Search NASA⌕ Search

Engineering topics

Kelley, Michael

Publications and source records attributed to Kelley, Michael.

At least 19 records

Materials Science of the Interstitial Doping Process

Particle accelerators are an increasingly important tool for frontier science. Growing initial and operating costs are a significant barrier for upgrades and for new machines. While everything matters, the major cost contributor is the SRF cavities and their ancillary facilities (e.g., cryoplant). Accordingly, the accelerator science community devotes much R&D effort to improving their energy efficiency (increased Q o ) and gradient (E acc ). While improved gradient is at the forefront for certain machines (ILC), improved quality factor has broader impact, benefitting all SRF applications. An important opportunity for accelerator science and technology to move forward arose in the course of building the LCLS-II, the second generation Linac Coherent Light Source at SLAC. At more or less the same time, researchers at Fermilab discovered that introducing a small amount of nitrogen to the niobium surface could improve the mid-range quality factor as much as three-fold. A firm resolution of how nitrogen confers its benefit attracts much current research interest. The key elements of the “nitrogen doping” process were vacuum bake at 800 °C, brief exposure to mTorr of nitrogen at several hundred degrees followed by electropolish (EP) to remove several microns from the surface to eliminate unwanted nitrides: While the process as a whole was novel, the comprising unit operations are familiar to the accelerator community. It was judged reasonable to adopt it as a cost-reduction technology for LCLS-II. Researchers carried out a program of varying process parameters and measuring performance in single-cell cavities, leading to a consensus stable protocol for the project. The transition to vendor fabrication and multiple niobium sources has presented unforeseen challenges of performance variation evidently not connected to anything that could be incorporated in a purchase specification. Moving beyond the high temperature N-doping process above, researchers reported a simplified process consisting entirely of tens of hours anneal in a N atmosphere at low temperatures (~120°C – 160°C) after 800 °C UHV bake. These processes typically yield a few-nm doped layer while the high temperature process yields at least a few to many micron doped layer. Even more recently, oxygen has been used to dope instead of nitrogen which leaves a few-µm O-alloyed layer upon vacuum annealing for 300 °C for ~3 hours. The investigation of these materials is just beginning, but the process simplification they may offer is surely attractive. The very low quantity of material that appears to be significant in the “infusion” process indicates the need for very careful control of gas species available for diffusion into the surface during low temperature treatment, both for process control and research to characterize the underlying dynamics. Oxygen alloying offers the further opportunity to utilize the decomposition of the surface native oxide as the dopant source. It is necessary to understand and (thus) manage this process. We have been supported by the Department of Energy Offices of High Energy Physics and Nuclear Physics to pursue this goal.

36 MATERIALS SCIENCE↗

SURFACE ROUGHNESS REDUCTION AND PERFORMANCE OF Nb3Sn FILM FOR SRF APPLICATIONS

Nb3Sn offers better RF performance (Q and Eacc) than Nb at any given temperature because of its superior superconducting properties. The potential deployment of Nb3Sn-coated SRF cavities at 4 K, delivering similar performance to that of Nb cavities at 2 K, will be a transformational technology to enable new classes of SRF accelerator applications. A clean and smooth surface can enhance the performance of the Nb3Sn-coated cavity, typically, the attainable acceleration gradient. The reduction of surface roughness is often linked with a correlative reduction in average coating thickness and grain size. A new approach to enhance the nucleation centers using the pre-deposition of Sn on Nb is introduced for surface roughness reduction. Besides Sn supply's careful tuning, the temperature profiles were varied to engineer the coating surface with reduced roughness as low as ~40 nm in 20 µm × 20 µm AFM scans, one-third that of the typical coating. Electropolishing of coated sample shows surface a clear surface smoothening. A few sets of coating parameters were used to coat 1.3 GHz sin-gle-cell cavities to understand the effects of roughness variation on the RF performance. This presentation discusses ways to reduce surface roughness with results from a systematic analysis of the samples and Nb3Sn-coated single-cell cavities.

