AVS 57th International Symposium & Exhibition
    Energy Frontiers Topical Conference Thursday Sessions
       Session EN+AS-ThM

Paper EN+AS-ThM10
Quantification of Hydrogen and Deuterium in Niobium and Niobium Oxide

Thursday, October 21, 2010, 11:00 am, Room Pecos

Session: Surface and Interface Analysis of Materials for Energy
Presenter: F.A. Stevie, North Carolina State University
Authors: P. Maheshwari, North Carolina State University
F.A. Stevie, North Carolina State University
G.R. Myneni, Jefferson Lab
G. Ciovati, Jefferson Lab
M. Rigsbee, North Carolina State University
D.P. Griffis, North Carolina State University
Correspondent: Click to Email

Superconducting Radio Frequency (SRF) cavities provide enhanced efficiency and reduced energy utilization in present day particle accelerators. Niobium (Nb) is the material of choice for these cavities due to its high critical temperature and critical magnetic field. In order to understand why certain treatments, especially a low temperature bake, improve performance, it is important to study Nb surface characteristics and identify elemental contamination that can affect the performance of the cavity. H, C, O, and N are of interest because they are interstitial impurities in Nb. In earlier work,[1] SIMS analysis using a CAMECA IMS-6F with Cs+ primary beam showed that C and N were probably not significant factors impacting performance and that there was a very high level of H in the Nb. TEM analysis also showed that the surface niobium oxide was a uniform layer with typical thickness about 6nm. Ion implants of C, N, O, and D into Nb provided quantification of C, N, O and indicated that D is very mobile in the Nb.[2]
 Analysis of samples before and after heat treatment showed that the H level could be dramatically reduced after certain heat treatments. Removal of the oxide with HF caused the H to return to its former level and the native oxide was again established. SIMS measurement of H in the niobium oxide showed a low H level and, as noted above, the oxide appears to be a very effective H barrier. One possible cause for the removal of H by low temperature heat treatment is the possible formation of openings in the oxide barrier which allows the hydrogen to exit the Nb surface, followed by the renewal of the oxide after heat treatment which does not allow H to re-enter. Another theory is that the heat treatments drive the H deeply into the Nb.
 In order to better understand the role of the niobium oxide, implants have now been made into a specially prepared 120nm thick niobium oxide layer on Nb substrate. H is shown to have an implant shape in the oxide and verify that H is not mobile in the oxide. An implant of D with peak at the oxide/Nb interface showed an implant shape up to the interface and a sharp drop once the Nb was reached. If the H relative sensitivity factor from the oxide is used to quantify the H in a Nb sample without heat treatment, the H concentration is measured as 2E22atoms/cm3.
 
[1] A. D. Batchelor, D. N. Leonard, P. E. Russell, F. A. Stevie, D. P. Griffis, G. R. Myneni, Proceedings of Single Crystal Niobium Technology Workshop, Brazil, AIP Conference Proceedings, Melville, NY (2007) 72-83.
[2] P. Maheshwari, H. Tian, C. Reece, G. Myneni, F. Stevie. M. Rigsbee, A. Batchelor, D. Griffis, Surf. Int. Anal. (in press 2010)