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Analysis of furnace contamination on superconducting radio frequency niobium using secondary-ion mass spectrometry
Abstract
Detection of surface contamination on niobium materials used in superconducting radio frequency (SRF) applications is difficult due to quantitative sensitivity and near-atomic depth resolution needed. Inspection of samples known to have experienced surface contamination was found to have inconsistent nitride coverage after high-temperature nitrogen gas exposure (“doping”). Here we compare contaminating species found on samples treated in several different vacuum furnaces, both “exposed” directly in the chamber and “protected” by containment shielding from evaporative sources with “furnace caps.” Typically, furnace caps are used to impede contamination from reaching the interior surface of cavities during the high-temperature vacuum bake that immediately precedes exposure to nitrogen gas. Although, to date, little is known about the effectiveness of these caps, SIMS results showed that they were effective in limiting contamination arising from the furnace environment. Inspection of sample surfaces by SEM showed a lack of nitrides present on contaminated specimens. TEM with energy dispersive spectroscopy performed on these samples revealed that a carbon-rich layer now existed, indicating that a relatively high contaminant load prevents the nucleation and growth of surface nitrides, while thus inhibiting interstitial nitrogen uptake. Except in extreme cases, subsequent removal of the top several micrometers of the surface via electropolishingmore »
- Authors:
-
[1];
[2];
[2];
[4]
- Virginia Polytechnic Institute and State University (Virginia Tech), Blacksburg, VA (United States)
- Thomas Jefferson National Accelerator Facility (TJNAF), Newport News, VA (United States)
- North Carolina State University, Raleigh, NC (United States)
- Virginia Polytechnic Institute and State University (Virginia Tech), Blacksburg, VA (United States); Thomas Jefferson National Accelerator Facility (TJNAF), Newport News, VA (United States)
- Publication Date:
- Research Org.:
- Thomas Jefferson National Accelerator Facility (TJNAF), Newport News, VA (United States)
- Sponsoring Org.:
- USDOE Office of Science (SC), Nuclear Physics (NP); National Science Foundation (NSF); USDOE Office of Science (SC), High Energy Physics (HEP)
- OSTI Identifier:
- 1973378
- Report Number(s):
- JLAB-ACC-23-3752; DOE/OR/23177-5709
Journal ID: ISSN 2166-2746; TRN: US2313889
- Grant/Contract Number:
- AC05-06OR23177; ECCS 1542100; ECCS 2025151; SC0014475
- Resource Type:
- Accepted Manuscript
- Journal Name:
- Journal of Vacuum Science and Technology B
- Additional Journal Information:
- Journal Volume: 41; Journal Issue: 3; Journal ID: ISSN 2166-2746
- Publisher:
- American Vacuum Society / AIP
- Country of Publication:
- United States
- Language:
- English
- Subject:
- 75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND SUPERFLUIDITY; superconductivity; focused ion beam; scanning electron microscopy; secondary ion mass spectrometry; depth profiling techniques; electron backscatter diffraction
Citation Formats
Angle, Jonathan W., Lechner, Eric M., Reece, Charles E., Stevie, Fred A., and Kelley, Michael J. Analysis of furnace contamination on superconducting radio frequency niobium using secondary-ion mass spectrometry. United States: N. p., 2023.
Web. doi:10.1116/6.0002624.
Angle, Jonathan W., Lechner, Eric M., Reece, Charles E., Stevie, Fred A., & Kelley, Michael J. Analysis of furnace contamination on superconducting radio frequency niobium using secondary-ion mass spectrometry. United States. https://doi.org/10.1116/6.0002624
Angle, Jonathan W., Lechner, Eric M., Reece, Charles E., Stevie, Fred A., and Kelley, Michael J. Fri .
"Analysis of furnace contamination on superconducting radio frequency niobium using secondary-ion mass spectrometry". United States. https://doi.org/10.1116/6.0002624.
@article{osti_1973378,
title = {Analysis of furnace contamination on superconducting radio frequency niobium using secondary-ion mass spectrometry},
author = {Angle, Jonathan W. and Lechner, Eric M. and Reece, Charles E. and Stevie, Fred A. and Kelley, Michael J.},
abstractNote = {Detection of surface contamination on niobium materials used in superconducting radio frequency (SRF) applications is difficult due to quantitative sensitivity and near-atomic depth resolution needed. Inspection of samples known to have experienced surface contamination was found to have inconsistent nitride coverage after high-temperature nitrogen gas exposure (“doping”). Here we compare contaminating species found on samples treated in several different vacuum furnaces, both “exposed” directly in the chamber and “protected” by containment shielding from evaporative sources with “furnace caps.” Typically, furnace caps are used to impede contamination from reaching the interior surface of cavities during the high-temperature vacuum bake that immediately precedes exposure to nitrogen gas. Although, to date, little is known about the effectiveness of these caps, SIMS results showed that they were effective in limiting contamination arising from the furnace environment. Inspection of sample surfaces by SEM showed a lack of nitrides present on contaminated specimens. TEM with energy dispersive spectroscopy performed on these samples revealed that a carbon-rich layer now existed, indicating that a relatively high contaminant load prevents the nucleation and growth of surface nitrides, while thus inhibiting interstitial nitrogen uptake. Except in extreme cases, subsequent removal of the top several micrometers of the surface via electropolishing appears to effectively eliminate any strong influence on the subsequent SRF cavity performance. With the absence of furnace cleaning, carbon contamination was found to be nearly 10× higher for protected nitrogen-doped and electropolished samples, with minimal metallic contamination detected for both processes. SIMS analysis was also performed to compare the cleanliness of samples fully prepared by such nitrogen “doping” with those prepared by a related process, involving the dissolution of niobium surface oxide and diffusion of oxygen into the surface. This oxygen doping or alloying process offers attractive advantages.},
doi = {10.1116/6.0002624},
journal = {Journal of Vacuum Science and Technology B},
number = 3,
volume = 41,
place = {United States},
year = {Fri May 12 00:00:00 EDT 2023},
month = {Fri May 12 00:00:00 EDT 2023}
}
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