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Synthesis of multi-walled carbon nanotube/polyhedral oligomeric silsesquioxane nanohybrid by utilizing click chemistry.

Yadav SK, Mahapatra SS, Yoo HJ, Cho JW - Nanoscale Res Lett (2011)

Bottom Line: A new hybrid material consisting of a polyhedral oligomeric silsesquioxane (POSS) and carbon nanotube (CNT) was synthesized by a simple and versatile approach entailing click coupling between azide moiety-functionalized POSS and alkyne-functionalized multi-walled CNTs.This approach provides a simple and convenient route to efficiently functionalize a wide variety of nanoscale nanostructure materials on the surface of CNTs.

View Article: PubMed Central - HTML - PubMed

Affiliation: Department of Textile Engineering, Konkuk University, Seoul 143-701, Korea. jwcho@konkuk.ac.kr.

ABSTRACT
A new hybrid material consisting of a polyhedral oligomeric silsesquioxane (POSS) and carbon nanotube (CNT) was synthesized by a simple and versatile approach entailing click coupling between azide moiety-functionalized POSS and alkyne-functionalized multi-walled CNTs. This approach provides a simple and convenient route to efficiently functionalize a wide variety of nanoscale nanostructure materials on the surface of CNTs.

No MeSH data available.


1H NMR and 13C NMR spectra of azide functionalized POSS. (a) 1H NMR spectrum of POSS-N3 and (b) 13C NMR spectrum of POSS-N3.
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Figure 3: 1H NMR and 13C NMR spectra of azide functionalized POSS. (a) 1H NMR spectrum of POSS-N3 and (b) 13C NMR spectrum of POSS-N3.

Mentions: The aim of this study is to prepare covalently functionalized MWNT-POSS nanohybrids by click chemistry between azide-functionalized POSS (POSS-N3) and alkyne-functionalized MWNTs (Figure 1). Alkyne-functionalized MWNTs are prepared via a solvent-free diazotization reaction and a coupling reaction between MWNTs and p-aminophenyl propargyl ether. POSS-N3 is prepared by a simple reaction of POSS with sodium azide in the presence of ammonium chloride. The success of click cycloaddition is supported by evidence from FT-IR, Raman, XPS, TEM, EDX, and TGA. As a confirmation of the reactions, Figure 2a shows the IR spectra of pure POSS, which has characteristic peaks at 1111 cm-1 for Si-O-Si stretching [18], 1462 cm-1 for CH2 stretching of cyclohexyl [19], and 1228 cm-1 for Si-CH2 stretching [20]. The azidation of the POSS molecule was also confirmed by comparison of the IR spectrum of pure POSS with that of POSS (POSS-N3) with azide-functionality. A new peak at 2107 cm-1 corresponding to the azide group [21], and simultaneously another peak at 3440 cm-1 for OH stretching were observed. The results of 1H NMR and 13C NMR measurements reveal clearly the POSS-N3 structure (Figure 3a,b). The charecteristic signals at δ = 3.18 and 3.12 ppm in 1H NMR, and δ = 69.2 and 52-53 in 13C NMR are assigned to the -CH proton and carbon of cyclohexane combined with -OH and N3 groups, respectively. Elemental anlysis results are also in good agreement with experimental values (Table 1), confirming the successful azidation of POSS. The click coupling between the alkyne-functionalized MWNTs and azide-functionalized POSS in the presence of Cu(I) catalyst provided a 1,2,3-triazole ring. This indicates that the POSS molecule is successfully attached to the surface of the MWNTs. Thus, the IR spectra of MWNT-POSS nanohybrid, featuring a azide peak of POSS molecules at 2107 cm,-1 completely disappeared, indicating the formation of 1,2,3-triazole after the click reaction.


Synthesis of multi-walled carbon nanotube/polyhedral oligomeric silsesquioxane nanohybrid by utilizing click chemistry.

Yadav SK, Mahapatra SS, Yoo HJ, Cho JW - Nanoscale Res Lett (2011)

1H NMR and 13C NMR spectra of azide functionalized POSS. (a) 1H NMR spectrum of POSS-N3 and (b) 13C NMR spectrum of POSS-N3.
© Copyright Policy - open-access
Related In: Results  -  Collection

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Figure 3: 1H NMR and 13C NMR spectra of azide functionalized POSS. (a) 1H NMR spectrum of POSS-N3 and (b) 13C NMR spectrum of POSS-N3.
Mentions: The aim of this study is to prepare covalently functionalized MWNT-POSS nanohybrids by click chemistry between azide-functionalized POSS (POSS-N3) and alkyne-functionalized MWNTs (Figure 1). Alkyne-functionalized MWNTs are prepared via a solvent-free diazotization reaction and a coupling reaction between MWNTs and p-aminophenyl propargyl ether. POSS-N3 is prepared by a simple reaction of POSS with sodium azide in the presence of ammonium chloride. The success of click cycloaddition is supported by evidence from FT-IR, Raman, XPS, TEM, EDX, and TGA. As a confirmation of the reactions, Figure 2a shows the IR spectra of pure POSS, which has characteristic peaks at 1111 cm-1 for Si-O-Si stretching [18], 1462 cm-1 for CH2 stretching of cyclohexyl [19], and 1228 cm-1 for Si-CH2 stretching [20]. The azidation of the POSS molecule was also confirmed by comparison of the IR spectrum of pure POSS with that of POSS (POSS-N3) with azide-functionality. A new peak at 2107 cm-1 corresponding to the azide group [21], and simultaneously another peak at 3440 cm-1 for OH stretching were observed. The results of 1H NMR and 13C NMR measurements reveal clearly the POSS-N3 structure (Figure 3a,b). The charecteristic signals at δ = 3.18 and 3.12 ppm in 1H NMR, and δ = 69.2 and 52-53 in 13C NMR are assigned to the -CH proton and carbon of cyclohexane combined with -OH and N3 groups, respectively. Elemental anlysis results are also in good agreement with experimental values (Table 1), confirming the successful azidation of POSS. The click coupling between the alkyne-functionalized MWNTs and azide-functionalized POSS in the presence of Cu(I) catalyst provided a 1,2,3-triazole ring. This indicates that the POSS molecule is successfully attached to the surface of the MWNTs. Thus, the IR spectra of MWNT-POSS nanohybrid, featuring a azide peak of POSS molecules at 2107 cm,-1 completely disappeared, indicating the formation of 1,2,3-triazole after the click reaction.

Bottom Line: A new hybrid material consisting of a polyhedral oligomeric silsesquioxane (POSS) and carbon nanotube (CNT) was synthesized by a simple and versatile approach entailing click coupling between azide moiety-functionalized POSS and alkyne-functionalized multi-walled CNTs.This approach provides a simple and convenient route to efficiently functionalize a wide variety of nanoscale nanostructure materials on the surface of CNTs.

View Article: PubMed Central - HTML - PubMed

Affiliation: Department of Textile Engineering, Konkuk University, Seoul 143-701, Korea. jwcho@konkuk.ac.kr.

ABSTRACT
A new hybrid material consisting of a polyhedral oligomeric silsesquioxane (POSS) and carbon nanotube (CNT) was synthesized by a simple and versatile approach entailing click coupling between azide moiety-functionalized POSS and alkyne-functionalized multi-walled CNTs. This approach provides a simple and convenient route to efficiently functionalize a wide variety of nanoscale nanostructure materials on the surface of CNTs.

No MeSH data available.