Nylon/Halloysite Nanotube Composites

Dr. Cathy Fleischer, President and CTO

Prof. Emmanuel Giannelis, Cornell University
Dr. Aaron Wagner, R&D Director

15 Schoen Place
Pittsford, NY 14534
Phone: 585-267-4850
Fax: 585-267-4855

NaturalNano, Inc.
Company founded December
2004
Initial focus on halloysite
nanotube applications in many
markets
Current focus on
commercialization of
nanocomposite products
Longer term focus on filled
tubes
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Halloysite Nanotubes (HNT)

Platy Clays
Exfoliation required
Complex chemistry
Non-standard equipment
Dispersion challenges

Halloysite Nanotubes

Ease of processing:
No exfoliation
Standard processing equipment

Improved Dispersion
Effective coupling to
polymer
Compatible with more
polymer systems
5

Applications
Platy Clays
Reinforcement (plastics)
Barrier (packaging films)
Dyeable (fibers)

Halloysite Nanotubes (HNTs)

Reinforcement (plastics)
Emerging
Controlled release:
Antimicrobial
Fragrances
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HNT Nanocomposites
Conventional Filler

Nanoclay

HNTs

Features:

Features:

Features:

High strength

High strength

High strength

Brittle

Not brittle

Not brittle

High weight

Lower weight

Lower weight

Process:

Process:

Process:

Standard equipment

Non-standard equipment

Standard equipment

Specialized chemistry

Lower process costs

Limited compatibility

Broad compatibility
7

Extrusion Comparison
Cornell Laboratory Extruder

Manufacturing Scale
Extruder

DSM twin screw

Microcompounder 5g
capacity

Werner Pfleiderer

100 rpm Co-rotating, under

flowing N2

400 rpm - Co-rotating

250C operation, single

controller

250C operation, multiple

zone controlled

29mm, 44:1 10kg/hr.

Testing and Analytical

Techniques
Tensile testing
Dynamic Mechanical Analysis (DMA)
Environmental Scanning Electron Microscopy
(ESEM)
FEI Quanta 200 with a Field Emission Gun
Operating at 25 KeV, working distance of 10mm
Low Vacuum
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Lab Scale Validation

Nylon/5% HNT
1.8

1.6
1.4
1.2

Values relative
to neat nylon

1
0.8
0.6
0.4
NaturalNano process
0.2
Platy clay
0
HNT as received

Modulus
Tensile Strength
Elongation

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Pilot Scale Trial Nylon/HNT

Dynamic Mechanical Analysis

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Pilot Scale Trial Nylon/HNT

Dynamic Mechanical Analysis

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Nylon/20% HNT
BSE ESEM Fracture Image

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Nylon/30% HNT
BSE ESEM Images

Surface

Fracture
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Nylon Nanocomposite Summary

Mechanical property enhancement obtained in the

lab are reproduced at pilot scale.
DMA results indicate that mechanical property
improvements are enhanced at elevated
temperatures.
Excellent dispersion is observed up to 30% HNT
levels.

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Polypropylene/5% HNT
Lab Scale

Increase in decomposition temperature

PP/PP-g-maleic anhydride (14/1) /5% HNT
composites
Decomposition temperature increased from
370C to 420C (temperature at 1.5% weight
loss)

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Polypropylene Pilot scale

Elastic Modulus

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Polypropylene Pilot Scale

Tensile Strength and Elongation

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Polypropylene/13% HNT
BSE ESEM Fracture Image

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Polypropylene Nanocomposite
Summary

Strength and modulus improvements are observed

without sacrificing elongation.
2X improvement in elastic modulus is obtained at
levels of 8-10% HNTs.
Good dispersion is observed up to levels of 10
-13% HNTs.

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Conclusions and Path Forward

Nylon and polypropylene HNT nanocomposites
have enhanced mechanical properties, without
sacrificing elongation.
Highly concentrated nanocomposite additives were
made which exhibit excellent dispersion.
Lab scale demonstrations were validated at the
pilot scale.
Future experiments will be conducted to drive to
higher concentration and greater property
enhancement.
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