Pudasaini, Uttar↗

SIMS CHARACTERIZATION OF NITROGEN DOPING OF LCLS-II-HE PRODUCTION CAVITIES

The thermal diffusion of nitrogen into the surface of niobium has been shown to yield superior low-loss SRF performance. An effective solution was identified and promptly employed in the production of cryomodules for LCLS-II. With added experience and R&D, a modified process was chosen for use in the upgrade for LCLS-II-HE. Largely motivated by this circumstance, supporting research has significantly refined the technique for making calibrated secondary ion mass spectrometry (SIMS) measurements of the N concentration depth profiles produced by production processes. Standardized reference samples were included with four HE production cavities in their N-doping furnace runs. We report the calibrated dynamic SIMS depth profiles of N, C, and O for these samples, together with the cryogenic acceptance test performance of the associated cavities. Interpretation and comparison with similar samples acquired in other furnaces highlights the importance of intentional process quality control of furnace conditions.

Reece, Charles↗

Topographic Evolution of Nb Surfaces Subjected to Electropolishing

Surface quality plays an important role in the performance of SRF cavities. We report the topographic evolution of H degassed, N and O doped Nb surfaces subjected to electropolishing using atomic force microscopy. N doped Nb shows a substantial increase in roughness due to formation of niobium nitrides into the surface. Implications of the topography on magnetic field enhancement and vortex entry are discussed.

Lechner, E.M.↗

SURFACE ROUGHNESS REDUCTION AND PERFORMANCE OF Nb3Sn FILM FOR SRF APPLICATIONS

Nb3Sn offers better RF performance (Q and Eacc) than Nb at any given temperature because of its superior superconducting properties. The potential deployment of Nb3Sn-coated SRF cavities at 4 K, delivering similar performance to that of Nb cavities at 2 K, will be a transformational technology to enable new classes of SRF accelerator applications. A clean and smooth surface can enhance the performance of the Nb3Sn-coated cavity, typically, the attainable acceleration gradient. The reduction of surface roughness is often linked with a correlative reduction in average coating thickness and grain size. A new approach to enhance the nucleation centers using the pre-deposition of Sn on Nb is introduced for surface roughness reduction. Besides Sn supply's careful tuning, the temperature profiles were varied to engineer the coating surface with reduced roughness as low as ~40 nm in 20 µm × 20 µm AFM scans, one-third that of the typical coating. Electropolishing of coated sample shows surface a clear surface smoothening. A few sets of coating parameters were used to coat 1.3 GHz sin-gle-cell cavities to understand the effects of roughness variation on the RF performance. This presentation discusses ways to reduce surface roughness with results from a systematic analysis of the samples and Nb3Sn-coated single-cell cavities.

Pudasaini, Uttar↗

SIMS CHARACTERIZATION OF NITROGEN DOPING OF LCLS-II-HE PRODUCTION CAVITIES

The thermal diffusion of nitrogen into the surface of niobium has been shown to yield superior low-loss SRF performance. An effective solution was identified and promptly employed in the production of cryomodules for LCLS-II. With added experience and R&D, a modified process was chosen for use in the upgrade for LCLS-II-HE. Largely motivated by this circumstance, supporting research has significantly refined the technique for making calibrated secondary ion mass spectrometry (SIMS) measurements of the N concentration depth profiles produced by production processes. Standardized reference samples were included with four HE production cavities in their N-doping furnace runs. We report the calibrated dynamic SIMS depth profiles of N, C, and O for these samples, together with the cryogenic acceptance test performance of the associated cavities. Interpretation and comparison with similar samples acquired in other furnaces highlights the importance of intentional process quality control of furnace conditions.

