Tribology Letters

, 44:99 | Cite as

Near-Edge X-ray Absorption Fine Structure Imaging of Spherical and Flat Counterfaces of Ultrananocrystalline Diamond Tribological Contacts: A Correlation of Surface Chemistry and Friction

  • A. R. Konicek
  • C. Jaye
  • M. A. Hamilton
  • W. G. Sawyer
  • D. A. Fischer
  • R. W. Carpick
Methods Paper


A recently installed synchrotron radiation near-edge X-ray absorption fine structure (NEXAFS) full field imaging electron spectrometer was used to spatially resolve the chemical changes of both counterfaces from an ultra- nanocrystalline diamond (UNCD) tribological contact. A silicon flat and Si3N4 sphere were both coated with UNCD, and employed to form two wear tracks on the flat in a linear reciprocating tribometer. The first wear track was produced using a new, unconditioned sphere whose surface was thus conditioned during this first experiment. This led to faster run-in and lower friction when producing a second wear track using the conditioned sphere. The large depth of field of the magnetically guided NEXAFS imaging detector enabled rapid, large area spectromicroscopic imaging of both the spherical and flat surfaces. Laterally resolved NEXAFS data from the tribological contact area revealed that both substrates had an as-grown surface layer that contained a higher fraction of sp2-bonded carbon and oxygen which was mechanically removed. Unlike the flat, the film on the sphere showed evidence of having graphitic character, both before and after sliding. These results show that the graphitic character of the sphere is not solely responsible for low friction and short run-in. Rather, conditioning the sphere, likely by removing asperities and passivating dangling bonds, leads to lower friction with less chemical modification of the substrate in subsequent tests. The new NEXAFS imaging spectroscopy detector enabled a more complete understanding of the tribological phenomena by imaging, for the first time, the surface chemistry of the spherical counterface which had been in continual contact during wear track formation.


Friction mechanisms Solid lubrication friction Spectroscopy Humidity Diamond Carbon Solid lubrication mechanisms Solid lubrication wear Coatings NEXAFS 



Funding was provided by Air Force grant FA9550-08-1-0024. This study was partially supported by the Nano/Bio Interface Center through the National Science Foundation NSEC DMR08-32802. Use of the Center for Nanoscale Materials was supported by the U.S. Department of Energy, Office of Science, Office of Basic Energy Sciences, under Contract No. DE-AC02-06CH11357. Use of the NSLS, Brookhaven National Laboratory, was supported by the U.S. Department of Energy, Office of Science, Office of Basic Energy Sciences, under Contract No. DE-AC02-98CH10886. The LARIAT was developed by Synchrotron Research, Inc. under NIST SBIR funding/Contract No. SB1341-04-C-0021. Certain commercial names are mentioned in this manuscript for purpose of example; this does not constitute an endorsement by the National Institute of Standards and Technology. The authors thank E. Principe for a critical reading of the manuscript. The authors gratefully acknowledge Dr. A.V. Sumant for coating flats and spheres with UNCD.


