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Organised by:
To register - Tel: +44 (0)20 7841 4811 UK: 0845 056 5069
Fax: +44 (0)20 7505 6001 Email: EPNconferences@emap.com
Online: www.nanosconference.com
Nanocomposites is
sponsored by:
Nanotubes
14-15 March 2006 Marriott Hotel, Brussels
16 March 2006 Marriott Hotel, Brussels
CARBON NANOTECHNOLOGIES ■
HYPERION CATALYSIS
NANOCYL
■
NASA
■ BAYERMATERIALSCIENCE
UNIVERSITY OF EDINBURGH ■ ROSSETER HOLDINGS
Nanocomposites
2006
Small technology means big business for plastics
The world’s first international conference on nanocomposites, now in its 6th year!
BASELL POLYOLEFINS ■ BYK-CHEMIE ■ CENTEXBEL
FORD MOTOR COMPANY ■ KABELWERK EUPEN ■ LANXESS
NANOCOR ■ POLYKEMI ■ SOUTHERN CLAY ■ UMICORE
Featuring expert speakers:
Featuring expert speakers:
Supported by:
To register - Tel: +44 (0)20 7841 4811 UK: 0845 056 5069 Fax: +44 (0)20 7505 6001 Email: EPNconferences@emap.com Online: www.nanosconference.com
Nanocomposites
2006
14-15 March 2006 - Marriott Hotel, Brussels
DAY ONE –TUESDAY 14 MARCH 2006
08:30 Registration
09:15 Chairman’s opening remarks
Chris Smith, Technology Editor
EUROPEAN PLASTICS NEWS & PLASTICS AND RUBBER WEEKLY
09:30 The challenges for delivering successful
application of nanocomposites
■ What are the challenges and what is needed from
research and development?
■ Examining cost consideration from the application point of view
■ Identifying commercial areas of applying nanotechnology
■ Understanding infrastructure for delivering
nanocomposite materials
Dr Joachim Grossman
Vice President Marketing and Sales Plastic Additives
SUD-CHEMIE AG
10.00 Nanoclays: Evolving products and applications
■ The CLOISITE® Nanoclay family
■ Getting the most out of the least amount of nanoclay
■ Evolving commercial applications based on synergies
with other functional additives
■ Co-development programs matching nanoclay with host polymer
Karl Kamena
Commercial Manager
SOUTHERN CLAY
10:30 Polymer-clay nanocomposites: commercial
success in polyamides
■ Nanoclay and nanocomposite technology overview
■ Polyamide nanocomposite via in situ polymerization
■ Imperm: a ultra high barrier resin based on nano-Nylon MXD6
■ Commercial application of polyamide based nanocomposites
Dr.Ying Liang
Technical Sales Manager - Polyamides
NANOCOR
11:00 Question and answer session
11:15 Morning refreshments
11.45 Advances in nano zinc oxide: Zano® as an additive to
plastics and plastic films for packaging, medical and
agricultural applications
■ From lab to industrial plant: supplying customers
with high performance solutions
■ Working with your customer to overcome challenges
of using new materials
■ Combining transparency with broad UV-A and UV-B protection
and the general anti-bacterial properties of zinc
Philip Eyckmans
Application Development Manager - Business Line Zinc Oxide
UMICORE
12.15 PANEL DISCUSSION
PACKAGING INDUSTRY PERSPECTIVE:
Innovative use of nanocomposites in packaging
■ Exploring the developments in single layer and multilayer film
where nanocomposites have an advantage over other polymers
■ Significantly reducing material costs through
using nanocomposites
■ Exploring what the industry still requires from
R&D in nanocomposites
12:45 Question and answer session
13.00 Lunch
UPDATE – LATEST RESEARCH
14.15
Development of new routes towards organoclay-based
nanocomposites
■ Examining techniques for selection of nanoclays
■ Overview of what nano clays really can do
■ Identifying the impact of processing methods on nanoclays
■ Assessing the ongoing areas of R&D in nanocomposites
and why new organoclay nanos are required to
meet requirements
■ Examples of research into further enhanced properties
14:45 Nanofiller-containing polyolefinic composites:
from production to applications
■ Assessing the choice of polymer to use with a particular clay
■ Examining the production, characterisation and properties
of organoclay-containing polyolefinic composites
■ Comparison with alternative carbon structure-containing
polyolefinic composites
■ Overview of applications – oautomotive, textiles and packaging
Guiseppe Ferrara
Project Leader
BASELL POLYOLEFINS
15.15 Question and answer session
15:30 Afternoon refreshments
UPDATE – LATEST RESEARCH
16.00 New results of flame retardant properties of nanocomposites
■ PVC and PE nanocomposites - fiction or technical reality?
