Analytical and Bioanalytical Chemistry

, Volume 383, Issue 1, pp 41–47 | Cite as

Soft X-ray scanning transmission X-ray microscopy (STXM) of actinide particles

  • Hans J. Nilsson
  • Tolek Tyliszczak
  • Richard E. Wilson
  • Lars Werme
  • David K. Shuh
Original Paper


A descriptive account is given of our most recent research on the actinide dioxides with the Advanced Light Source Molecular Environmental Science (ALS-MES) Beamline 11.0.2 soft X-ray scanning transmission X-ray microscope (STXM) at the Lawrence Berkeley National Laboratory (LBNL). The ALS-MES STXM permits near-edge X-ray absorption fine structure (NEXAFS) and imaging with 30-nm spatial resolution. The first STXM spectromicroscopy NEXAFS spectra at the actinide 4d5/2 edges of the imaged transuranic particles, NpO2 and PuO2, have been obtained. Radiation damage induced by the STXM was observed in the investigation of a mixed oxidation state particle (Np(V,VI)) and was minimized during collection of the actual spectra at the 4d5/2 edge of the Np(V,VI) solid. A plutonium elemental map was obtained from an irregular PuO2 particle with the dimensions of 650 × 650 nm. The Pu 4d5/2 NEXAFS spectra were collected at several different locations from the PuO2 particle and were identical. A representative oxygen K-edge spectrum from UO2 was collected and resembles the oxygen K-edge from the bulk material. The unique and current performance of the ALS-MES STXM at extremely low energies (ca. 100 eV) that may permit the successful measurement of the actinide 5d edge is documented. Finally, the potential of STXM as a tool for actinide investigations is briefly discussed.


