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C1s high resolution XP spectra of graphite, nanodiamond, and graphite samples with increasing laser power treatment. Adapted from P. Merel, M. Tabbal, M. Chaker, S. Moisa, and J. Margot, Appl. Surf. Sci. , 1998, 136 , 105.

Alternatively, annealing nanodiamond thin films at very high temperatures creates graphitic layers on the nanodiamond surface, increasing sp 2 content. The extent of graphitization increases with the temperature at which the sample is annealed, as shown in [link] .

Deconvoluted high resolution C1s XP spectra for annealed nanodiamond. 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.

Reaction completion

Comparing the relative intensities of various C1s peaks can be powerful in verifying that a reaction has occurred. Fluorinated carbon materials are often used as precursors to a broad range of variously functionalized materials. Reaction of fluorinated SWNTs (F-SWNTs) with polyethyleneimine (PEI) leads to decreases in the covalent carbon-fluoride C1s peak, as well as the evolution of the amine C1s peak. These changes are observed in the C1s spectra of the two samples ( [link] ).

High resolution C1s XP spectra of F-SWNTs (top) and PEI-SWNTs (bottom). Adapted with permission from E. P. Dillon, C. A. Crouse, and A. R. Barron, ACS Nano , 2008, 2 , 156. Copyright: American Chemical Society (2008).

Nature and extent of functionalization

XPS can also be applied to determine the nature and extent of functionalization. In general, binding energy increases with decreasing electron density about the atom. Species with more positive oxidation states have higher binding energies, while more reduced species experience a greater degree of shielding, thus increasing the ease of electron removal.

The method of fluorination of carbon materials and such factors as temperature and length of fluorination affect the extent of fluoride addition as well as the types of carbon-fluorine bonds present. A survey scan can be used to determine the amount of fluorine compared to carbon. High resolution scans of the C1s and F1s peaks can also give information about the proportion and types of bonds. A shift in the peaks, as well as changes in peak width and intensity, can be observed in spectra as an indication of fluorination of graphite. [link] shows the Cls and F1s spectra of samples containing varying ratios of carbon to fluorine.

C1s and F1s high resolution XP spectra for graphite fluorides. Adapted from I. Palchan, M. Crespin, H. Estrade-Szwarckopf, and B. Rousseau. Chem. Phys. Lett. , 1989, 157 , 321.

Furthermore, different carbon-fluorine bonds show characteristic peaks in high resolution C1s and F1s spectra. The carbon-fluorine interactions in a material can range from ionic to covalent. Covalent carbon-fluorine bonds show higher core electron binding energies than bonds more ionic in character. The method of fluorination affects the nature of the fluorine bonds. Graphite intercalation compounds are characterized by ionic carbon-fluorine bonding. [link] shows the F1s spectra for two fluorinated exfoliated graphite samples prepared with different methods.

High resolution F1s XP spectra of two fluorinated exfoliated graphite samples. Adapted from A. Tressaud, F. Moguet, S. Flandrois, M. Chambon, C. Guimon, G. Nanse, E. Papirer, V. Gupta, and O.P. Bahl. J. Phys. Chem. Solids , 1996, 57 , 745.

Also, the peaks for carbons attached to a single fluorine atom, two fluorine atoms, and carbons attached to fluorines have characteristic binding energies. These peaks are seen in that C1s spectra of F- and PEI-SWNTs shown in [link] .

High resolution C1s XP spectra of F-SWNTs (top) and PEI-SWNTs (bottom). Adapted with permission from E. P. Dillon, C. A. Crouse, and A. R. Barron, ACS Nano , 2008, 2 , 156. Copyright: American Chemical Society (2008).

[link] lists various bonds and functionalities and the corresponding C1s binding energies, which may be useful in assigning peaks in a C1s spectrum, and consequently in characterizing the surface of a material.

Summary of selected C1s binding energies.
Bond/Group Binding Energy (eV)
C-C 284.0-286.0
C-C (sp 2 ) 284.3-284.6
C-C (sp 3 ) 285.0-286.0
C-N 285.2-288.4
C-NR 2 (amine) 285.5-286.4
O=C-NH (amide) 287.9-288.6
-C = N (nitrile) 266.3-266.8
C-O 286.1-290.0
O=C-OH (carboxyl) 288.0-289.4
-C-O (epoxy) 286.1-287.1
-C-OH (hydroxyl) 286.4-286.7
-C-O-C- (ether) 286.1-288.0
-C=O (aldehyde/ketone) 287.1-288.1
C-F 287.0-293.4
-C-F (covalent) 287.7-290.2
-C-F (ionic) 287.0-287.4
C -C-F 286.0-287.7
C-F 2 291.6-292.4
C-F 3 292.4-293.4
C-S 285.2-287.5
C-Cl 287.0-287.2

Conclusion

X-ray photoelectron spectroscopy is a facile and effective method for determining the elemental composition of a material’s surface. As a quantitative method, it gives the relative ratios of detectable elements on the surface of the material. Additional analysis can be done to further elucidate the surface structure. Hybridization, bonding, functionalities, and reaction progress are among the characteristics that can be inferred using XPS. The application of XPS to carbon nanomaterials provides much information about the material, particularly the first few atomic layers, which are most important for the properties and uses of carbon nanomaterials.