■ Nanocomposites - unwanted side reactions
■ Highly effective nanostructured flame retardants
other than montmorillonite
Dr Günter Beyer
Manager of Chem-Phys Laboratory
KABELWERK EUPEN
To register - Tel: +44 (0)20 7841 4811 UK: 0845 056 5069 Fax: +44 (0)20 7505 6001 Email: EPNconferences@emap.com Online: www.nanosconference.com
16.30 Heat resistance and reaction to fire of polymer nanocomposites
■ Preparation of polymer nanocomposite: influence of processing
conditions and of the nanodispersion on heat and fire resistance,
including the use of organoclays and POSS in different polymeric
matrices (PS, EPDM, TPU and PP)
■ Modification of the nanofillers: preparation of organo-modified
LDH and of surface treated carbon nanotubes. Evaluating
nanofillers are modified in PP and in PS in terms of
flammability and heat stability
Prof Serge Bourbigot and Sophie Duquesne
ECOLE NATIONALE SUPERIEURE DE CHIMIE DE LILLE (ENSCL)
17.00 Question and answer session
17.15 Chairman’s closing remarks
17.30 End of day one and drinks reception
DAY TWO - 15 MARCH 2006
08.00 BREAKFAST BRIEFING
Exploring the potential for Europe to remain the
leading producer of niche high performance materials
■ Examining the future landscape for nanocomposites
on a global scale
■ Producing commercial quantities of nanocomposites
and delivery to market
■ Ensuring a successful route to market
Del Stark
EUROPEAN NANOTECHNOLOGY TRADE ALLIANCE
09.30 Chairman’s opening remarks
09.45 Outlining the real life-cycle of nanocomposites
and their future potential
■ Assessing the long-term thermal stability of the most
commonly applied nancomposite materials
■ Developments in scratch resistance properties
■ Discussing the performance of nancomposites in high heat
conditions and recent improvements
■ Material cost implications of the improvements in the
lifecycle of nanocomposites
Tim Harper
CEO
CIENTIFCA
10.15 A new method to control clay-polymer nanocomposite quality
■ A novel and simple infrared technique to assess degree
of clay dispersion
■ Tuning of processing parameters to achieve optimum results
■ Selection of nanoclay chemistry to match polymer matrix
Wouter L. Ijdo, Ph.D
R&D Manager
ELEMENTIS SPECIALTIES
10.45 Question and answer session
11:00 Morning refreshments
11.30 Exploring the business case of nano-fillers for
automotive applications
■ Identifying performance targets for nanocomposites
■ Cost-benefit analysis of nanocomposite performance
■ Commercial nanocomposites vs. conventional automotive materials
Dr Lebzy Gonzalez
Technical Expert
FORD MOTOR COMPANY
12.00 The role of nanoclay in developing single material
plastic fuel tanks
■ Analysing potential areas of commercialisation under-the-hood
and the cost advantages for the automotive industry
■ Reducing emissions with nanocomposites in
thermoformed fuel systems
■ Using nancomposites that are compatible with heat
resistance requirements of new fuels
Henrik Erikksson
Development Manager
POLYKEMI
12:30 Question and answer session
12:45 Lunch
14.15 Advances in the use of nanocomposites in the textile industry
■ Overview of the advances in nanocomposite developments
for the textile industry
■ Main problems and limitations to be overcome to make
nanocomposites suitable for textile extrusion
■ Overview of research work with nanoclay based nanocomposites
at industrially relevant conditions and equipment
■ Perspectives with carbon nanotubes and other nanoparticles
Dr Valja Everaert
Project Manager
CENTEXBEL
14.45 The use of nanosized functional materials
in paint and plastics applications
■ Examining progress in clear coatings
■ Advances in applications for barrier enhanced
coatings and adhesives, scratch resistant coatings
■ Developments in UV protection using inorganic materials
■ Other areas as a potential market for these coatings
Dr Thomas Sawitowski
Head of Nanotechnology Department
BYK-CHEMIE
15.15 Developments in applications for polyamide nanocomposites
■ Examining flame retardance for electronic application
■ Applications requiring films with barrier properties
■ Advances in nanocomposites for film and their
application in the packaging industry
■ Developments in nanocomposites for fuel lines
Marcus Schaefer
Product and Application Development
LANXESS
15.45 Question and answer session
16.00 Chairman’s closing remarks and end
of Nanocomposites conference
Nanotubes
Organised by:
© Emap PLC 2005. The
programme may change due
to unforeseen circumstances.
Emap reserves the right to alter
the venue and/or speakers.
