Chromatographic Purification and Properties of Soluble Single-Walled Carbon Nanotubes

Zhao, Bin; Huang, Hui; Niyogi, Sandip; Itkis, Mikhail E.; Hamon, Mark A.; Bhowmik, Paragranjita; Meier, Mark S.; Haddon, Robert C.

doi:10.1021/ja010488j

Cited by 129 publications

(105 citation statements)

References 22 publications

(32 reference statements)

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“…Several approaches have been attempted to remove these impurities, such as gas phase reaction, 15Ϫ17 acid oxidation, 18Ϫ20 electrochemical oxidation, 21 filtration, 22 and chromatography; 23 however, no method produces both high yields and scalability. For large-scale purification, gas phase oxidation is very attractive since it is simple to scale up and low in cost.…”

Section: ϫ3mentioning

confidence: 99%

Room Temperature Purification of Few-Walled Carbon Nanotubes with High Yield

et al. 2008

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Purification of high-quality few-walled carbon nanotubes (fWNTs) was developed by slow but selective oxidation in hydrogen peroxide (H 2 O 2 ) at room temperature. The purity, nanotubes' structure, and thermal stability of purified fWNTs were characterized by transmission electron microscopy (TEM), Raman spectroscopy, and thermogravimetric analysis (TGA), respectively. The results showed that fWNTs could be selectively purified by prolonging the stirring time in 30 wt % H 2 O 2 solution. Highly purified fWNTs were obtained, having a high G/D ratio in Raman spectra and good thermal stability indicating the good quality of the purified fWNTs.The approach provides a simple low cost method for purification that also has higher nanotube yield than other purification methods.

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Section: ϫ3mentioning

confidence: 99%

Room Temperature Purification of Few-Walled Carbon Nanotubes with High Yield

et al. 2008

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“…However in this case sample damage was increased, and indeed by the end of the procedure the sample vanished completely due to successive exposure to oxidation by heat and acid. Although the use of HNO 3 acid is known to purify raw nanotubes [28], the low final yield (∼3.8 wt.%, as indicated in Tab. 2) obtained from this procedure shows that HNO 3 introduces significantly more defects on the surface of the nanotubes than HCl treatment, which facilitates their subsequent destruction during oxidation due to loss of structural integrity.…”

Section: Procedures 3 [P3]mentioning

confidence: 99%

Purification of single-walled carbon nanotubes

Yaya

Ewels

Wagner

et al. 2011

Eur. Phys. J. Appl. Phys.

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Abstract. We present a study of purification of single-walled carbon nanotubes (SWCNTs) using different oxidation temperatures and chemical treatments. We have developed a simple two annealing-steps procedure resulting in high nanotube purity with minimal sample loss. The process involves annealing the SWCNTs at 300 • C for 2 h with subsequent reflux in 6 M HCl at 130 • C, followed by further annealing at 350 • C for 1 h with reflux in 6 M HCl at 130 • C. The process results in effective removal of carbon impurities and metal particles which are associated with SWCNTs production. The process is less time consuming (complete in 4.5 h) than conventional acid purification methods which require over 5 h, and less destructive than conventional methods with a yield of 26%. SWCNT purity was assessed using Raman spectroscopy, thermogravimetry and scanning electron microscopy coupled with energy-dispersive X-ray spectroscopy.

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“…Fig. 5 shows the solution-phase NIR absorption spectra of sample Dispersion 6 in the range of 850-1290 nm, corresponding to the second optical absorption bands originating from semiconducting SWNTs (S 22 ). To estimate the real purity of our purified sample, a reference is necessary.…”

Section: Shortened Carbolex Swntsmentioning

confidence: 99%

“…Fig. 11 shows the solution-phase NIR absorption spectra of the reaction mixture, Dispersions 2-10 and Residue in the range of 850-1290 nm, corresponding to the second optical absorption bands originating from semiconducting SWNTs (S 22 ). Purity calculations reveal that the relative purities of Dispersions 2-10 and Residue with respect to the reaction mixture are 5.1 and 1.1, respectively.…”

Section: Full-length Carbolex Swntsmentioning

confidence: 99%

“…Such dissolution not only provides an effective approach to bundle exfoliation and chemical maneuverability of SWNTs, but also allows the removal of varying impurities from nanotubes by microfiltration [16], capillary electrophoresis separation [17], and chromatographic isolation [22]. In the case of covalent functionalization, the amidation or esterification of the carboxylic acid groups of oxidized SWNT material and adding reactive groups onto the sidewalls were proposed [20].…”

Section: Introductionmentioning

confidence: 99%

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Centrifugal purification of chemically modified single-walled carbon nanotubes

Jia

Lian

Ishitsuka

et al. 2005

Science and Technology of Advanced Materials

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A wet chemistry procedure which couples chemical functionalization and a dispersion-centrifugation cycle was applied to the dissolution and purification of as-prepared electric-arc produced single-walled carbon nanotubes (SWNTs). It is validated that K 2 S 2 O 8 treatment generates hydrophilic groups such as carboxyl and hydroxyl on the surfaces of varying carbons, whereas such treatment also causes no severe destruction on the structure of SWNTs. Amidation of the K 2 S 2 O 8 -treated and mixed acids shortened SWNTs leads them largely soluble in tetrahydrofuran (THF) or other organic solvents. The soluble sample was fractionated via a dispersion-centrifugation cycle and highly pure and well-separated SWNTs were successfully obtained in the middle fractions. The purity of the centrifugally fractionated samples is qualitatively estimated with Raman spectroscopy, scanning electron microscope (SEM), and atomic force microscopy (AFM). Quantitative optical absorption spectroscopy and thermogravimetric analysis show that about 60% nanotubes in the starting material are transferred into liquid phase and the carbonaceous purity reaches as high as 129% of a reference sample R2, an 'impurity-free' fragment of soot directly from the arc chamber. q

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Chromatographic Purification and Properties of Soluble Single-Walled Carbon Nanotubes

Cited by 129 publications

References 22 publications

Room Temperature Purification of Few-Walled Carbon Nanotubes with High Yield

Room Temperature Purification of Few-Walled Carbon Nanotubes with High Yield

Purification of single-walled carbon nanotubes

Centrifugal purification of chemically modified single-walled carbon nanotubes

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