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Historically, niobium has been used as the superconducting material in SRF cavities. Due the high operational costs, other materials are currently being considered. Nb₃Sn coatings have been investigated over the past several decades, motivated by potentially higher operating temperatures. More recently niobium has been doped with nitrogen to improve the quality factor (Q). Currently, a need for better understanding still exists for both mechanisms. EBSD has been shown to be a viable technique to determine the crystallographic orientation and the size of the Nb₃Sn grains. The EBSD maps obtained show a bimodal distribution of grain sizes with smaller Nb₃Sn grains found present near the Nb₃Sn/Nb interface. In addition to the Nb₃Sn coatings, N-doped niobium coupons were analyzed by EBSD and found that the coupon had preferred surface orientation. The EBSD analysis was found to be vital as specific grains could be targeted in SIMS to better understand the diffusion of nitrogen with respect to crystal orientation., Proceedings of the 19th International Conference on RF Superconductivity, SRF2019, Dresden, Germany

Understanding of Nb₃Sn nucleation and growth is essential to the progress with Nb₃Sn vapor diffusion coatings of SRF cavities. Samples representing different stages of Nb₃Sn formation have been produced and examined to elucidate the effects of nucleation, growth, process conditions, and impurities. Nb₃Sn films from few hundreds of nm up to ~15 µm were grown and characterized using AFM, SEM/EDS, XPS, EBSD, SIMS, and SAM. Microscopic examinations of samples suggest the mechanisms behind Nb₃Sn thin film nucleation and growth. RF measurements of coated cavities were combined with material characterization of witness samples to adapt the coating process in "Siemens" coating configuration. Understanding obtained from sample studies, applied to cavities, resulted in Nb₃Sn cavity with quality factor 2 ×10¹⁰ at 15 MV/m accelerating gradient at 4 K, without "Wuppertal" Q-slope. We discuss the genesis of the Nb₃Sn thin film in a typical tin vapor diffusion process, and its consequences to the coating of SRF cavities., Proceedings of the 19th International Conference on RF Superconductivity, SRF2019, Dresden, Germany

The promise of better performance and significant cost reduction make Nb3Sn-coated Nb SRF cavities an attractive option when compared to traditional Nb SRF cavities. Historically, the vapor diffusion technique for coating Nb cavities with Nb3Sn has proven to be the most successful, and is currently practiced in several research facilities with minor variations. Using modern characterization tools, we examined the Nb3Sn coating prepared in different systems and/or under different conditions. Identically prepared high RRR (~ 300) Nb samples were coated using existing standard protocols at different coating facilities. The microstructure and composition of Nb3Sn coatings were found to be similar when examined with scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDS). Atomic force microscopy (AFM) was performed on each sample and the topographies of the samples were then compared in terms of power spectral densities (PSDs). Secondary ion mass spectrometry (SIMS) depth profiles revealed trace amounts of Ti in some of the samples., Proceedings of the 18th Int. Conf. on RF Superconductivity, SRF2017, Lanzhou, China

The Nb3Sn-coated cavities aim to enhance perfor-mance and significantly reduce cost. Their fabrication involves tin vapor diffusion coating of Nb3Sn on the interior surface of a Nb cavity. Controlled removal of first few layers to obtain a smoother and cleaner surface could be desirable to improve the high field RF perfor-mance. Our first results from the application of elec-tropolishing and oxypolishing techniques on Nb3Sn-coated surfaces indicated reduced surface roughness, and the surface composition appeared nominally unchanged. Systematic studies explore the effect of different polish-ing parameters into the roughness and composition. We present the latest results from SEM/EDS and AFM studies of Nb3Sn-coated samples treated with electropolishing and oxypolishing., Proceedings of the 9th Int. Particle Accelerator Conf., IPAC2018, Vancouver, BC, Canada

The potential of Nb3Sn for SRF cavities is widely recognized and renewed R&D efforts continue to bring new insights about material structure and its properties. We have systematically coated niobium with Nb3Sn using "vapor diffusion" under varying coating conditions to elucidate the reaction of tin with niobium at the temperatures of interest. The analysis of the coated samples is revealing new understanding about the two-stage nucleation/deposition ("vapor diffusion") process that allows us to form a hypothesis regarding Nb3Sn formation mechanism. The essential aspect of nucleation is the deposition of a high coverage, nanoscale thin tin film with particle assemblage by decomposition of tin chloride on the niobium surface at temperatures sufficient for reduction of the thick niobium oxide film, usually at about 500°C. The deposition is followed by the reaction of tin from tin vapor with the niobium surface to form Nb3Sn at about 1200°C, where the surface and grain boundaries start to play key role in the formation process initiation and progression. These findings improve understanding of the Nb3Sn growth in the typical vapor diffusion process used for accelerator cavity coatings., Proceedings of the 18th Int. Conf. on RF Superconductivity, SRF2017, Lanzhou, China

