In-situ Synchrotron X-Ray Photoelectron Spectroscopy Study of Medium-Temperature Baking of Niobium for SRF Application

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Main Authors: Prudnikava, Alena, Tamashevich, Yegor, Makarova, Anna, Smirnov, Dmitry, Knobloch, Jens
Format: Preprint
Published: 2023
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author Prudnikava, Alena
Tamashevich, Yegor
Makarova, Anna
Smirnov, Dmitry
Knobloch, Jens
author_facet Prudnikava, Alena
Tamashevich, Yegor
Makarova, Anna
Smirnov, Dmitry
Knobloch, Jens
contents In the present work the chemical composition of niobium surface upon 200-400 °C baking similar to "medium-temperature baking" and "furnace baking" of cavities is explored in-situ by synchrotron X-ray photoelectron spectroscopy (XPS). Our findings imply that below the critical thickness of $Nb_2O_5$ layer (about 1 nm) niobium starts to interact actively with surface impurities, such as carbon and phosphorus. By studying the kinetics of the native oxide reduction, the activation energy and the rate-constant relation have been determined and used for the calculation of the oxygen-concentration depth profiles. It has been established that the controlled diffusion of oxygen when the native-oxide layer represents an oxygen source is realized at temperatures 200-300 °C, while at 400 °C the pentoxide is completely reduced and the doping level is determined by an ambient oxygen partial pressure. Fluorine (F to Nb atomic ratio is about 0.2) after the buffered chemical polishing was found to be incorporated into the surface layer probed by XPS (about 4.6 nm), and its concentration increased during the low-temperature baking (F/Nb up to 0.35 at 230 °C) and depleted at higher temperatures (F/Nb=0.11 at 400 °C). Thus, the influence of fluorine on the performance of mid-T baked, mild-baked (120 °C/48 h) and nitrogen-doped cavities must be considered. The possible role of fluorine in the educed $Nb^{+5}$ to $Nb^{+4}$ reaction under the impact of an X-ray beam at room temperature and during the thermal treatment is also discussed. The range of temperature and duration parameters of the thermal treatment at which the niobium surface would not be contaminated with impurities is determined for industrial applications.
format Preprint
id arxiv_https___arxiv_org_abs_2312_06529
institution arXiv
publishDate 2023
record_format arxiv
spellingShingle In-situ Synchrotron X-Ray Photoelectron Spectroscopy Study of Medium-Temperature Baking of Niobium for SRF Application
Prudnikava, Alena
Tamashevich, Yegor
Makarova, Anna
Smirnov, Dmitry
Knobloch, Jens
Accelerator Physics
Materials Science
Superconductivity
In the present work the chemical composition of niobium surface upon 200-400 °C baking similar to "medium-temperature baking" and "furnace baking" of cavities is explored in-situ by synchrotron X-ray photoelectron spectroscopy (XPS). Our findings imply that below the critical thickness of $Nb_2O_5$ layer (about 1 nm) niobium starts to interact actively with surface impurities, such as carbon and phosphorus. By studying the kinetics of the native oxide reduction, the activation energy and the rate-constant relation have been determined and used for the calculation of the oxygen-concentration depth profiles. It has been established that the controlled diffusion of oxygen when the native-oxide layer represents an oxygen source is realized at temperatures 200-300 °C, while at 400 °C the pentoxide is completely reduced and the doping level is determined by an ambient oxygen partial pressure. Fluorine (F to Nb atomic ratio is about 0.2) after the buffered chemical polishing was found to be incorporated into the surface layer probed by XPS (about 4.6 nm), and its concentration increased during the low-temperature baking (F/Nb up to 0.35 at 230 °C) and depleted at higher temperatures (F/Nb=0.11 at 400 °C). Thus, the influence of fluorine on the performance of mid-T baked, mild-baked (120 °C/48 h) and nitrogen-doped cavities must be considered. The possible role of fluorine in the educed $Nb^{+5}$ to $Nb^{+4}$ reaction under the impact of an X-ray beam at room temperature and during the thermal treatment is also discussed. The range of temperature and duration parameters of the thermal treatment at which the niobium surface would not be contaminated with impurities is determined for industrial applications.
title In-situ Synchrotron X-Ray Photoelectron Spectroscopy Study of Medium-Temperature Baking of Niobium for SRF Application
topic Accelerator Physics
Materials Science
Superconductivity
url https://arxiv.org/abs/2312.06529