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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.


FT-IR and Raman spectra of nanomaterials. (A) IR spectra of pure POSS (a), POSS-N3 (b), MWNT-POSS nanohybrid (c), and MWNTs-alkyne (d). (B) Raman spectra of pristine MWNTs, MWNTs-alkyne, and MWNT-POSS nanohybrid.
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Figure 2: FT-IR and Raman spectra of nanomaterials. (A) IR spectra of pure POSS (a), POSS-N3 (b), MWNT-POSS nanohybrid (c), and MWNTs-alkyne (d). (B) Raman spectra of pristine MWNTs, MWNTs-alkyne, and MWNT-POSS nanohybrid.

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)

FT-IR and Raman spectra of nanomaterials. (A) IR spectra of pure POSS (a), POSS-N3 (b), MWNT-POSS nanohybrid (c), and MWNTs-alkyne (d). (B) Raman spectra of pristine MWNTs, MWNTs-alkyne, and MWNT-POSS nanohybrid.
© Copyright Policy - open-access
Related In: Results  -  Collection

License
Show All Figures
getmorefigures.php?uid=PMC3211168&req=5

Figure 2: FT-IR and Raman spectra of nanomaterials. (A) IR spectra of pure POSS (a), POSS-N3 (b), MWNT-POSS nanohybrid (c), and MWNTs-alkyne (d). (B) Raman spectra of pristine MWNTs, MWNTs-alkyne, and MWNT-POSS nanohybrid.
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.