In order to fully understand nitrogen addition techniques it is vital to have a full understanding of the material, including the content, location, and speciation of nitrogen contained in the treated Nb. In this work Secondary Ion Mass Spectrometry (SIMS) is used to elucidate content and location. Dynamic SIMS nitrogen analysis is reported, for the first time, for "as-received" cavity grade niobium from three separate suppliers. In addition, a number of method and instrumental issues are discussed including depth resolution, detection limit, and quantification., Proceedings of the 18th Int. Conf. on RF Superconductivity, SRF2017, Lanzhou, China

Nb3Sn is a potential candidate to replace Nb in SRF accelerator cavities to reduce cost and advance perfor-mance. Tin vapor diffusion is the preferred technique to realize such cavities by growing a few microns thick Nb3Sn coating on the interior surface of the niobium cavity. The coating process typically uses temperatures of 1100-1200 °C for 3-6 hours. It is important to better understand the coating process, and optimize the coating parameters to overcome the current limitation on the performance of Nb3Sn coated SRF cavities. We investi-gate Nb3Sn coatings prepared in the temperature range of 900-1200 °C and duration of 3 - 12 hours using various material characterization tools. Variation of these pa-rameters appears to have notable effect on microstructure and topography of the obtained surface., Proceedings of the 9th Int. Particle Accelerator Conf., IPAC2018, Vancouver, BC, Canada

Understanding the improvement of the SRF cavity quality factor by low-level nitrogen addition ("N-doping") is attracting much attention from researchers. Precise, repeatable measurement of the nitrogen profile in the parts-per-thousand to parts-per-million range is vital. Secondary Ion Mass Spectrometry (SIMS) is the approach of choice because of excellent sensitivity and depth resolution. Accurate quantitation must consider sample properties, such as surface topography and crystal structure, calibration of the instrument with reference materials, and data analysis. We report the results of a SIMS study in which polycrystal and single crystal coupons were N-doped, each accompanied by new SRF-grade niobium sheet equivalent to a single cell cavity., Proceedings of the 28th Linear Accelerator Conf., LINAC2016, East Lansing, MI, USA

The potential for higher operating temperatures and increased accelerating gradient has attracted SRF researchers to Nb3Sn coatings on niobium for nearly 50 years. The two-step tin vapor diffusion: nucleation followed by deposition appears to be a promising technique to prepare Nb3Sn coatings on interior cavity surface. We have undertaken a fundamental materials study of the nucleation and deposition steps. Nucleation was accomplished within parameter ranges: 300 - 500 °C, 1 - 5 hrs duration, 5 mg - 1 g SnCl2 and 1 g Sn. The resulting deposit consists of (< 10%) coverage of tin particles, as determined by SEM/EDS, while XPS and SAM discovered extra tin film between these particles. Preliminary results by EBSD show no evident effect of substrate crystallography on the crystallography of the final coating. Substantial topography was found to develop during the coating growth., Proceedings of the North American Particle Accelerator Conf., NAPAC2016, Chicago, IL, USA

The current state of the art processing of niobium superconducting radio frequency cavities with nitrogen diffusion is performed at 800C in a furnace with a partial pressure of approximately ~20 mtorr of nitrogen. Multiple studies have shown the bulk of the nitrogen absorbed by the niobium forms a thick (1-3 microns) non-superconducting nitride layer which must be removed to produce optimal RF results. The depth profiling of interstitial nitrogen and surface nitrides has already been probed using SIMS measurements. These measurements have also been modeled by extrapolating data from nitride growth studies performed at atmospheric pressure and temperatures above 1000 C (**). One open question is whether there is a diffusion zone at lower temperature in which the niobium will absorb nitrogen but not create a non-superconducting nitride layer; or is the absorption of nitrogen only possible by first forming a nitride buffer layer which then frees up nitrogen for absorption. A systematic study of absorption rate vs. temperature and correlated SIMS measurements needs to be performed to answer this question. We report on the absorption rate vs. temperature from 400 C to 900 C of cavity grade niobium with metallurgically flat witness samples. The witness samples surface depth profile of NbN via SIMS's will be presented and correlated to the absorption.**, Proceedings of the 28th Linear Accelerator Conf., LINAC2016, East Lansing, MI, USA