Actinide STXM NEXAFS Spectromicroscopy Plutonium Neptunium 


  1. 1.
    Denlinger JD, Rotenberg E, Warwick T, Visser G, Nordgren J, Guo J-H, Skytt P, Kevan SD, McCutcheon KS, Tobin JG, Shuh DK, Bucher JJ, Edelstein NM, Tonner BP (1995) Rev Sci Instrum 66:1342–1345CrossRefGoogle Scholar
  2. 2.
    Terry J, Schulze RK, Lashley J, Farr JD, Zocco T, Heinzelman K, Rotenberg E, Shuh DK, Van der Laan G, Tobin JG (2002) Surf Sci 499:L141–L147CrossRefGoogle Scholar
  3. 3.
    Tobin JG, Chung BW, Wadddill GD, Schulze RK, Terry J, Farr JD, Zocco T, Shuh DK, Heinzelman K, Rotenberg E, Van der Laan G (2003) Phys Rev B 68:155109CrossRefGoogle Scholar
  4. 4.
    Moore KT, Wall MA, Schwartz AJ, Chung BW, Shuh DK, Schulze RK, Tobin JG, (2003) Phys Rev Lett 90:196064CrossRefGoogle Scholar
  5. 5.
    Shuh DK, Butorin SM, Guo J-H, Nordgren J (2004) Mater Res Soc Symp Proc 802:131–136Google Scholar
  6. 6.
    Bluhm H, Andersson K, Araki T, Benzerara K, Brown GE Jr, Dynes JJ, Ghosal S, Hansen H-Ch, Hemminger JC, Hitchcock AP, Ketteler G, Kneedler E, Lawrence JR, Leppard GG, Majzlam J, Mun BS, Myneni SCB, Nilsson A, Ogasawara H, Ogletree DF, Pecher K, Shuh DK, Salmeron M, Tonner B, Tyliszczak T, Yoon TH (2005) J Electron Spectr (in press)Google Scholar
  7. 7.
    Sharmasarkar S, Traina SJ, Tyliszczak T, Nilsson HJ, Shuh DK, in preparation (2005)Google Scholar
  8. 8.
    Stohr J (1992) NEXAFS spectroscopy. Springer series in surface science 25, Springer-Verlag, Berlin Heidelberg New YorkGoogle Scholar
  9. 9.
    Kilcoyne ALD, Tyliszczak T, Steele WF, Fakra S, Hitchcock P, Franck K, Anderson E, Harteneck B, Rightor EG, Mitchell GE, Hitchcock AP, Yang L, Warwick T, Ade H (2003) J Synch Rad 10:125CrossRefGoogle Scholar
  10. 10.
    Coonley MS (2004) (ed) Actinide oxides I and II. Actinide research quarterly 2 and 3, Nucl Mat Tech Div, Los Alamos National Laboratory, Los Alamos, NM, USAGoogle Scholar
  11. 11.
    Wu ZY, Jollet F, Gota S, Thromat N, Gautier-Soyer M, Petit T (1999) J Phys Condens Matter 11:7185–7194CrossRefGoogle Scholar
  12. 12.
    Tyliszczak T, Warwick T, Kilcoyne ALD, Fakra S, Shuh DK, Yoon TH, Brown GE Jr, Andrews S, Chembrolu V, Strachan J, Acremann Y (2004) Synch Rad Instrum 2003. AIP Conf Proc 705:1356–1359CrossRefGoogle Scholar
  13. 13.
    Kilcoyne ALD, Tyliszczak T (2004) Synch Rad Instrum 2003. AIP Conf Proc 705:605–607CrossRefGoogle Scholar
  14. 14.
    Harteneck BD, Olynick DL, Veklerov E, Tendulkar M, Liddle JA, Kilcoyne ALD, Tyliszczak T (2004) J Vac Sci Technol B 22:3186–3190CrossRefGoogle Scholar
  15. 15.
    Advanced Light Source Molecular Science Beamline Webpages, LBN L, Berkeley, CA, (2005);;
  16. 16.
    Hitchcock AP (2004) Axis Version 21q (09-June-04). McMaster University, Hamilton ON CanadaGoogle Scholar
  17. 17.
    Browne E, Firestone RB (1986) In: Shirley VS (ed) Table of radioactive isotopes. Wiley, New York, pp C14–C16Google Scholar
  18. 18.
    Center for X-ray optics, X-ray Interactions with Matter, LBNL, Berkeley, CA, USA;
  19. 19.
    Kalkowski G, Kaindl G, Brewer WD, Krone W (1987) Phys Rev B 35:2667–2677CrossRefGoogle Scholar
  20. 20.
    Van der Laan G, Moore KT, Tobin JG, Chung BW, Wall MA, Schwartz AJ (2004) Phys Rev Lett 93:097401CrossRefPubMedGoogle Scholar
  21. 21.
    de Groot FMF (1991) PhD Thesis, X-ray absorption of transition metal oxides. University of Nijmegen, Nijmegen, The NetherlandsGoogle Scholar
  22. 22.
    Conradson SD, Abney KD, Begg BD, Brady ED, Clark DL, den Awer C, Ding M, Dorhout PK, Espinosa-Faller FJ, Gordon PJ, Haire RJ, Hess NJ, Hess RF, Keough DW, Lander GH, Lupinetti AJ, Morales LA, Neu MP, Palmer PD, Paviet-Hartmann P, Reilly SD, Runde WH, Tait CD, Veirs DK, Wastin F (2004) Inorg Chem 43:116–131CrossRefPubMedGoogle Scholar
  23. 23.
    Tyliszczak T, Nilsson HJ, Nachimuthu P, Shuh DK (2005) unpublished experimental resultsGoogle Scholar
  24. 24.
    Jollet F, Petit T, Gota S, Thromat N, Gautier-Soyer M, Pasturel A (1997) J Phys Condens Matter 9:9393–9401CrossRefGoogle Scholar
  25. 25.
    Buck EC, Colella M, Smith KL, Lumpkin GR (2002) Mat Res Soc Symp Proc 713:655–662Google Scholar

Copyright information

© Springer-Verlag 2005

Authors and Affiliations

  • Hans J. Nilsson
    • 1
    • 2
  • Tolek Tyliszczak
    • 1
  • Richard E. Wilson
    • 1
    • 3
  • Lars Werme
    • 2
    • 4
  • David K. Shuh
    • 1
  1. 1.The Glenn T. Seaborg Center, Chemical Sciences DivisionLawrence Berkeley National LaboratoryBerkeleyUSA
  2. 2.SKBStockholmSweden
  3. 3.Nuclear Sciences DivisionLawrence Berkeley National LaboratoryBerkeleyUSA
  4. 4.Department of PhysicsUppsala UniversityUppsalaSweden

Personalised recommendations