Analysis of the strategy for superconducting cavity material procurement and quality management is done on the basis of the experience with the cavity production for the European X-ray Free Electron Laser (EXFEL) facility. An adjustment of the material specification to EXFEL requirements, procurement of material, quality control (QC), documentation, and shipment to cavity-producers have been worked-and carried out by DESY. A multistep process of qualification of the material suppliers included detailed material testing, single-and nine-cell cavity fabrication and cryogenic radiofrequency tests. Production of about 25,000 semi-finished parts of high purity niobium and niobium-titanium alloy in a period of three years has been divided finally between companies Heraeus, Tokyo Denkai, Ningxia OTIC, and PLANSEE. Large-grain (LG) material as a possible option for the EXFEL has been considered and resulted in the production of one cryogenic module consisting of seven (out of eight) LG cavities. They fulfilled the EXFEL requirements and showed even 25 to 30% higher unloaded quality factor. A possible shortage of the required quantity of LG material on the market leaded, however, to the choice of conventional fine grain material. The eddy-current scanning has been applied as an additional QC tool for the niobium sheets and contributed significantly to the material qualification and sorting. 2% of the sheets have been rejected what potentially could affect up to 1/3 of the cavities. The main imperfections and defects in the rejected sheets have been analyzed. Samples containing foreign material inclusions have been extracted from the sheets and electrochemically polished. Some inclusions remained even after 150 µm surface layer removal. Indications of foreign material inclusions have been found in the industrially fabricated and treated cavities and a deeper analysis of the defects has been performed.
(100) oriented niobium (Nb) crystals annealed in the vacuum conditions close to that used in mass production of 1.3 GHz superconducting radio-frequency cavities for linear accelerators, and treated in nitrogen at a partial pressure of 0.04 mbar at temperatures of 800 °C and 900 °C have been studied. The surfaces of the nitrogen-treated samples were investigated by means of various surface-sensitive techniques, including grazing-incidence X-ray diffraction, X-ray photoemission spectroscopy and scanning electron microscopy with energy-dispersive X-ray spectroscopy in planar view and on cross-sections prepared by a focused ion beam. The appearance of a dense layer of epitaxial rectangular precipitates has been observed for the Niobium nitrided at 900°C. Increased nitrogen concentration in the near surface region was detected by glow-discharge optical-emission spectroscopy, focused ion-beam cross-sectional images and X-ray photoelectron spectroscopy. Crystalline phases of NbO and β-Nb 2 N were identified by X-ray diffraction. This information was confirmed by X-ray photoelectron measurements, which in addition revealed the presence of Nb 2 O 5 , NbON, NbN and NbN x O y components on the surface. These results establish the near-surface Nb phase composition after high-temperature nitrogen treatment, which is important for obtaining a better understanding of the improved RF cavity performance.
The structural and chemical composition of the surface layer (100-140 nm) of niobium radiofrequency cavities operating at cryogenic temperature has enormous impact on their superconducting characteristics. During the last years, cavities treated with a new thermal processing recipe, so-called nitrogen infusion, have demonstrated an increased efficiency and high accelerating gradients. The role and importance of nitrogen gas has been a topic of many debates. In the present work we employ variable-energy synchrotron X-ray photoelectron spectroscopy (XPS), to study the niobium surface subjected to the following treatments: vacuum annealing at 800°C, nitrogen infusion, and vacuum heat treatment as for the infusion process but without nitrogen supply. Careful analysis of XPS energy-distribution curves revealed a slightly increased thickness of the native oxide Nb2O5 for the infused samples (~3.8 nm) as compared to the annealed one (~3.5 nm) which indicates insignificant oxygen incorporation into niobium during 120°C baking and no effect of nitrogen on the formation of oxides or other niobium phases. By conducting an additional in-situ annealing experiment and analyzing the niobium after the failed infusion process, we conclude that the vacuum furnace hygiene particularly during the high-temperature stage is the prerequisite for success of any treatment recipe.
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