627
Full Paper
Macromolecular
Chemistry and Physics
wileyonlinelibrary.com DOI: 10.1002/macp.201100659
Ethylene- co-Norbornene Copolymers Grafted
Carbon Nanotube Composites by In Situ
Polymerization
Laura Boggioni,* Giulia Scalcione, Andrea Ravasio, Fabio Bertini,
Cristina D’Arrigo, Incoronata Tritto
Vinyl functionalized multiwalled carbon nanotubes (MWCNT-vinyl) are synthesized and used
as monomers to prepare poly(ethylene- co-norbornene)-grafted carbon nanotube composites
by in situ polymerization with [Ti( η
5
-C
5
Me
5
)(N=C
t
Bu
2
)Cl
2
] activated with methylalumoxane
(MAO). The glass transition temperatures ( T
g
) of grafted MWCNT composites are more than
30 °C higher than those of copolymers. This difference is
rationalized by the immobilization of the copolymer chain
to the MWCNT surface by a covalent bond. The Young’s mod-
ulus is shown to increase by more than 200% compared to
poly(ethylene- co-norbornene) by incorporating 3.4 wt% func-
tionalized MWCNT.
L. Boggioni, G. Scalcione, A. Ravasio, F. Bertini, I. Tritto
Istituto per lo Studio delle Macromolecole, Consiglio
Nazionale delle Ricerche, via E. Bassini 15, 20133 Milano, Italy
E-mail: boggioni@ismac.cnr.it
C. D’Arrigo
Istituto per lo Studio delle Macromolecole, Consiglio
Nazionale delle Ricerche, Via De Marini 6, 16149 Genova, Italy
blending methods generally used for preparing nano-
composites are not suitable for polyolefins.
[4]
The in situ
polymerization of monomers in the presence of nanopar-
ticles and CNT is a promising method for obtaining nano-
composites in which nanotubes are dispersed individually
at nanometer level.
[5–7]
Copolymers of ethylene (E) with norbornene (N) [P(E-
co-N)] are thermoplastic materials that have recently
received great attention because of their attractive
properties
[8,9]
such as high T
g
, high optical transparency,
excellent moisture barrier, and chemical resistance. These
distinctive properties enable them to be utilized for a
wide variety of uses in advanced packaging, engineering
components, and optical applications.
Among the in situ methodologies hitherto reported,
P(E- co-N)-MWCNT were obtained with MAO-activated
metallocenes by polymerization filling technique (PFT),
[6]
and more recently by in situ synthesis with a highly active
methylalumoxane (MAO) free catalytic system.
[9]
Another method involves in situ polymerization in
the presence of functionalized nanotubes which can be
inserted into the polymer chain, resulting in covalent
attachment of nanotubes to the polymer. Consequently,
better dispersion and formation of a strong interface
between nanotubes and polymer matrix are achieved.
1. Introduction
The carbon nanotubes (CNT) are endowed with inter-
esting properties that modify the characteristics of the
polymer matrix in which they are embedded.
[1–4]
The
blending of polymer matrices with well dispersed CNT
as the filler (in low concentration, less than 5 wt%) may
enhance and modify the mechanical, electric, dielectric,
thermal, and crystallization properties of the host mate-
rial or even induce new nanoeffects. Such enhancement
and thus the success of a nanocomposite is related to the
achievement of a good dispersion of the nanofiller in the
polymer matrix. This is hindered by the tendency of CNT
to agglomerate in bundles due to van der Waals interac-
tions. Several approaches have been used to overcome
such difficulty and to enhance chemical compatibility
between CNT and polymer chains. Solution and melt
Ti
N
Cl
Cl
O
O
O
O
O
O
t
Bu
t
Bu
i) toluene, TIBA
ii) ultrasounds
iii)
+ MAO
O
O
3
3
3
3
Macromol. Chem. Phys. 2012, 213, 627−634
© 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim