Low degree of functionalization of Single-Walled Carbon Nanotubes probed by highly sensitive characterization techniques

Lejosne, Johann; Mercier, Guillaume; Mamane, Victor; Fort, Yves; Marêché, J.F.; McRae, E.; Valsaque, Fabrice; Vigolo, Brigitte

doi:10.1016/j.carbon.2011.03.019

Cited by 13 publications

(14 citation statements)

References 24 publications

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“…For comparison, it is 3.9 × 10 −13 A for f-SWNT-5min, 6.5 × 10 −13 A for f-SWNT-10min, and goes down to 2.4 × 10 −13 A for f-SWNT-15min. For all samples, the relative intensity of the recorded m / z of chlorobenzene turned out to be different from our expectations with intensities for the fragments containing chlorine ( m / z 112 and 114) being less intense than those from the phenyl part ( m / z 50 and 51) [6]. It is noteworthy that this difference is more pronounced for f-SWNT-15min.…”

Section: Resultscontrasting

confidence: 83%

“…It is recognized to be an efficient way to confer specific surface properties [ 5 ]. However, the methods generally used for the covalent functionalization of CNTs often require long reaction times (from several hours to days) [ 6 ]. The reaction times can be considerably reduced to a few minutes by using microwave-induced heating [ 7 ] as shown by the increasing number of publications in the past years [ 8 ].…”

Section: Introductionmentioning

confidence: 99%

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Chemi- vs physisorption in the radical functionalization of single-walled carbon nanotubes under microwaves

Mamane¹,

Mercier²,

Shukor³

et al. 2014

Beilstein J. Nanotechnol.

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SummaryThe effect of microwaves on the functionalization of single-walled carbon nanotubes (SWNTs) by the diazonium method was studied. The usage of a new approach led to the identification of the strength of the interaction (physical or chemical) between the functional groups and the carbon nanotube surface. Moreover, the nature (chemical formula) of the adsorbed/grafted functional groups was determined. According to thermogravimetric analysis coupled with mass spectrometry and Raman spectroscopy, the optimal functionalization level was reached after 5 min of reaction. Prolonged reaction times can lead to undesired reactions such as defunctionalization, solvent addition and polymerization of the grafted functions. The strength (chemi- vs physisorption) of the bonds between the grafted functional groups and the SWNTs is discussed showing the occurrence of physical adsorption as a consequence of defunctionalization after 15 min of reaction under microwaves. Several chemical mechanisms of grafting could be identified, and it was possible to distinguish conditions leading to the desired chemical grafting from those leading to undesired reactions such as physisorption and polymerization.

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Section: Resultscontrasting

confidence: 83%

Section: Introductionmentioning

confidence: 99%

Chemi- vs physisorption in the radical functionalization of single-walled carbon nanotubes under microwaves

Mamane¹,

Mercier²,

Shukor³

et al. 2014

Beilstein J. Nanotechnol.

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“…The pristine MWCNT have a weight loss of 2 wt% at 750 °C and the MWCNT‐COOH (B) and MWCNT‐vinyl (B) have a weight loss of 12, and 16 wt%, respectively (Figure 1). The degree of functionalization of CNT can be calculated from TGA data 19. For instance, the degree of functionalization of MWCNT‐COOH (B) was estimated as one carboxylic group per 34 carbon atoms.…”

Section: Resultsmentioning

confidence: 99%

Ethylene‐co‐Norbornene Copolymers Grafted Carbon Nanotube Composites by In Situ Polymerization

Boggioni

Scalcione

Ravasio

et al. 2012

Macro Chemistry & Physics

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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 )(NϭC 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 modulus is shown to increase by more than 200% compared to poly(ethylene-co -norbornene) by incorporating 3.4 wt% functionalized MWCNT.blending methods generally used for preparing nanocomposites are not suitable for polyolefi ns. [ 4 ] The in situ polymerization of monomers in the presence of nanoparticles and CNT is a promising method for obtaining nanocomposites in which nanotubes are dispersed individually at nanometer level. [5][6][7] Copolymers of ethylene (E) with norbornene (N) [P(Eco -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 fi lling 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.

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“…This result, compared with the 1.1 atomic percentage of COOH groups per nanotube, suggests the conversion of ~92.7% of the carboxylic acid groups. 18,19 In order to assess the integrity of the SWNTs, we compared the spectra of unmodified SWNT and functionalized SWNT via Raman spectroscopy. This analysis suggested that the inherent structure of the SWNT was maintained through the functionalization process.…”

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confidence: 99%

One-step synthesis of fluorescently labelled, single-walled carbon nanotubes

et al. 2015

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Low degree of functionalization of Single-Walled Carbon Nanotubes probed by highly sensitive characterization techniques

Cited by 13 publications

References 24 publications

Chemi- vs physisorption in the radical functionalization of single-walled carbon nanotubes under microwaves

Chemi- vs physisorption in the radical functionalization of single-walled carbon nanotubes under microwaves

Ethylene‐co‐Norbornene Copolymers Grafted Carbon Nanotube Composites by In Situ Polymerization

One-step synthesis of fluorescently labelled, single-walled carbon nanotubes

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