16 March 2006 - Marriott Hotel, Brussels
DAY THREE - 16 MARCH 2006
08.30 Registration and refreshments
09.00 Chairman’s opening remarks
Chris Smith
Technology Editor
EUROPEAN PLASTICS NEWS AND PLASTICS & RUBBER WEEKLY
09.15 Carbon nanotubes: A review of their multi-functional
properties and current commercial applications
■ Introducing commercial carbon nanotubes and their
benefits in polymers
■ How to improve dispersion of carbon nanotubes
and maximize the added-value
■ Reviewing their current performances vs. other additives
■ Current status and perspectives of commercial applications
Olivier Decroly
Business Development Director
NANOCYL
09.45 Commercial applications of tubular fullerenes (‘buckytubes’)
■ Buckytube properties and benefits (conductivity, toughness,
dimensional stability, etc.)
■ Buckytube applications, including case studies
■ Conductive polymer compounds
■ Advanced composites
■ Coatings
David A. Karohl
Director of Business Development
CARBON NANOTECHNOLOGIES
10.15 Assessing the advantages of using high performance polymers
in applications requiring a tailored, specialist product
■ Measuring the benefits and weaknesses of nanotubes
and nanofibres over traditional polymer additives
■ Exploring future pricing structures and predicting when
costs will come down
■ Scaling-up production processes to accommodate
high performance materials
■ Case studies of innovative applications
Vladislav Ryzhkov
R&D Director
ROSSETER HOLDINGS
10.45 Question and answer session
11.00 Morning refreshments
11.30 The second wave of commercializing nanotubes:
new resins, new applications
■ Examining new developments in higher performance resins,
including thermally sensitive resins, thermosets and elastomers
Cost/performance benefit of using nanotubes in applications
Analysis of market penetration and future opportunities
Patrick Collins
Marketing Director
HYPERION CATALYSIS
12.00 Applications and properties of Baytubes®/polymer composites
■ NT/polymer composite
■ Compounding
■ Product development
Dr Michael Bierdel and Dr Reiner Rudolf
High Viscosity Technology
BAYERMATERIALSCIENCE
NEW RESEARCH
12.30 Essential update on health and safety issues
relating to nanotubes
■ Current scope of research into the health effects of nanotubes
■ Outlining the responsibilities of R&D departments
and mitigating risk
■ Ensuring low risk from exposure to nanotubes
throughoutthe product chain
■ Levels of risk to the consumer in specific applications
Ken Donaldson
Professor of Respiratory Toxicology
UNIVERSITY OF EDINBURGH
13.00 Question and answer session
13.15 Lunch
TUTORIAL - CARBON NANOTUBE BASED TECHNOLOGY
Dr Meyya Meyyappan
Director, Center for Nanotechnology
NASA AMES RESEARCH CENTER
14.30 Session I
Understanding the remarkable properties of nanotubes
■ CNT properties
■ Growth techniques particularly CVD and plasma CVD
■ Patterned growth
■ Vertical alignment
■ Challenges in controlling the diameter
■ Chirality
15.30 Afternoon refreshments
16.00 Session II
Examining scaleup issues for large scale production,
characterization; and a detailed discussion of revolutionary
applications, including:
■ Electronics devices
■ Computing and data storage technology
■ Sensors
■ Detectors
■ Field emission displays and devices
■ Nanoelectromechanical systems (nems) high strength composites
■ Aerospace systems
■ As tip in scanning probe microscopy(spm) for imaging
and nanolithography
17.00 Question and answer session
17.15 Chairman’s closing remarks and end of conference
Sponsorship and Exhibition
Opportunites
Nanocomposites 2006 and
Nanotubes is the leading
international forum for the industry.
Our tailored sponsorship packages
offer you a number of ways to
promote your business and raise
your profile in this competitive
market. To raise your profile,
please contact Levent Tounjer,
Commercial Manager on
Tel +44 (0)20 8277 5510
Fax +44 (0)20 8277 5103
Levent.tounjer@emap.com
Nanocomposites & Nanotubes
2006
Nanocomposites 2006
European Plastics News and PRW are pleased
to announce the programme for this year’s
conference on Nanocomposites.
With a programme that balances commercial aims
and marketing strategies with advances in research
and development, this is the only conference on
Nanocomposites that you cannot afford to miss!
Remarkable advances in technology that will
impact the future value of your business
The packaging and automotive industries are experiencing
the value-added benefits of these exciting commercialised
developments. Attend this conference to find out the future
opportunities in applications and the potential new markets.
You will hear about the latest commercial
benefits of using nanocomposites in specific
applications, including:
You will hear about developments in properties of nanocomposites,
get an update on the affordability of these high performance
materials and see the latest applications to benefit.
Hear presentations that examine the latest
developments in high performance materials,
including properties such as:
What’s new for 2006?