  1. 1.
    Espinosa, H.D., Peng, B., Prorok, B.C., Moldovan, N., Auciello, O., Carlisle, J.A., Gruen, D.M., Mancini, D.C.: Fracture strength of ultrananocrystalline diamond thin films-Identification of weibull parameters. J. Appl. Phys. 94, 6076–6084 (2003)CrossRefGoogle Scholar
  2. 2.
    Espinosa, H.D., Prorok, B.C., Peng, B., Kim, K.H., Moldovan, N., Auciello, O., Carlisle, J.A., Gruen, D.M., Mancini, D.C.: Mechanical properties of ultrananocrystalline diamond thin films relevant to MEMS/NEMS devices. Exp. Mech. 43, 256–268 (2003)CrossRefGoogle Scholar
  3. 3.
    Konicek, A.R., Grierson, D.S., Gilbert, P.U.P.A., Sawyer, W.G., Sumant, A.V., Carpick, R.W.: Origin of ultralow friction and wear in ultrananocrystalline diamond. Phys. Rev. Lett. 100, 235502 (2008)CrossRefGoogle Scholar
  4. 4.
    Hamilton, M. A., Konicek, A. R., Grierson, D. S., Sumant, A. V., Auciello, O., Sawyer, W. G.,Carpick, R. W.: Environmental performance limits of ultrananocrystalline diamond films. In: Proceedings of the STLE/ASME International Joint Tribology Conference, vols. 9–10 (2009)Google Scholar
  5. 5.
    Auciello, O., et al.: Are diamonds a MEMS’ best friend? IEEE. Microw. Mag. 8, 61–75 (2007)CrossRefGoogle Scholar
  6. 6.
    Sumant, A.V., Grierson, D.S., Gerbi, J.E., Birrell, J., Lanke, U.D., Auciello, O., Carlisle, J.A., Carpick, R.W.: Toward the ultimate tribological interface: surface chemistry and nanotribology of ultrananocrystalline diamond. Adv. Mater. 17, 1039–1045 (2005)CrossRefGoogle Scholar
  7. 7.
    Sumant, A.V., Grierson, D.S., Gerbi, J.E., Carlisle, J.A., Auciello, O., Carpick, R.W.: Surface chemistry and bonding configuration of ultrananocrystalline diamond surfaces and their effects on nanotribological properties. Phys. Rev. B 76, 235429 (2007)CrossRefGoogle Scholar
  8. 8.
    Kim, H.I., Lince, J.R., Eryilmaz, O.L., Erdemir, A.: Environmental effects on the friction of hydrogenated DLC films. Tribol. Lett. 21, 53–58 (2006)CrossRefGoogle Scholar
  9. 9.
    Eryilmaz, O.L., Erdemir, A.: On the hydrogen lubrication mechanism(s) of DLC films: an imaging TOF–SIMS study. Surf. Coat. Technol. 203, 750–755 (2008)CrossRefGoogle Scholar
  10. 10.
    Chromik, R.R., Winfrey, A.L., Luning, J., Nemanich, R.J., Wahl, K.J.: Run-in behavior of nanocrystalline diamond coatings studied by in situ tribometry. Wear 265, 477–489 (2008)CrossRefGoogle Scholar
  11. 11.
    Anders, S., Stammler, T., Fong, W., Bogy, D.B., Bhatia, C.S., Stohr, J.: Investigation of slider surfaces after wear using photoemission electron microscopy. J. Vac. Sci. Technol. A 17, 2731–2736 (1999)CrossRefGoogle Scholar
  12. 12.
    Anders, S., Stammler, T., Fong, W., Chen, C.-Y., Bogy, D.B., Bhatia, C.S., Stohr, J.: Study of tribochemical processes on hard disks using photoemission electron microscopy. J. Tribol-Trans. ASME. 121, 961–967 (1999)CrossRefGoogle Scholar
  13. 13.
    Canning, G.W., Fuller, M.L.S., Bancroft, G.M., Kasrai, M., Cutler, J.N., De Stasio, G., Gilbert, B.: Spectromicroscopy of tribological films from engine oil additives. Part I. Films from ZDDP’s. Tribol. Lett. 6, 159–169 (1999)CrossRefGoogle Scholar
  14. 14.
    Grierson, D.S., et al.: Tribochemistry and material transfer for the ultrananocrystalline diamond-silicon nitride interface revealed by X-ray photoelectron emission spectromicroscopy. J. Vac. Sci. Technol. B 25, 1700–1705 (2007)CrossRefGoogle Scholar
  15. 15.
    Sumant, A.V., Auciello, O., Yuan, H.C., Ma, Z., Carpick, R.W., Mancini, D.C.: Large-area low-temperature ultrananocrystalline diamond (UNCD) films and integration with CMOS devices for monolithically integrated diamond MEMS/NEMS-CMOS systems. Proc. SPIE-Int. Soc. Opt. Eng. 7318, 731817 (2009)Google Scholar
  16. 16.
    Rennie, A.C., Dickrell, P.L., Sawyer, W.G.: Friction coefficient of soft contact lenses: measurements and modeling. Tribol. Lett. 18, 499–504 (2005)CrossRefGoogle Scholar
  17. 17.
    Hayward, I.P., Singer, I.L., Seitzman, L.E.: Effect of roughness on the friction of diamond on CVD diamond coatings. Wear 157, 215–227 (1992)CrossRefGoogle Scholar
  18. 18.
    Gago, R., Vinnichenko, M., Jager, H.U., Belov, A.Y., Jimenez, I., Huang, N., Sun, H., Maitz, M.F.: Evolution of sp2 networks with substrate temperature in amorphous carbon films: experiment and theory. Phys. Rev. B 72, 14120–14121 (2005)CrossRefGoogle Scholar
  19. 19.
    Gago, R., Jimenez, I., Albella, J.M.: Detecting with X-ray absorption spectroscopy the modifications of the bonding structure of graphitic carbon by amorphisation, hydrogenation and nitrogenation. Surf. Sci. 482–485, 530–536 (2001)CrossRefGoogle Scholar
  20. 20.
    Osswald, S., Yushin, G., Mochalin, V., Kucheyev, S.O., Gogotsi, Y.: Control of sp2/sp3 carbon ratio and surface chemistry of nanodiamond powders by selective oxidation in air. J. Am. Chem. Soc. 128, 11635–11642 (2006)CrossRefGoogle Scholar
  21. 21.
    Coffman, F.L., Cao, R., Pianetta, P.A., Kapoor, S., Kelly, M., Terminello, L.J.: Near-edge X-ray absorption of carbon materials for determining bond hybridization in mixed sp 2/sp 3 bonded materials. Appl. Phys. Lett. 69, 568–570 (1996)CrossRefGoogle Scholar
  22. 22.
    Stohr, J.: NEXAFS Spectroscopy. Springer-Verlag, Berlin (1992)Google Scholar
  23. 23.
    Jaouen, M., Tourillon, G., Delafond, J., Junqua, N., Hug, G.: A NEXAFS characterization of ion-beam-assisted carbon-sputtered thin films. Diam. Relat. Mater. 4, 200–206 (1995)CrossRefGoogle Scholar
  24. 24.
    Ishii, I., Hitchcock, A.P.: The oscillator strengths for C1 s and O1 s excitation of some saturated and unsaturated organic alcohols, acids and esters. J. Electron. Spectrosc. 46, 55–84 (1988)CrossRefGoogle Scholar

Copyright information

© Springer Science+Business Media, LLC 2011

Authors and Affiliations

  • A. R. Konicek
    • 1
    • 5
  • C. Jaye
    • 2
  • M. A. Hamilton
    • 3
    • 6
  • W. G. Sawyer
    • 4
  • D. A. Fischer
    • 2
  • R. W. Carpick
    • 3
  1. 1.Physics & Astronomy DepartmentUniversity of PennsylvaniaPhiladelphiaUSA
  2. 2.Material Measurement LaboratoryNational Institute of Standards and TechnologyGaithersburgUSA
  3. 3.Department of Mechanical Engineering and Applied MechanicsUniversity of PennsylvaniaPhiladelphiaUSA
  4. 4.Mechanical and Aerospace Engineering DepartmentUniversity of FloridaGainesvilleUSA
  5. 5.National Institute of Standards and Technology (NIST)GaithersburgUSA
  6. 6.Exactech, IncGainesvilleUSA

Personalised recommendations