**4. Conclusion**

The most frequent method for preparing polymer nanotubes composites has been mixing nanotubes and polymer in a suitable solvent and to evaporate the solvent to form composite film. But to increase the advantages at its best, one needs: (i) high interfacial area between nanotubes and polymer; and, (ii) strong interfacial interaction. Unfortunately this solvent technique does not help much in achieving these targets; and as a result a nanocomposite having properties much inferior to theoretical expectations are obtained. In order to obtain higher contact area between nanotubes and polymer, the issue of dispersion needs to be ad‐ dressed. Uniform dispersion of these nanotubes produces immense internal interfacial area, which is the key to enhancement of properties of interest. On the other hand, modification of nanotubes surface through functionalisation is required for creating an effective interaction with the host matrix and to make nanotubes soluble and dispersible.

associated to nanotube–nanotube interactions. Due to the high aspect ratio of CNT the per‐

Polymer Nanocomposites Containing Functionalised Multiwalled Carbon NanoTubes

http://dx.doi.org/10.5772/50710

103

Université de Lyon, Université Lyon 1, CNRS UMR5223, Ingénierie des Matériaux Poly‐

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[4] Grossiord, N., Loos, J., Regev, O., & Koning, C. E. (2006). Toolbox for dispersing car‐ bon nanotubes into polymers to get conductive nanocomposites. *Chemistry of Materi‐*

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black surface by trapping polymer radicals. *Polymer*, 48(10), 2866-2873.

Emmanuel Beyou, Sohaib Akbar, Philippe Chaumont and Philippe Cassagnau

mères: IMP@UCBL, 15 boulevard Latarget, F-69622 Villeurbanne, France

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bon Nanotubes. *Macromolecules*, 39(16), 5194-5205.

colation threshold can be expected to be less than 2% of CNT.

**Author details**

**References**

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The idea of grafting PE or PP with the help of peroxide during extrusion is exciting. It was shown that cumlyoxly radical generated by thermolysis of DCP can abstract hydrogen from polyolefin chains, thus creating polyolefin macroradicals. Then, these macroradicals add to the unsaturated carbon bonds on the surface of the nanotubes. The upside of this strategy is that radicals have short lifetimes which make the procedure possible in an extruder where the residence time is generally low. On the contrary, the downside is the low selectivity of radicals leading to a competition between radical combination reactions and radical addi‐ tion reactions. Alkanes can be used as model for PE to perform the grafting of PE onto nano‐ tubes. The results were interesting however the degree of PE grafting remained lower than the model (weight loss by TGA = 22% as compared to a weight loss of 30% in case of penta‐ decane). LDPE grafting density on nanotubes was 1.1mg.m-2 while incorporation of TEMPO raised the grafting density to 1.4mg.m-2. End functionalised PE can also be used for PE graft‐ ing onto nanotubes with dichlorobenzene as solvent. As emphasized by TEM images, a lay‐ er of considerable thickness has been grafted around the periphery of the nanotubes.

In order to follow the same strategy for nanotubes functionalisation with PP, tetramethyl‐ pentadecane has been selected as a model compound for PP. It was successfully grafted onto carbon nanotubes with a grafting density of 0.92 mg/m2 . However, the grafting of PP onto nanotubes did not permit to obtain reproductible results. SEM images of the PP-*g*-MWCNTs nanocomposites with filler loadings of 3wt% in PP matrix did not show a significant im‐ provement in MWCNTs dispersion within the PP matrix although sizes of the aggregates were slightly reduced.

In addition, it can be expected that the rheological percolation, and subsequently the nonlinearity effect, depend on nanotube dispersion and aspect ratio. Low shear deformations in‐ duced an aggregation mechanism, but these aggregates broke down at high shear, forming small aggregates with less entanglements. In a high viscous polymer media, it was shown that carbon nanotubes could not be considered anymore as Brownian entities. A general rheological trend for CNTs-based nanocomposites is the appearance of a transition from a liquid-like behaviour to a solid-like behaviour increasing with the CNT content because it is associated to nanotube–nanotube interactions. Due to the high aspect ratio of CNT the per‐ colation threshold can be expected to be less than 2% of CNT.

### **Author details**

**4. Conclusion**

The most frequent method for preparing polymer nanotubes composites has been mixing nanotubes and polymer in a suitable solvent and to evaporate the solvent to form composite film. But to increase the advantages at its best, one needs: (i) high interfacial area between nanotubes and polymer; and, (ii) strong interfacial interaction. Unfortunately this solvent technique does not help much in achieving these targets; and as a result a nanocomposite having properties much inferior to theoretical expectations are obtained. In order to obtain higher contact area between nanotubes and polymer, the issue of dispersion needs to be ad‐ dressed. Uniform dispersion of these nanotubes produces immense internal interfacial area, which is the key to enhancement of properties of interest. On the other hand, modification of nanotubes surface through functionalisation is required for creating an effective interaction

