SINGLE WALL CARBON NANOTUBES A UNIQUE ADDITIVE FOR ELECTRICALLY CONDUCTIVE PLASTICS MPG SEMINAR 28TH NOVEMBER 2016 Michael Enotiades European Sales Manager Office: +352 661 2799 0373 Mobile: +352 661 184 007 [email protected]
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SINGLE WALL CARBON NANOTUBES A UNIQUE ADDITIVE FOR ELECTRICALLY CONDUCTIVE
PLASTICSMPG SEMINAR 28TH NOVEMBER 2016
Michael EnotiadesEuropean Sales Manager
Office: +352 661 2799 0373Mobile: +352 661 184 007
CONTENTS
OCSiAl
Single Wall Carbon Nanotubes
SWCNT in thermoplastics
OCSiAl products
Summary and path forward
1
2
3
4
5
ABOUT OCSiAl1
2009Founded to develop scalable synthesis of single wall carbon nanotubes (SWCNT)
2013Award patent for scalable SWCNT production
Launched Graphetron V1.0 nanotube reactor10 T/Y capacity
2014Began large scale industrial sampling
2016260+ people, 30 Ph.D.
Product lines for batteries, plastics, composites, coatings, elastomers
10 TONS/YR OUTPUT90% of Global SWCNT Production
4,200 m2
FACILITY
1 OCSiAl PRODUCTION FACILITYGRAPHETRON V1.0 SWCNT REACTOR
OCSiAl GROUP WORLDWIDE
Sunnyvale,CA
Incheon
Luxembourg
MoscowNovosibirskColumbus,
OH
Shenzhen,Hong-KongMumbai
1
CONTENTS
OCSiAl
Single Wall Carbon Nanotubes
SWCNT in thermoplastics
OCSiAl products
Summary and path forward
1
2
3
4
5
SINGLE WALL CARBON NANOTUBES(SWCNT)
Diameter 1.5-2.0 nm
Length > 5 μm
Wall thickness 1 atom
2
Thermal stability
Strongerthan steel
Surface area The highest length to diameter ratio
One ofthe best conductorsin the world
up to
1000 °C100 times
1g =2 basketball
courts
several
thousand times
5 timeslighter than copper
TUBALL™SWCNT WITH EXCEPTIONAL PROPERTIES
2
CONCENTRATION OFPARTICLES ~0.1%
0,5 mm
NANOFIBERS SWCNTMICROPARTICLES
A B C
0,5 mm
0,5 mm
0,5 mm
0,5 mm
0,5 mm
0,5 mm
0,5 mm0,5 mm
1
1
11
1 0 1 0 1 0
00
00
00
11
2 TUBALL™FORMS ITS OWN CONDUCTIVE 3D NETWORKAT ULTRA LOW CONCENTRATIONS
2
CONDUCTIVE CARBON BLACK
TUBALL™
TUBALL™ VS. CARBON BLACK
2
1 um
MWCNT TUBALL™
200 um200 um
1 um
MWCNT TUBALL™
TUBALL™ VS. MWCNT
CONTENTS
OCSiAl
Single Wall Carbon Nanotubes
SWCNT in thermoplastics
OCSiAl products
Summary and path forward
1
2
3
4
5
INSULATIVE
ANTISTATIC
DISSIPATIVE
CONDUCTIVE
Metals
Standard Plastics
CONDUCTIVE PLASTICS
in ESD applications
1014
1012
1010
108
106
104
102
1
10-2
10-4
10-14
10-12
10-10
10-8
10-6
10-4
10-2
1
102
104
Resistivity(W cm)
Conductivity(S/cm)
3 TUBALL™ CONDUCTIVITY RANGES
Solution Mixing Melt Mixing In Situ Polymerization
© 2013 Beyou et al.; licensee InTech.
3 TUBALL™ INCORPORATION METHODS
1. Preparation of a MB at 2% CNT
2. Masterbatch dilution on twin screw for compounds preparation
3
Twin screw
DISPERSION THROUGH 2 STEPS PROCESS
TUBALL™ MELT MIXING APPROACHFOCUS ON POLYOLEFINS
1.0E+01
1.0E+02
1.0E+03
1.0E+04
1.0E+05
1.0E+06
1.0E+07
1.0E+08
0 0.05 0.1 0.15 0.2 0.25
Volu
me r
esis
tivity,
Wc
m
TUBALL single wall carbon nanotubes, %
CONCEPT VALIDATION ON MICROCOMPOUNDER
Percolation is observed at very low dosages
3 TUBALL™ IN POLYPROPYLENE
PROCESS OPTIMIZATION ENABLES CONDUCTIVE COMPOUNDS AT LOW DOSAGE
3
Berstorff ZE-25: 25mm co-rotating, L/D 48
TUBALL™ IN POLYPROPYLENE
3 TUBALL™ IN POLYPROPYLENE
3
1.0E+03
1.0E+05
1.0E+07
1.0E+09
1.0E+11
1.0E+13
1.0E+15
Low T° (MB andCmpd)
High T° (MB andCmpd)
Influence of Process temperature
0,1% CNT 0,2% CNT
Vo
lum
e re
sist
ivit
y(o
hm
*cm
)
Higher Temperature tends toreduce the Van de Waalsinteractions between the tubes.
High temperature reducesviscosity of molten polymer,facilitating incorporation.
Low T° : 220°C High T° : 250°C
TUBALL™ IN POLYPROPYLENE
Target a High Specific Mechanical Energy during compounding:
– High ratio/amount of kneading elements
– High screw speed
– Decrease output rate
– Optimize processing temperature
3 TUBALL™ IN POLYPROPYLENE
GENERAL GUIDELINES FOR MASTERBATCH PREPARATION
3 CONDUCTIVITY IN POLYOLEFINS
TASK: Achieve less than 104 Ohm.cm resistivity, while maintaining a tensilestrength of 12 MPa and an elongation at break of 70-200%IDEAS: Hybrid carbon black and TUBALLTM system
40 wt.% Carbon blackConductive
10-20 wt.% Carbon black+ 0,2 wt.% TUBALL
Decreasing physical-mech. properties
Impossible to use PE Possible to use PE
3
PRELIMINARY RESULTS – Property modification
CONDUCTIVITY IN POLYOLEFINS
Tuball (%) CB (%) Polymer R (Ohm.cm) Tensile strength (MPa)
Elongation at break (%)
0.2 24 LDPE 103 14 120
3
1.0E+02
1.0E+04
1.0E+06
1.0E+08
1.0E+10
1.0E+12
1.0E+14
LLDPE HDPE LDPE
Masterbatch of 2% TUBALL™diluted in MFI 20 resin
0,05 % CNT 0,1% CNT 0,2% CNT
VR
Oh
m.c
m
Haake Polylab PTW 16/40, 16 mm co-rotating, L/D 40
TUBALL™ IN POLYETHYLENECONDUCTIVE POLYETHYLENES OBTAINED AT LOW CNT DOSAGE
CONTENTS
OCSiAl
Single Wall Carbon Nanotubes
SWCNT in thermoplastics
OCSiAl products
Summary and path forward
1
2
3
4
5
SPECIFICATION VALUE
CARBON CONTENT, wt. % >85
CNT, wt. % ≥75
NUMBER OF LAYERS CNT 1-2
OUTER MEAN DIAMETER CNT, nm 1.8±0.4
LENGTH OF CNT, μm >5
METAL IMPURITIES, wt. % <15
Certificate of analysis by Intertek#: IWTN/COA/W663/001 (14 May 2014)
4
TUBALLTM
Dosage
Melt flow index
at 230°C/2.16kg
(ASTM D1238)
Melting point
(ISO 11357)
Real density
(internal
method)
Moisture
content
(at packaging)
2 wt. % 10 g/10 min 165 °С 918 kg/m3 < 0.01% ppm
Primary characteristics of TUBALLTM PLAST_E PP
Primary characteristics of TUBALLTM PLAST_E PE
TUBALLTM
Dosage
Melt flow index
at 190°C/2.16kg
(ASTM D1238)
Melting point
(ISO 11357)
Real density
(internal
method)
Moisture
content
(at packaging)
2 wt. % 2.9 g/10 min 127 °С 941 kg/m3 < 0.01% ppm
PLAST_E MASTERBATCHESDEMONSTRATORS FOR POLYOLEFINS
1.0E+02
1.0E+03
1.0E+04
1.0E+05
1.0E+06
1.0E+07
1.0E+08
0 0.5 1 1.5 2 2.5 3
Su
rfa
ce
re
sis
tivity,
Ω/s
q
TUBALL™ MATRIX 202, wt.%
Incorporation approach
MATRIX 202 FOR SOFT PVCDEVELOPMENTAL GRADE
4
CONTENTS
OCSiAl
Single Wall Carbon Nanotubes
SWCNT in thermoplastics
OCSiAl products
Summary and path forward
1
2
3
4
5
5 SUMMARY
1. OCSiAl has developed a continuous, high volume process for producing
nanotubes.
2. TUBALL™ is a high quality, very conductive single wall carbon nanotube
product.
3. TUBALL™ can be incorporated in thermoplastics through melt mixing.
4. Conductive networks can be created in polymer matrices at
low TUBALL™ dosages without compromising properties.
5. More solutions for thermoplastics are under development.
5 REACH (EU) AND EPA (USA)
1. Tuball is compliant in the EU for
commercial sales up to 1 T/Y
2. REACH application for up to 10 T/Y has
been achieved. File number
01-2120130006-75-0000
3. OCSiAl is in the final stages of preparing
PMN for EPA
OCSiAl GROUPRedefining materials
Reinventing technologies
THANK YOU FOR YOUR ATTENTION !
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