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Abstract Surface structures on radio-frequency (RF) superconductors are crucially important in determining their interaction with the RF field. Here we investigate the surface compositions, structural profiles, and valence distributions of oxides, carbides, and impurities on niobium (Nb) and niobium–tin (Nb₃Sn)in situunder different processing conditions. We establish the underlying mechanisms of vacuum baking and nitrogen processing in Nb and demonstrate that carbide formation induced during high-temperature baking, regardless of gas environment, determines subsequent oxide formation upon air exposure or low-temperature baking, leading to modifications of the electron population profile. Our findings support the combined contribution of surface oxides and second-phase formation to the outcome of ultra-high vacuum baking (oxygen processing) and nitrogen processing. Also, we observe that vapor-diffused Nb₃Sn contains thick metastable oxides, while electrochemically synthesized Nb₃Sn only has a thin oxide layer. Our findings reveal fundamental mechanisms of baking and processing Nb and Nb₃Sn surface structures for high-performance superconducting RF and quantum applications. 

Intermetallic Nb3Sn alloys have long been believed to form through Sn diffusion into Nb. However, our observations of significant oxygen content in Nb3Sn prompted an investigation of alternative formation mechanisms. Through experiments involving different oxide interfaces (clean HF-treated, native oxidized, and anodized), we demonstrate a thermodynamic route that fundamentally challenges the conventional Sn diffusion mechanism for Nb3Sn nucleation. Our results highlight the critical involvement of a SnOx intermediate phase. This new nucleation mechanism identifies the principles for growth optimization and new synthesis of high-quality Nb3Sn superconductors. 

Abstract Workbench-size particle accelerators, enabled by Nb₃Sn-based superconducting radio-frequency (SRF) cavities, hold the potential of driving scientific discovery by offering a widely accessible and affordable source of high-energy electrons and x-rays. Thin-film Nb₃Sn RF superconductors with high quality factors, high operation temperatures, and high-field potentials are critical for these devices. However, surface roughness, non-stoichiometry, and impurities in Nb₃Sn deposited by conventional Sn-vapor diffusion prevent them from reaching their theoretical capabilities. Here we demonstrate a seed-free electrochemical synthesis that pushes the limit of chemical and physical properties in Nb₃Sn. Utilization of electrochemical Sn pre-deposits reduces the roughness of converted Nb₃Sn by five times compared to typical vapor-diffused Nb₃Sn. Quantitative mappings using chemical and atomic probes confirm improved stoichiometry and minimized impurity concentrations in electrochemically synthesized Nb₃Sn. We have successfully applied this Nb₃Sn to the large-scale 1.3 GHz SRF cavity and demonstrated ultra-low BCS surface resistances at multiple operation temperatures, notably lower than vapor-diffused cavities. Our smooth, homogeneous, high-purity Nb₃Sn provides the route toward high efficiency and high fields for SRF applications under helium-free cryogenic operations. 

Abstract Superconducting radio‐frequency (SRF) resonators are critical components for particle accelerator applications, such as free‐electron lasers, and for emerging technologies in quantum computing. Developing advanced materials and their deposition processes to produce RF superconductors that yield nΩ surface resistances is a key metric for the wider adoption of SRF technology. Here, ZrNb(CO) RF superconducting films with high critical temperatures (T_c) achieved for the first time under ambient pressure are reported. The attainment of aT_cnear the theoretical limit for this material without applied pressure is promising for its use in practical applications. A range ofT_c, likely arising from Zr doping variation, may allow a tunable superconducting coherence length that lowers the sensitivity to material defects when an ultra‐low surface resistance is required. The ZrNb(CO) films are synthesized using a low‐temperature (100 – 200 °C) electrochemical recipe combined with thermal annealing. The phase transformation as a function of annealing temperature and time is optimized by the evaporated Zr‐Nb diffusion couples. Through phase control, one avoids hexagonal Zr phases that are equilibrium‐stable but degradeT_c. X‐ray and electron diffraction combined with photoelectron spectroscopy reveal a system containing cubic β‐ZrNb mixed with rocksalt NbC and low‐dielectric‐loss ZrO₂. Proof‐of‐concept RF performance of ZrNb(CO) on an SRF sample test system is demonstrated. BCS resistance trends lower than reference Nb, while quench fields occur at approximately 35 mT. The results demonstrate the potential of ZrNb(CO) thin films for particle accelerators and other SRF applications.