Reece, Charles↗

Challenges to Reliable Production Nitrogen Doping of Nb for SRF Accelerating Cavities

Over the last several years, alloying of the surface layer of niobium SRF cavities has been demonstrated to beneficially lower the superconducting RF surface resistance. Nitrogen, titanium, and oxygen have all been demonstrated as effective alloying agents, occupying interstitial sites in the niobium lattice within the RF penetration depth and even deeper, when allowed to thermally diffuse into the surface at appropriate temperatures. The use of nitrogen for this function has been often termed ’nitrogen doping’ and is being applied in the LCLS-II and LCLS-II HE projects. We report characterization studies of the distribution of nitrogen into the exposed niobium surface and how such distribution is affected by the quality of the vacuum furnace environment in which the doping takes place, and the complexity of nitride crystal growth on different grain orientations of surface niobium. Using state-of-the-art quantification methods by dynamic secondary ion mass spectrometry (SIMS) depth profiling in niobium, we identify several phenomena involving furnace-sourced contamination. We also highlight a potential issue with N₂ flow constraints from the flange ’caps’ used during heat treatments.

Reece, Charles↗

Modeling O and N Alloying in Nb for SRF Applications

N and O-alloyed superconducting radio frequency cavities exhibit extraordinary quality factors. Developing diffusion models that describe interstitial N and O in Nb is important for optimizing alloyed cavity quality factors and accelerating gradients. N and O-alloyed Nb samples are examined with SEM AND SIMS and their diffusion profiles modeled.

Lechner, Eric↗

Characterization of NbTiN Thin Film Structures

Approaching the bulk Nb material RF performance limits has urged development of alternative superconducting materials for superconducting radio frequency (SRF) accelerator cavities for further performance enhancement. A promising theory has predicted that thin film structures of superconductor-insulator-superconductor (SIS) [1] can delay magnetic flux penetration in accelerator cavities to higher fields. A candidate superconductor for the SIS structures is NbTiN. A few key aspects of SIS structures development are high quality individual layers, sharp interfaces and optimum thickness for first flux penetration (Hfp) delay. High quality monocrystalline NbTiN films are deposited by reactive DC magnetron sputtering. In a parallel development, interface quality was assessed by depositing bilayers of 3 nm NbTiN with ~1 nm AlN repeated up to 16 times with no increase in roughness of the structure. The stacked layers form a metamaterial, which could exhibit Tc greater than bulk NbTiN [2]. This contribution presents the characterization of the surface, material and superconductivity of NbTiN with concentration on the Hfp enhancement for 200 to 5 nm films and multilayer nanostructures.

Beverstock, David↗

Nb3Sn growth on niobium in vapor diffusion process and its application to large RF surface

Nb3Sn-coated SRF cavities can potentially achieve superior performance in terms of quality factor, accelerating gradient, and operating temperature. Tin vapor diffusion process of Nb3Sn coating on Nb is a simple, yet efficacious technique to fabricate Nb3Sn-coated SRF cavities. The process comprises two¬ steps: ?nucleation? followed by ?deposition?. The crucible with Sn/SnCl2 and the substrate at a constant temperature of about 500 °C for several hours is the ?nucleation?; the crucible and the substrate at a constant temperature, typically, above 1000 °C is the ?deposition? step. Using custom-built sample coating chamber, we have coated over a hundred samples to systematically study the vapor diffusion process under varying process conditions and at different stages of the coating process. The surfaces, thus obtained, were investigated with surface studies techniques, such as SEM/EDS, AFM, XPS, SAM, SIMS, EBSD and TEM. Based on the experimental results, we will discuss nucleation and growth of Nb3Sn coating during vapor diffusion process.

Pudasaini, Uttar↗

Surface Characterization of NbTiN multilayer films for accelerator applications

Further enhancement of superconducting accelerating cavity performance calls upon the development of materials beyond bulk niobium (Nb). Superconducting RF (SRF) is a surface phenomenon; for most superconducting materials the RF penetration depth is in the range of hundreds of nanometers. Due to the field penetration enhancement occurring in films with a thickness smaller than their nominal penetration depth, multilayer superconductor/insulator/superconductor (SIS) structures are theorized to have potential to support surface magnetic fields beyond the reach of the current SRF cavities. A candidate superconductor for SIS structures is the ternary compound NbTiN. SIS structures based on NbTiN and AlN are currently under development at JLab. NbTiN can be deposited with nominal superconducting parameters using DC reactive magnetron sputtering. This contribution presents the characterization of surface, material and superconducting properties of NbTiN films and SIS structures. Notably, the first flux penetration (Hfp) measured by SQUID magnetometry of 200 to 5 nm thick films and Hfp enhancement by multilayer structures is evaluated.