For the first time, this year’s Nanocomposites includes
an exclusive one-day event on Nanotubes.
Outstanding networking opportunities
Make sure you register for the extra networking opportunities that
we are offering this year. Places are limited – do book early for the
Pre-conference Wine Tasting on 13 March and the Breakfast
Briefing on 15 March.
Nanotubes
Nanotubes is a unique one day event that combines both
industry presentations and an in-depth tutorial. It will look
at real applications, developments in performance, cost
expectations and health and safety issues.
Dr Meyya Meyyappan, Director, Center for Nanotechnology,
NASA AMES RESEARCH CENTER will present an in-depth
tutorial on carbon nanotube based technology.
Understand how the combination of remarkable mechanical
properties and unique electronic properties of carbon nanotubes
(CNTs) offers significant potential for revolutionary applications
in electronics devices, computing and data storage technology,
sensors, detectors, field emission displays and devices,
nanoelectromechanical systems(NEMS), high strength composites,
aerospace systems, as tip in scanning probe microscopy(SPM)
for imaging and nanolithography, and a number of other areas.
The carbon nanotube synthesis, characterisation and applications
touch upon all disciplines of science and engineering. Learn how
you can incorporate them into your business strategy
Dr Meyyappan is a founding member of the Interagency
Working Group on Nanotechnology (IWGN) established
by the Office of Science and Technology Policy(OSTP).
The IWGN is responsible for putting together the National
Nanotechnology Initiative.
This massive three-day event will feature focused debates,
pre-conference networking sessions, a drinks reception and a
breakfast briefing to insure you meet new contacts and learn
about the latest innovations in this exciting arena.
Read what delegates said about Nancomposites 2005:
‘The best two-day nanocomposite
conference in the world’
HONEYWELL
‘A must for anyone working in nanocomposites’
SUD-CHEMIE
And about Nanotubes:
‘Good mix of academic and technical lectures’
BAYERMATERIALSCIENCE
‘Good conference with application-centred people’
SGL CARBON
■ Film
■ Coatings
■ Paint
■ Barrier
■ Toughness
■ Stiffness
■ Transparency
■ Flame Retardancy
■ Recyclability
■ Textiles
■ Electronics
Please quote the conference
code Y521 and delegate’s
name in your correspondence
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Cancellations made before 14 February 2006 will be charged at
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WAYS TO REGISTER
Nanocomposites & Nanotubes
2006
Nanocomposites 2006, 14-15 March 2006
Please register ____ delegate(s) at the rate of
€1199 + VAT @ 17.5% = €1408.83
Nanotubes, 16 March 2006
Please register ____ delegate(s) at the rate of
€699 + VAT @ 17.5% = €821.33
Nanocomposites and Nanotubes, 14-16 March 2006
Please register ____ delegate(s) at the rate of
€1699 + VAT @ 17.5% = �€1996.33
Breakfast Briefing
€99 + VAT @ 17.5% = €116.33
(Includes full breakfast)
GROUP BOOKING DISCOUNTS AVAILABLE
(on normal rate). For information about group discounts
please contact the conference team using the details
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14 - 16 March 2006
Marriott Brussels, Rue A. Orts 3-7, Grand Place, Brussels 1000, Belgium
Tel: +32 2 516 9090 Fax: +32 2 516 9000
16/03/06 Brussels V.A. Ryzhkov Assessing the advantages …2
Agenda
• Measuring the benefits and weaknesses of
nanotubes and nanofibres over traditional
polymer additives
• Exploring future pricing structures and
predicting when costs will come down
• Scaling-up production processes to
accommodate high performance materials
• Case studies of innovative applications
16/03/06 Brussels V.A. Ryzhkov Assessing the advantages …3
I. Measuring the benefits and weaknesses of
CNTs and CNFs over traditional polymer
additives (commercial ABS, PC, PPS, PTFE are considered)
• Typically, addition of 10-40wt% of Carbon Fibers increases
electric conductivity in 10-15 orders of magnitude, thermo-
conductivity in 2-4 times, and tensile strength in 2-3 times,
respectively. Carbon Spheres, Graphite, and Carbon Black
are typically less successive enhancers
• Typically, addition of 20 - 40 wt% of Glass Fibers increases
tensile strength in 2-3 times and thermo-conductivity in 1.5-2
times, respectively, meanwhile increasing dielectric
properties
• Metallic additives essentially increase specific weight
16/03/06 Brussels V.A. Ryzhkov Assessing the advantages …4
Percolation thresholds provided by carbon additives
1 10 100 1000 10000
0.1
1
10
5
2
50
20
arc-MWNTs, 7
9,SWNT2
4,CNFs
SWNT1, 8
sh-MW NTs, 6
10,SWNT3
5,CVD-MWNTs
3,Fibers
2,Carbon Black
1,Spheres
Loading, %
Length/diameter, a.u.