Bibliography

  • J. Bockris, Modern Electrochemistry 2A , 2 nd ed., Springer (2001).
  • E. P. Dillon, C. A. Crouse, and A. R. Barron, ACS Nano , 2008, 2 , 156.
  • Y. G. Gogotsi, and I. V. Uvarova, Nanostructured materials and coatings for biomedical and sensor applications, Kluwer Academic Publishing (2003).
  • F. Liang, J. M. Beach, P. K. Rai, W. H. Guo, R. H. Hauge, M. Pasquali, R. E. Smalley, and W. E. Billups, Chem. Mater. , 2006, 18 , 1520.
  • P. Merel, M. Tabbal, M. Chaker, S. Moisa, and J. Margot, Appl. Surf. Sci. , 1998, 136 , 105.
  • T. Nakajima, Graphite fluorides and carbon-fluorine compounds , CRC Press, Boca Raton (1991).
  • I. Palhan, M. Crespin, H. Estrade-Szwarckopf, and B. Rousseau. Chem. Phys. Lett. , 1989, 157 , 321.
  • A. Tressaud, F. Moguet, S. Flandrois, M. Chambon, C. Guimon, G. Nanse, E. Papirer, V. Gupta, and O. P. Bahl. J. Phys. Chem. Solids , 1996, 57 , 745.
  • 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.
  • C. M. Yang, H. Kanoh, K. Kaneko, M. Yudasaka, and S. Iijima, J. Phys. Chem. B , 2002, 106 , 8994.

Questions & Answers

where we get a research paper on Nano chemistry....?
Maira Reply
nanopartical of organic/inorganic / physical chemistry , pdf / thesis / review
Ali
what are the products of Nano chemistry?
Maira Reply
There are lots of products of nano chemistry... Like nano coatings.....carbon fiber.. And lots of others..
learn
Even nanotechnology is pretty much all about chemistry... Its the chemistry on quantum or atomic level
learn
Google
da
no nanotechnology is also a part of physics and maths it requires angle formulas and some pressure regarding concepts
Bhagvanji
hey
Giriraj
Preparation and Applications of Nanomaterial for Drug Delivery
Hafiz Reply
revolt
da
Application of nanotechnology in medicine
what is variations in raman spectra for nanomaterials
Jyoti Reply
I only see partial conversation and what's the question here!
Crow Reply
what about nanotechnology for water purification
RAW Reply
please someone correct me if I'm wrong but I think one can use nanoparticles, specially silver nanoparticles for water treatment.
Damian
yes that's correct
Professor
I think
Professor
Nasa has use it in the 60's, copper as water purification in the moon travel.
Alexandre
nanocopper obvius
Alexandre
what is the stm
Brian Reply
is there industrial application of fullrenes. What is the method to prepare fullrene on large scale.?
Rafiq
industrial application...? mmm I think on the medical side as drug carrier, but you should go deeper on your research, I may be wrong
Damian
How we are making nano material?
LITNING Reply
what is a peer
LITNING Reply
What is meant by 'nano scale'?
LITNING Reply
What is STMs full form?
LITNING
scanning tunneling microscope
Sahil
how nano science is used for hydrophobicity
Santosh
Do u think that Graphene and Fullrene fiber can be used to make Air Plane body structure the lightest and strongest. Rafiq
Rafiq
what is differents between GO and RGO?
Mahi
what is simplest way to understand the applications of nano robots used to detect the cancer affected cell of human body.? How this robot is carried to required site of body cell.? what will be the carrier material and how can be detected that correct delivery of drug is done Rafiq
Rafiq
if virus is killing to make ARTIFICIAL DNA OF GRAPHENE FOR KILLED THE VIRUS .THIS IS OUR ASSUMPTION
Anam
analytical skills graphene is prepared to kill any type viruses .
Anam
Any one who tell me about Preparation and application of Nanomaterial for drug Delivery
Hafiz
what is Nano technology ?
Bob Reply
write examples of Nano molecule?
Bob
The nanotechnology is as new science, to scale nanometric
brayan
nanotechnology is the study, desing, synthesis, manipulation and application of materials and functional systems through control of matter at nanoscale
Damian
Is there any normative that regulates the use of silver nanoparticles?
Damian Reply
what king of growth are you checking .?
Renato
What fields keep nano created devices from performing or assimulating ? Magnetic fields ? Are do they assimilate ?
Stoney Reply
why we need to study biomolecules, molecular biology in nanotechnology?
Adin Reply
?
Kyle
yes I'm doing my masters in nanotechnology, we are being studying all these domains as well..
Adin
why?
Adin
what school?
Kyle
biomolecules are e building blocks of every organics and inorganic materials.
Joe

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