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Analysis and applications for carbon nanomaterials

Chemical speciation

The XP survey scan is an effective way to determine the identity of elements present on the surface of a material, as well as the approximate relative ratios of the elements detected. This has important implications for carbon nanomaterials, in which surface composition is of greatest importance in their uses. XPS may be used to determine the purity of a material. For example, nanodiamond powder is a created by detonation, which can leave nitrogenous groups and various oxygen containing groups attached to the surface. [link] shows a survey scan of a nanodiamond thin film with the relative atomic percentages of carbon, oxygen, and nitrogen being 91.25%, 6.25%, and 1.7%, respectively. Based on the XPS data, the nanodiamond material is approximately 91.25% pure.

Survey XPS of a nanodiamond thin film. Adapted from F. Y. Xie, W. G. Xie, J. Chen, X. Liu, D. Y. Lu, and W. H. Zhang, J. Vac. Sci. Tech. B , 2008, 26 , 102.

XPS is a useful method to verify the efficacy of a purification process. For example, high-pressure CO conversion single-walled nanotubes (HiPco SWNTs) are made using iron as a catalyst. [link] shows the Fe2p XP spectra for pristine and purified HiPco SWNTs.

High resolution scan of Fe2p peak for pristine and purified HiPco SWNTs. Adapted with permission from C. M. Yang, H. Kanoh, K. Kaneko, M. Yudasaka, and S. Iijima, J. Phys. Chem. B , 2002, 106 , 8994. Copyright: American Chemical Society (2002).

For this application, XPS is often done in conjunction with thermogravimetric analysis (TGA), which measures the weight lost from a sample at increasing temperatures. TGA data serves to corroborate the changes observed with the XPS data by comparing the percentage of weight loss around the region of the impurity suspected based on the XP spectra. The TGA data support the reduction in iron content with purification suggested by the XP spectra above, for the weight loss at temperatures consistent with iron loss decreases from 27% in pristine SWNTs to 18% in purified SWNTs. Additionally, XPS can provide information about the nature of the impurity. In [link] , the Fe2p spectrum for pristine HiPco SWNTs shows two peaks characteristic of metallic iron at 707 and 720 eV. In contrast, the Fe2p spectrum for purified HiPco SWNTs also shows two peaks at 711 and 724 eV, which are characteristic of either Fe 2 O 3 or Fe 3 O 4 . In general, the atomic percentage of carbon obtained from the XPS spectrum is a measure of the purity of the carbon nanomaterials.

Bonding and functional groups

XP spectra give evidence of functionalization and can provide insight into the identity of the functional groups. Carbon nanomaterials provide a versatile surface which can be functionalized to modulate their properties. For example, the sodium salt of phenyl sulfonated SWNTs is water soluble. In the XP survey scan of the phenyl sulfonated SWNTs, there is evidence of functionalization owing to the appearance of the S2p peak. [link] shows the survey XP spectrum of phenyl sulfonated SWNTs.

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Source:  OpenStax, Carbon nanotubes. OpenStax CNX. Sep 30, 2013 Download for free at http://cnx.org/content/col11576/1.1
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