1 SIMS Characterization of Impurity Elements in Nb: The Effect of Heat Treatments ncsu.edu/aif jlab.org 1 P. Maheshwari, F. Stevie, D. Griffis, M. Rigsbee.

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1 SIMS Characterization of Impurity Elements in Nb: The Effect of Heat Treatments ncsu.edu/aif jlab.org 1 P. Maheshwari, F. Stevie, D. Griffis, M. Rigsbee North Carolina State University G. Myneni, G. Ciovati Jefferson Laboratory

2 ncsu.edu/aif jlab.org 2 Large grain sample Secondary Ion Mass Spectrometry (SIMS) Escape depth of sputtered species only few Angstroms All elements and isotopes measurable (including H) ppm to ppb detection limit nm depth resolution typical, 1-2nm at low energies R. G. Wilson, F. A. Stevie, C. W. Magee: Secondary Ion Mass Spectrometry, Wiley-Interscience (1989)

3 ncsu.edu/aif jlab.org 3 1. Effect of High Temperature HT 800 o C/3hrs, 120 o C/12hrs 1200 o C/6hrs 800 o C/3hrs, 400 o C/20min Control H levels decrease up to a factor of 100, believed to be responsible for improvement in Q o (~45% at 90 mT, 2.0 K, 1.5 GHz); Insignificant changes in O, C and N levels

4 ncsu.edu/aif jlab.org 4 No heat treatment (Control) Intense hydride peaks observed in the mass spectra of a non heat treated sample; greatly reduced after high temperature heat treatment After 800 o C/3hrs, 400 o C /20min heat treatment SIMS measurements at 14.5 keV impact energy with Cs + NbH 5 - NbH 4 - NbH 3 - NbH 2 - Nb - NbH - Nb - NbH 2 - NbH - 1. Effect of High Temperature on Nb Hydrides

5 ncsu.edu/aif jlab.org 5 2. Effect of Baking Some change in H, Some diffusion of O in Nb (first 60nm), Reduction in Q-drop might be related to impurities? SIMS Analysis 6 keV Cs + (Low Energy) 120 o C/48hrs Control O Concentration after 120 o C/48 hrs HT H Levels after 120 o C/48 hrs HT H - /Nb - Ratio 120 o C/48hrs Control

6 ncsu.edu/aif jlab.org 6 3. O and Ti diffusion in Nb for HT >1000 o C O diffuses to the surface of Nb above 1000 o C in the presence of Ti Conc. (atoms/cm 3 ) 1400 o C/3hrs 1200 o C/2hrs,120 o C/12hrs O concentration in Nb Conc. (atoms/cm 3 ) 1400 o C/3hrs 1200 o C/2hrs,120 o C/12hrs Ti concentration in Nb SIMS measurements: 14.5 keV impact energy with Cs + SIMS measurements: 5.5 keV impact energy with O 2 +

7 4. Impurities in Grain Boundaries of LG Nb No segregation of H at grain boundary Segregation of C at grain boundary Grain Boundary of Bicrystal TOF SIMS Analysis using 25 keV Bi 3+ after sputtering for 3 min with 10 keV Cs o C/3hrs, 120 o C/24hrs Control

8 ncsu.edu/aif jlab.org 8 5. Quantification of H in Nb using Nb 2 O 5 Oxide acts as a passivation layer on the Nb surface; anodization of a control sample used to create a layer, about 150nm in thickness D and H implanted into the oxide to create SIMS standards Peaks observed for H, D in Niobium Oxide H increases as Oxide-Nb interface reached D implanted to place peak at Nb oxide/Nb interface SIMS measurements at 6 keV impact energy with Cs + Oxide Substrate

9 ncsu.edu/aif jlab.org 9 5. Estimate of H in Nb SIMS measurements at 6 keV impact energy with Cs + Matrix signal similar in oxide and in Nb, can use RSF from oxide to quantify H in Nb H concentration estimated to be 2e22 atoms/cm 3 ≈ 37 % atomic H on a control Nb sample surface 2E22 at./cm 3 Since the Nb secondary ion intensity shows little change between oxide and substrate, an estimate of H in Nb can be made using the RSF derived by taking Niobium Oxide implant as standard

10 Low Energy SIMS Analysis 6 keV Cs + ; Ti : 1.25 keV O o C/3hrs,120 o C/12hrs SRF cavity had record Q 0 of 4.6  at 90 mT, 2.0 K, 1.5 GHz ( Yesterday’s talk by P. Dhakal ) H - /Nb - Ratio Control 1400 o C/3hrs,120 o C/12hrs H - /Nb - Ratio Conc. (at/cm 3 )

Corroborated by NRA Analysis Control 800 o C/2hrs, 120 o C/24hrs Courtesy : Pacific Northwest National Lab., USA

Conclusions H seen to influence cavity performance, cavity efficiency increases by an average of 40% after heat treatment, possibly due to the reduction of H. H concentrations of ~40 at.% in BCP-treated Nb samples have been estimated by SIMS. H depth profiling is limited by matrix effect and high diffusion rate C segregation at grain boundaries was found by TOF-SIMS after heat treatment at 800 °C Significant concentrations (> 1 at.%) of Ti,O and low H levels were found in sample heat treated at 1400 °C (cavity with record Q 0 )