The idea of grafting PE or PP with the help of peroxide during extrusion is exciting. It was shown that cumlyoxly radical generated by thermolysis of DCP can abstract hydrogen from polyolefin chains, thus creating polyolefin macroradicals. Then, these macroradicals add to the unsaturated carbon bonds on the surface of the nanotubes. The upside of this strategy is that radicals have short lifetimes which make the procedure possible in an extruder where the residence time is generally low. On the contrary, the downside is the low selectivity of radicals leading to a competition between radical combination reactions and radical addi‐ tion reactions. Alkanes can be used as model for PE to perform the grafting of PE onto nano‐ tubes. The results were interesting however the degree of PE grafting remained lower than the model (weight loss by TGA = 22% as compared to a weight loss of 30% in case of penta‐ decane). LDPE grafting density on nanotubes was 1.1mg.m-2 while incorporation of TEMPO raised the grafting density to 1.4mg.m-2. End functionalised PE can also be used for PE graft‐ ing onto nanotubes with dichlorobenzene as solvent. As emphasized by TEM images, a lay‐

er of considerable thickness has been grafted around the periphery of the nanotubes.

carbon nanotubes with a grafting density of 0.92 mg/m2

were slightly reduced.

In order to follow the same strategy for nanotubes functionalisation with PP, tetramethyl‐ pentadecane has been selected as a model compound for PP. It was successfully grafted onto

nanotubes did not permit to obtain reproductible results. SEM images of the PP-*g*-MWCNTs nanocomposites with filler loadings of 3wt% in PP matrix did not show a significant im‐ provement in MWCNTs dispersion within the PP matrix although sizes of the aggregates

In addition, it can be expected that the rheological percolation, and subsequently the nonlinearity effect, depend on nanotube dispersion and aspect ratio. Low shear deformations in‐ duced an aggregation mechanism, but these aggregates broke down at high shear, forming small aggregates with less entanglements. In a high viscous polymer media, it was shown that carbon nanotubes could not be considered anymore as Brownian entities. A general rheological trend for CNTs-based nanocomposites is the appearance of a transition from a liquid-like behaviour to a solid-like behaviour increasing with the CNT content because it is

. However, the grafting of PP onto

with the host matrix and to make nanotubes soluble and dispersible.

102 Syntheses and Applications of Carbon Nanotubes and Their Composites

Emmanuel Beyou, Sohaib Akbar, Philippe Chaumont and Philippe Cassagnau

Université de Lyon, Université Lyon 1, CNRS UMR5223, Ingénierie des Matériaux Poly‐ mères: IMP@UCBL, 15 boulevard Latarget, F-69622 Villeurbanne, France

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**Chapter 6**

**Characterization and Morphology of Modified Multi-**

**Rubber (TPNR) Composite**

http://dx.doi.org/10.5772/50726

**1. Introduction**

properties of CNTs.

Mou'ad A. Tarawneh and Sahrim Hj. Ahmad

Additional information is available at the end of the chapter

**Walled Carbon Nanotubes Filled Thermoplastic Natural**

Carbon nanotubes describes a specific topic within solid-state physics, but is also of interest in other sciences like chemistry or biology. Actually the topic has floating boundaries, because we are at the molecule level. In the recent years carbon nanotubes have become more and more popular to the scientists. Initially, it was the spectacularly electronic properties, that were the basis for the great interest, but eventually other remarkable properties were also discovered. The first CNTs were prepared by M. Endo in 1978, as part of his PhD studies at the Universi‐ ty of Orleans in France. Although he produced very small diameter filaments (about 7 nm) using a vapour-growth technique, these fibers were not recognized as nanotubes and were not studied systematically. It was only after the discovery of fullerenes, C60, in 1985 that re‐ searchers started to explore carbon structures further. In 1991, when the Japanese electron microscopist Sumio Iijima [1] observed CNTs, the field really started to advance. He was studying the material deposited on the cathode during the arc-evaporation synthesis of full‐ erenes and came across CNTs. A short time later, Thomas Ebbesen and Pulickel Ajayan, from Iijima's lab, showed how nanotubes could be produced in bulk quantities by varying the arc-evaporation conditions. However, the standard arc-evaporation method only pro‐ duced only multiwall nanotubes. After some research, it was found that the addition of met‐ als such as cobalt to the graphite electrodes resulted in extremely fine single wall nanotubes. The synthesis in 1993 of single-walled carbon nanotubes (SWNTs) was a major event in the development of CNTs. Although the discovery of CNTs was an accidental event, it opened the way for a flourishing research into the properties of CNTs in labs all over the world, with many scientists demonstrating promising physical, chemical, structural, and optical

> © 2013 Tarawneh and Ahmad; licensee InTech. This is an open access article distributed under the terms of the Creative Commons Attribution License (http://creativecommons.org/licenses/by/3.0), which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.

© 2013 Tarawneh and Ahmad; licensee InTech. This is a paper distributed under the terms of the Creative Commons Attribution License (http://creativecommons.org/licenses/by/3.0), which permits unrestricted use,

distribution, and reproduction in any medium, provided the original work is properly cited.