Practical SRF cavities may be subjected to one or more processes after nominally complete preparation. Successful implementation of such processes in Nb3Sn coated cavities requires the understanding of material's response to these treatments. SRF-grade Nb samples, coated with Nb3Sn by the widely used tin vapor diffusion process were subjected to one or more of the following: hydrofluoric acid (HF) rinsing, oxypolishing, buffered chemical polishing (BCP) or electrochemical treatment. They were examined by materials characterization tech-niques including scanning electron microscopy (SEM) with energy dispersive X-ray spectroscopy (EDS), atomic force microscopy (AFM), and X-ray photoelectron spec-troscopy (XPS). The effects compared to niobium are different enough in most cases that further development is desirable to routinely obtain a favorable result., Proceedings of the 8th Int. Particle Accelerator Conf., IPAC2017, Copenhagen, Denmark

The potential for higher operating temperature and higher gradient have motivated SRF cavity researchers to pursue Nb3Sn as an alternative to Nb for nearly fifty years. Far and away the most common embodiment has been a few micron-thick Nb3Sn layer on the cavity interior surface obtained by vapor diffusion coating, with one or another set of parameters. While many cavities have been made and RF tested, reports of dissecting a cavity in detail to examine the coating and relate it to RF measurements are rare. We coated a BCP-treated single cell cavity in a typical process of tin/tin chloride activation at 500 C followed by tin vapor deposition at 1200 C. After RF-testing, we cut and examined sections from several locations to learn composition, thickness topography of the interior surface. The effect of process variables, such as surface preparation, process temperature and duration, and vapor chemistry needs to be explored., Proceedings of the 28th Linear Accelerator Conf., LINAC2016, East Lansing, MI, USA

Although SRF accelerators are an invaluable research tool they can be painfully expensive to construct and operate at the current level of SRF technology. This cost is significantly due to the necessity to operate at a temperature of only 2K. Considerable research is currently underway into next generation SRF cavity technologies such as Ndoping and Nb3Sn coating. Both of these technologies will lower the cryogenic load of accelerators, correspondingly lowering both construction and operating costs. However, current understanding of either technology is incomplete and in order to elucidate the underlying mechanisms there is a need to push current characterization methods forward. In this work, ion beam techniques (e.g. focused ion beam (FIB)), and electron backscatter diffraction (EBSD) were applied to help understand Nb3Sn coating mechanisms. This presentation will focus on characterization, providing examples of EBSD work, along with discussion of some of the issues encountered while trying to produce high quality EBSD data., Proceedings of the 8th Int. Particle Accelerator Conf., IPAC2017, Copenhagen, Denmark

Exploiting both the new Nb3Sn coating system and the materials characterization tools nearby, we report our progress in low-loss Nb3Sn films development. Nb3Sn films a few micrometers thick were grown on Nb coupons as well as single- and multi-cell cavities by the Sn-diffusion technique. Films structure and composition were investigated on coated samples and cavity cutouts with characterization tools including SEM/EDS/EBSD, AFM, XPS, SIMS towards correlating film growth and RF loss to material properties and deposition parameters. Cavity coating efforts focused on establishing techniques for coating progressively more complicated RF structures, and understanding limiting mechanisms in coated cavities. Nb3Sn coated 1.5 GHz 1-cell and 1.3 GHz 2-cell cavities have shown quality factors of 10¹⁰ at 4.3 K, with several cavities reaching above Eacc = 10 MV/m. The dominant limiting mechanisms were low field quenches and quality factor degradation above 8 MV/m. The surface data indicates a near-stoichiometric Nb3Sn consistent with the transition temperature and gap measurements. The Nb3Sn layer is covered with Nb2O5 and SnO2 native oxides and has little memory of the pre-coating surface., Proceedings of the 17th International Conference on RF Superconductivity, SRF2015, Whistler, BC, Canada

The structure and composition of Nb3Sn films obtained by diffusion coating niobium coupons and SRF cavities were investigated by x-ray photoelectron spectroscopy (XPS), secondary ion mass spectroscopy (SIMS) and scanning electron microscopy (SEM) with energy-dispersive x-ray spectroscopy (EDS) and electron back-scatter diffraction (EBSD), including native surfaces, depth profiles and cross-sections. We find that the native surface oxide is significantly tin-rich, we have measured depth profiles. We find that the grains apparent in the SEM images are individual crystallites having no evident relationship to the substrate or each other., Proceedings of the 17th International Conference on RF Superconductivity, SRF2015, Whistler, BC, Canada