Search

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"). 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. [ABSTRACT FROM AUTHOR]

The importance of SIMS analyses for "N-doped" impurity alloyed niobium and other surface-alloyed materials continues to increase. A major hurdle is the uncertainty of instrument calibration due to changes in sample height either from sample surface topography or from the sample holder itself. The CAMECA sample holder design allows for many types of samples to be analyzed. However, a drawback is that the holder faceplate can bend, contributing an uncertainty in the relative sensitivity factor (RSF) used to quantify the SIMS results. Here, we describe an improved sample holder having a reinforced faceplate, which prevents deflection and reduces uncertainty. Simulations show that the new design significantly reduces deflection from 10 μm to 5 nm. Sample measurements show a reduction of RSF uncertainty from this source from 4.1% to 0.95%. Grain orientation has long been suspected to affect RSF measurement as well. A bicrystal implant standard, consisting of randomly oriented and [001] grains, was successively rotated 15° between analyses. It was observed that 20% of the analyses performed on the randomly oriented grain exhibited anomalously high RSF values as well as slow sputter rates. These features were associated with the changing grain normal orientation with respect to the primary Cs+ beam. The grain orientation associated with the rise in RSF was simulated and determined to be the [101] crystallographic plane, thus indicating that ion channeling was responsible for the significantly increased RSF. Focused ion beam analysis confirmed slower sputter rates for the cardinal crystallographic orientations, indicating that ion channeling occurred for each. [ABSTRACT FROM AUTHOR]

Accurate secondary ion mass spectroscopy measurement of nitrogen in niobium relies on the use of closely equivalent standards, made by ion implantation, to convert nitrogen signal intensity to nitrogen content by determination of relative sensitivity factors (RSFs). Accurate RSF values for ppm-range nitrogen contents are increasingly critical, as more precision is sought in processes for next-generation superconducting radiofrequency (SRF) accelerator cavities. Factors influencing RSF value measurements were investigated with the aim of reliably attaining better than 10% accuracy in nitrogen concentrations at various depths into the bulk. This has been accomplished for materials typical of SRF cavities at the cost of increased attention to all aspects. [ABSTRACT FROM AUTHOR]

The potential of Nb3Sn for superconducting radio frequency cavities is widely recognized, and renewed R&D efforts continue to bring new insights about the material's structure and properties. We have systematically coated niobium samples with Nb3Sn for different durations. Several samples were coated over ("overcoat") multiple times to elucidate the growth kinetics of Nb3Sn during the tin vapor-diffusion process. Analysis of coated samples is consistent with the model in which tin diffuses via grain boundaries to the Nb3Sn-Nb interface, where the growth of Nb3Sn into the niobium bulk takes place. Similar scaling laws are found for Nb3Sn grain growth and layer thickness. Nonparabolic layer growth is consistent with significant grain growth, which reduces the number of Sn transport channels. An examination of patchy regions in Nb3Sn coating, revealing large single-crystalline grains, points to impeded Nb3Sn layer growth due to low grain boundary density, resulting in a significantly thinner coating in those areas. [ABSTRACT FROM AUTHOR]

Electron field emission (FE) from broad-area metal surfaces is known to occur at much lower electric field than predicted by Fowler-Nordheim law. Although micron or submicron particles are often observed at such enhanced field emission (EFE) sites, the strength and number of emitting sites and the causes of EFE strongly depend on surface preparation and handling, and the physical mechanism of EFE remains unknown. To systematically investigate the sources of this emission, a dc scanning field emission microscope (SFEM) has been built as an extension to an existing commercial scanning electron microscope (SEM) equipped with an energy-dispersive spectrometer for emitter characterization. In the SFEM chamber of ultrahigh vacuum (∼ 10[sup -9] Torr), a sample is moved laterally in a raster pattern (2.5 µm step resolution) under a high voltage anode microtip for field emission detection and localization. The sample is then transferred under vacuum by a hermetic retractable linear transporter to the SEM chamber for individual emitter site characterization. Artificial marks on the sample surface serve as references to convert x, y coordinates of emitters in the SFEM chamber to corresponding positions in the SEM chamber with a common accuracy of ± 100-200 µm in x and y. Samples designed to self-align in sample holders are used in each chamber, allowing them to retain position registration after non-in situ processing to track interesting features. No components are installed inside the SEM except the sample holder, which does not affect the routine operation of the SEM. The apparatus is a system of low cost and maintenance and significant operational flexibility. Field emission sources from planar niobium— the material used in high-field rf superconducting cavities for particle accelerator—have been studied after different surface preparations, and significantly reduced field emitter density has been achieved by refining the preparation... [ABSTRACT FROM AUTHOR]