______________________________________________________
6, sh-MWNTs – ROSSETER’s naturally short arc carbon MWNTs
16/03/06 Brussels V.A. Ryzhkov Assessing the advantages …5
Optimal loadings of additives for improvement of
electro-conductivity of CF4-cathodes in LIB
• Ideally, the smallest 1μm-CF4-particles can be
covered (like a C60-structure) with 90 typical
sh-MWNTs (225nm in length, 2*10^6 at.C),
providing loadings for such ultra-thin powders of
~ 0.25wt%. Typical CF4-particles having
median sizes of 4-5μmcan be covered with
360 typical sh-MWNTs (like a C240-structure),
resulting in minimum loadings of ~ 0.01 wt%.
SWNTs can provide same levels (considering median bundle of 20
tubes), whereas conventional straight arc-MWNTs (median length 2-
5μm) are too long to cover such small particles effectively.
CVD-MWNTs and CNFs can provide loading levels of 0.05-1wt%,
which is comparable with what Carbon Black (L/d= 10:1, d ~100nm)
can provide. Carbon Fibers fail to do the job for such smal particles
16/03/06 Brussels V.A. Ryzhkov Assessing the advantages …6
Electric Behavior of PC composites
0 5 10 15 20
100
101
102
103
104
105
106
107
108
109
1010
1011
1012
1013
1014
Volume resistivity (Ω-cm)
Carbon additive (wt%)
Carbon Fibers
CVD-MWNTs
Carbon Black
16/03/06 Brussels V.A. Ryzhkov Assessing the advantages …7
Mechanical behavior of PC composites
0 5 10 15 20 25 30
1
10
100
Carbon Fibers
C.Black
CVD-MWNTs
T.S.(MPa), T.M.(GPa), Elong.(%)
Carbon additives (wt%)
T.Strength
Elongation
T.Modulus
16/03/06 Brussels V.A. Ryzhkov Assessing the advantages …8
Electric behavior of PTFE-composites
0 4 8 12 16 20 24
100
101
102
103
104
105
106
107
108
109
1010
1011
PTFE / Conductive Carbon
PTFE / Graphite
Volume Resistivity (Ω-cm)
Additive (wt%)
Ftoroplast-4 / sh-MWNT
16/03/06 Brussels V.A. Ryzhkov Assessing the advantages …9
Mechanical behavior of sh-MWNT-PVA composites
02468
100
120
140
160
180
Tensile Strength, Modulus (%)
Carbon Additive (wt%)
Strength
Modulus
16/03/06 Brussels V.A. Ryzhkov Assessing the advantages …10
Summary of advantages & disadvantages:
• CNTs and CNFs provide enhanced composites’
electro-conductivity at much lower loadings (1-4wt%)
than conventional additives do
• SWNTs, arc-MWNTs and thin CVD-MWNTs
essentially improve mechanic characteristics even at
loadings of 1-5 wt%, whereas thicker CVD-MWNTs
and GNFs seem behaving like Carbon Fibers,
perhaps, requiring higher concentrations which are
difficult to achieve because of the dispersion problems
for long CNTs and CNFs. Sh-MWNTs are easily
dispersed and incorporated into any polymer matrices
• The main disadvantage of CNTs and CNFs over CFs
are high prices
16/03/06 Brussels V.A. Ryzhkov Assessing the advantages …11
II. Exploring future pricing structures and
predicting when costs will come down
• Nanotube prices are considered as being the main
hurdle towards their industrial applications, especially
in polymer composites
• Unfortunately, there is no sign for a dramatic drop of
nanotube prices towards the industrial target of ~ $100
per kg.
• Typically, recent nanotube prices are ~ $60-200 per
gram of 50-70% SWNTs and ~ $1-15 per gram of raw
arc MWNTs and/or 90-95% CVD-MWNTs
16/03/06 Brussels V.A. Ryzhkov Assessing the advantages …12
Recent pricing for 50-80% SWNTs
1999 2000 2001 2002 2003 2004 2005 2006
0
100
200
300
400
500
60%
45%
80%
65%
70%
80%
60%
Price ($/gram)
Carbolex
Nanocyl
CNI
NanCarbLab
NanoCarbLab
NanoCraft
NSAM
16/03/06 Brussels V.A. Ryzhkov Assessing the advantages …13
Recent MWNT pricing: the closest target is $1/g
2001 2002 2003 2004 2005 2006 2007
0
4
8
12
16
20
24 Colour lines - CVD-MWNT, C=90-95wt%
Black lines - 40-60wt% arc-MWNTs, C>99wt%
Price ($/g)
RHL, arc
MER, arc
NSAMthin
NSAMthick
NSAM, CNF
SunNano
MER, CVD
NSyl, industr
16/03/06 Brussels V.A. Ryzhkov Assessing the advantages …14
What are the hurdles? Are they temporary or for ever?
