Needs

•Very Complex CNS produced at high speeds on various sustrates

•Need for high speed real-time analytical tools 

•Surface analysis techniques

• Determine variations in density

•Type of nanostructures 

•Functionalization
Thank You

Questions ?