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Survey XP spectrum of F-DWNTs (O. Kuznetsov, Rice University).

Subsequently, high resolution scans of the peaks can be obtained to give more information. Elements of the same kind in different states and environments have slightly different characteristic binding energies. Computer software is used to fit peaks within the elemental peak which represent different states of the same element, commonly called deconvolution of the elemental peak. [link] and [link] show high resolutions scans of C1s and F1s peaks, respectively, from [link] , along with the peak designations.

Deconvoluted high resolution C1s spectrum of F-DWNTs (O. Kuznetsov, Rice University).
Deconvoluted high resolution F1s spectrum of F-DWNTs (O. Kuznetsov, Rice University).

Limitations

Both hydrogen and helium cannot be detected using XPS. For this reason, XPS can provide only relative, rather than absolute, ratios of elements in a sample. Also, elements with relatively low atomic percentages close to that of the detection limit or low detection by XPS may not be seen in the spectrum. Furthermore, each peak represents a distribution of observed binding energies of ejected electrons based on the depth of the atom from which they originate, as well as the state of the atom. Electrons from atoms deeper in the sample must travel through the above layers before being liberated and detected, which reduces their kinetic energies and thus increases their apparent binding energies. The width of the peaks in the spectrum consequently depends on the thickness of the sample and the depth to which the XPS can detect; therefore, the values obtained vary slightly depending on the depth of the atom. Additionally, the depth to which XPS can analyze depends on the element being detected.

High resolution scans of a peak can be used to distinguish among species of the same element. However, the identification of different species is discretionary. Computer programs are used to deconvolute the elemental peak. The peaks may then be assigned to particular species, but the peaks may not correspond with species in the sample. As such, the data obtained must be used cautiously, and care should be taken to avoid over-analyzing data.

Xps for carbon nanomaterials

Despite the aforementioned limitations, XPS is a powerful surface technique that can be used to accurately detect the presence and relative quantities of elements in a sample. Further analysis can provide information about the state and environment of atoms in the sample, which can be used to infer information about the surface structure of the material. This is particularly useful for carbon nanomaterials, in which surface structure and composition greatly influence the properties of the material. There is much research interest in modifying carbon nanomaterials to modulate their properties for use in many different applications.

Sample preparation

Carbon nanomaterials present certain issues in regard to sample preparation. The use of graphite tape is a poor option for carbon nanomaterials because the spectra will show peaks from the graphite tape, adding to the carbon peak and potentially skewing or overwhelming the data. Instead, a thin indium foil (between 0.1 and 0.5 mm thick) is used as the sample substrate. The sample is simply pressed onto a piece of the foil.

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Source:  OpenStax, Nanomaterials and nanotechnology. OpenStax CNX. May 07, 2014 Download for free at http://legacy.cnx.org/content/col10700/1.13
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