• Any CNT/CNF production needs catalysts and their removal before a
CNT/CNF application. Thinner CVD-CNTs and CNFs require more
expensive catalysts, suffering from defects upon purification in much
higher extent than the thicker ones. Typically, post-purification
annealing is required to improve the CVD-CNTs’/CNFs’ quality and at
least 3-5wt% of catalysts is inevitably left inside the CVD-CNTs and
CNFs after the purification and annealing
• For most applications highly defective external layers of the CVD-
CNTs / CNFs can be considered as useless admixture of disordered
graphite and/or amorphous carbon, highly reducing useful parts of
CNT / CNF contents and making them comparable with typical
contents of perfect arc MWNTs in raw cathode deposits (40-60wt%)
• Typically, raw cathode deposits of arc MWNTs contain less than 0.1-
0.2 wt% of metallic admixtures (“natural” admixtures of Fe work as an
effective catalyst), eliminating the purification needs / problems
16/03/06 Brussels V.A. Ryzhkov Assessing the advantages …15
Conventional Gas-phase Carbon Arcs suffers from:
• A rather high price of High Purity (99.99%) Graphite (HPG) for
anodes (~ $100 per kg) deteriorated by a very low conversion
(~25%) of the anode graphite to a nanotube core deposit,
resulting in a fraction of HPG price as much as $400 per kg
• Small cross sections of the anodes resulting in low nanotube
yields of 2-5g/h per anode and production costs of conventional
arc-MWNTs as high as $1,000-2,000 per kg
• CNTs with median lengths of 200- 500 nm are considered as
non-toxic and easily dispersed, whereas conventional arc
CNTs and CVD-CNTs have lengths of 2- 10 μmwhich
complicates their uniform dispersion in most solvents /
polymers and raises questions regarding their toxicity
• Cutting long nanotubes in such short pieces causes additional
costs and defects
16/03/06 Brussels V.A. Ryzhkov Assessing the advantages …16
ROSSETER produces Naturally Short Carbon Multi Wall
Nanotubes (sh-MWNTs) using proprietary
Self-regulated Liquid-phase Arc-discharge (SLA) process
• Anodes are made of a cheap technical grade graphite (≥99%) costing
few $ per kg and containing optimal levels of “natural” admixture of
Fe of 0.03-0.1wt%, whereas typical content of Fe in HPG is 0.005-
0.01wt%
• Combination of Liquid-phase (lowering temperature) with higher
contents of the catalyst results in shorter MWNTs and highly
increased nanotube yields, so far, up to 100-150 g/h per anode in
contrast with GCA’s yields of ~ 2-5 g/h per anode
• Anodes’ cross sections and conversions are increased up to 5-6cm2
(~ 0.5cm2 in GCAs) and ~ 100% (~25% in GCAs), respectively, due
to effective cooling and a feedback from hydrocarbon liquids. Optimal
gaps between anodes and cathodes are self-regulated due to correct
feedbacks from hydrocarbon liquids
• As a result, the projective production cost is $100-200 per kg of raw
sh-MWNT deposits upon producing tons
16/03/06 Brussels V.A. Ryzhkov Assessing the advantages …17
III. Scaling-up production processes to
accommodate high performance materials
16/03/06 Brussels V.A. Ryzhkov Assessing the advantages …18
Necessary requirements before scaling up:
• Ability to produce in bulk cheap and high-quality
nanotubes with controllable / reproducible parameters
• Demand for such nanotubes, i.e. a successful
combination of availability of promising applications
and “good will” of potential producers
• Ability to characterize in bulk nanotubes and
composites, providing reproducible qualities of the
composites’ goods
• Clear understanding of what kinds of products are
going to be scaled up, toxic or safe? If nanotubes are
toxic, could nanotube composites be safe?
• If not, what are the limitations for applications of
nanotube composites?
16/03/06 Brussels V.A. Ryzhkov Assessing the advantages …19
Are sh-MWNTs a high-quality reproducible
product meeting demands?
•Yes, as Ros1 raw deposits contain ≥99wt% of
different carbon forms, including 40-60wt% of
shMWNTs and 20-30wt% of carbon polyhedral
nanoparticles (onions), whereas metals (mainly, Fe)
are less than 0.1-0.2wt%
•Yes
, as short median lengths of 200 - 350 nm provide
good dispersions and presumably non-toxic materials
•Yes
, as narrow median outer (8 -12 nm) and inner
diameters (2 -3 nm) provide flawless tough nanotubes
having high specific surfaces of 300-200 m2/g
resulting in dramatic improvements of polymer
composites even at rather low loadings (1-4wt%) of
sh-MWNTs
16/03/06 Brussels V.A. Ryzhkov Assessing the advantages …20
Cathode deposit structure according to our view on
the nanotube growth in arcs
16/03/06 Brussels V.A. Ryzhkov Assessing the advantages …21
Powdering the cathode deposits:
-deposits are easily layered between DOG and onion layers;
- soft oxidation burns layers of amorphous carbon providing very
fine (1 micron) powders; - MWNTs are mainly inside the particles;
- onions, DOG and Me nanoparticles are atop
Consequences:
Consequences:
-
-Me (0.03
Me (0.03-
-0.1wt%) can be
0.1wt%) can be
ultimately removed from fine
ultimately removed from fine
powders as they are at the
powders as they are at the
particles
particles’
’top;
top;
-
-DOG can be separated from
DOG can be separated from
MWNTs
MWNTs & onions;
& onions;
-
-surface analyses (SEM,
surface analyses (SEM,
AES,
AES,…
…) show lower MWNT
) show lower MWNT
contents
contents
16/03/06 Brussels V.A. Ryzhkov Assessing the advantages …22
SEM image of a layered deposit (Ros1)
16/03/06 Brussels V.A. Ryzhkov Assessing the advantages …23
AFM image of mildly ultra-sonicated Ros1 powder:
vertically aligned sh-MWNTs are aggregated in „islands“
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Further ultrasound treatment results in ultimate
dispersions of individual sh-MWNTs (TEM)
16/03/06 Brussels V.A. Ryzhkov Assessing the advantages …25
Just another morphology of sh-MWNTs (TEM)
16/03/06 Brussels V.A. Ryzhkov Assessing the advantages …26
Typical HR-TEM images of sh-MWNTs
16/03/06 Brussels V.A. Ryzhkov Assessing the advantages …27
HR-TEM images of typical sh-MWNTs
16/03/06 Brussels V.A. Ryzhkov Assessing the advantages …28
Buckyonions are main and useful carbon admixture
In our view, onions are non-grown MWNTs and their
content can be controlled in SLA
16/03/06 Brussels V.A. Ryzhkov Assessing the advantages …29
Graphitic sheets are typically made of 2-4 layers
16/03/06 Brussels V.A. Ryzhkov Assessing the advantages …30
Partially ordered and disordered graphite
16/03/06 Brussels V.A. Ryzhkov Assessing the advantages …31
Me nanoparticles are seen in proximity to the tubes
16/03/06 Brussels V.A. Ryzhkov Assessing the advantages …32
Metallic nanoparticles make less than 0.2-
0.1wt%, they are small and not covered with carbon,
and, therefore, they can be quantitatively removed
16/03/06 Brussels V.A. Ryzhkov Assessing the advantages …33
Should we scale up the nanotube production
right now?
•YES, as we able to produce cheap and high-quality
nanotubes with controllable / reproducible parameters in
bulk
• May be, as the availability of promising applications for
novel nanotube-polymer composites (see Chapter IV) can
facilitate meeting a “good will” of potential composite
producers
• May be, as appropriate techniques and standards for
characterization of nanotubes & composites in bulk are
under development
• May be, as at least short CNTs seem to be non-toxic
16/03/06 Brussels V.A. Ryzhkov Assessing the advantages …34
IV. Case studies of innovative applications
• Special pre-oxidation of raw sh-MWNTs (ROSSETER’s
proprietary process) followed by special plasma-chemical
treatments* facilitates successful incorporation of sh-MWNTs
into any polymer matrices *
• Typically, sh-MWNT-composite films, coating, plates, and
moldings are formed from nanotube dispersions in polymer
solvents. Mixing nanotubes with powdered / granulated
polymers followed by melting also gives good results *
• Teflon, polyimide and epoxy resins are first choice polymer
composites for sh-MWNTs at the moment *
_______________________________________________________
* - Dr. Alexander K. Filippov, General Director of PLASMAS Ltd,
St Petersburg, Russia, www.plasmas.spb.ru , plasmas@list.ru PLASMAS
16/03/06 Brussels V.A. Ryzhkov Assessing the advantages …35
sh-MWNT-Ftoroplast-4 films produced by
PLASMAS PLASMAS
Composite F-4 films with
different nanotube contents,
thicknesses (10-200 μm),
widths (5, 10 and 15 cm) and
unlimited lengths are
prepared by formation from
nanotubes’ dispersions in
solutions of Ftoroplast-4.
Thin films containing 1-2wt%
of sh-MWNTs are electrically
conductive and optically
transparent
16/03/06 Brussels V.A. Ryzhkov Assessing the advantages …36
80-90wt%-sh-MWNT-Ftoroplast-4-composite
films produced by PLASMAS
PLASMAS
80-90wt%-sh-MWNT-
Ftoroplast-4 composite
films are electrically
conductive, “soft” and
flexible and can be
twisted in any way and
direction almost without a
limitation.
The composites
demonstrate highly
increased Young
modulus, no irreversible
plastic deformation and
improved thermo-stability.
16/03/06 Brussels V.A. Ryzhkov Assessing the advantages …37
Main applications of sh-MWNT-polymer composites
currently under development by PLASMAS
• Electrodes for batteries and accumulators having
variety of configurations and sizes with highly
increased specific capacities and long-life
• Construction elements and paintings for cars, aircrafts,
ships, submarines, etc
• Safe and harmless heating elements & sensors in
textiles, buildings, cars, aircrafts, etc
• EMI protection & laser limiters, modulators and
switches
• Effective solar elements
PLASMAS
16/03/06 Brussels V.A. Ryzhkov Assessing the advantages …38
sh-MWNT-polyimide composite coatings
demonstrate promising non-linear optical properties **:
___________________________________________________________________
** - PLASMAS and Dr. Natalia V. Kamanina (Vavilov State Optical Institute),
kamanin@ffm.ioffe.ru ,St Petersburg, Russia
PLASMAS
• The best ever Optical Limiters: Photo-sensitive and non-sensitive
1-2%-sh-MWNT-polyimide composite films are used as light-guided
non-linear filters intensively absorbing irradiation in visible and near-
IR ranges (down to 1%-n0.1% in comparison with conventional 10-
15%) for protection of human eye and optical sensors from highly-
intense laser irradiation (can be used also for displays, etc)
• The fastest ever modulators and switches of laser irradiation for LCD:
switching speed is 0.1-0.3 ms in comparison with 7-9 ms for
conventional switches and 4ms for recently announced Samsung
switch
• Solar elements: Effective transformation of solar light in electricity
16/03/06 Brussels V.A. Ryzhkov Assessing the advantages …39
Enhancement of Li-ion-batteries
• Improvements of LIB specific capacity can be achieved as a
result of increase of specific surface area of the carbonaceous
anode via introduction of disorder/defects in the nanotube
walls
• However, a disorder of exterior nanotube surface causes
dramatic reduction of nanotube electric conductivity, adhesive
properties and package density, eventually increasing the first
cycle’s irreversible discharge capacity, reducing cycle-life and
self-discharge characteristics
• sh-MWNTs enable using a very different approach as defects
and disorder can be introduced inside the nanotubes’ walls
(as scrolls), whereas the nanotubes’ exterior surface is
flawless
PLASMAS
16/03/06 Brussels V.A. Ryzhkov Assessing the advantages …40
Prototypes of Li-Ion Batteries
developed by PLASMAS
SEM image of a LIB anode structure based on sh-MWNTs
Cylindrical type
LIBs with shMWNTs
PLASMAS
16/03/06 Brussels V.A. Ryzhkov Assessing the advantages …41
Integration of sh-MWNTs in LIB anodes:
specific capacity is more than doubled over commercial;
1st cycle’s behavior is excellent; long life is expected
PLASMAS
12345678
200
300
400
500
600
700
commercial, C<300mAh/g, η=93-96%
Sheng's nanocomposite, η=93-96%
sh-MWNTs/graphite, η=95-97%
Specific capacity (mAh/g)
Cycle number (a.u.)
16/03/06 Brussels V.A. Ryzhkov Assessing the advantages …42
Conclusions
• Carbon nanotubes and nanofibers have been proved as
the first choice additive for high performance polymers
• Various bulk production methods offer high-quality CNT /
CNF products but their prices are still high
• Absence of appropriate techniques and standards for bulk
characterization of nanotubes / composites complicated by
uncertainty of their toxicity delays a “good will” of potential
composite producers to scale up these novel industries
• Cheap, easily dispersed and presumably non-toxic
sh-MWNTs have a great potential for high performance
polymers
16/03/06 Brussels V.A. Ryzhkov Assessing the advantages …43
Acknowledgements
• to Mrs. Maria Xenophontos, Rosseter’s founder and
managing director, for her constant support of the
work
• to Dr. Alexander K. Filippov, General Director of
PLASMAS Ltd, and to Dr. Natalia V. Kamanina, Head
of Lab of Photophysics of fullerene-containing media
at Vavilov State Optical Institute, St Petersburg,
Russia for their extensive and productive researches
of novel composites based on Rosseter nanotube
materials
• to the Organizing Committee for the opportunity to
report to the Conference