Beringer, Douglas↗

Nb3Sn Multilayer Sequential Sputtering at Jefferson Lab

Nb3Sn-coated Nb SRF cavities are studied due to their potential of providing a higher accelerating gradient over Nb SRF cavities. Magnetron sputtering can be a feasible alternative to conventional tin vapor diffusion process to fabricate Nb3Sn for SRF cavities. By depositing Nb and Sn layers separately and annealing afterwards, the stoichiometry of the coated films can be controlled to create Nb3Sn. To understand the formation of Nb3Sn at higher annealing temperatures, a comparative study of deposition and processing conditions is required. We have sputtered Nb and Sn multilayers and post-deposition annealed at 850, 950, 1000, 1100 and 1200 °C for 3 hours. The structural properties of the annealed films were characterized by X-ray diffraction (XRD) and compared to as-coated films. The film microstructures and compositions were examined by scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDS). The superconducting transition of the films were measured by surface resistivity data obtained down to cryogenic temperatures. A new cavity deposition system with a cylindrical magnetron has been designed to implement the sequential sputtering technique onto a single-cell cavity.

Eremeev, Grigory↗

Genesis of topography in buffered chemical polishing of niobium for application to superconducting radiofrequency accelerator cavities

Topography arising from the final etch step in preparing niobium superconducting radiofrequency (SRF) accelerator cavities is understood to significantly impact cavity performance at high field levels. This study investigated the effect of process temperature and time on the etch rate and topography arising from the widely-used buffered chemical polishing (BCP). This study aims to understand more thoroughly the genesis of topography in BCP of polycrystalline niobium, with the ultimate aim of finding a path to surface smoothness comparable to that obtained by electro-polishing (EP). It was found that the etch process is controlled by the surface reaction; and that the etch rate varies with crystallographic orientation. The familiar micron-scale roughening necessarily results. Gas evolution has an impact, but is secondary. The major outcome is that surface smoothness comparable to EP appears to be inherently unachievable for polycrystalline niobium using BCP, setting an upper limit to the gradient for which it is useful.

Reece, Charles↗

Examination of cutouts from Nb3Sn coated cavity inner surfaces

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.

Eremeev, Grigory↗

Progress towards Nb3Sn CEBAF Injector Cryomodule

Operations at 4 K instead of 2 K have the potential to reduce the operational cost of an SRF linac by a factor of 3, if the cavity quality factor can be maintained. Cavities coated with Nb3Sn have been shown to achieve the accelerating gradients above 10 MV/m with a quality factor around 1010 at 4 K. Because such performance is already pertinent for CEBAF injector cryomodule, we are working to extend these results to CEBAF accelerator cavities envisioning coating of two CEBAF 5-cell cavities with Nb3Sn. They will be installed in an injector cryomodule and tested with beam. The progress on this path is reported in this contribution.

Eremeev, Grigory↗

Experimental Study of Nucleation for Nb3Sn Diffusion Coatings on Niobium SRF cavities

Nb3Sn has the potential to achieve superior performance both in terms quality factor and accelerating gradient resulting in significant reduction in both initial and operating costs of SRF linacs. Cavity interior surface coatings are obtained by two-step vapor diffusion: nucleation followed by deposition. To gain more understanding of nucleation and its effect on the subsequent coating, we investigated the effect of varying parameters in a typical tin/tin chloride process. We report findings obtained by SEM/EDS, AFM, SAM and other materials characterization approaches.

Pudasaini, Uttar↗

Investigation of Nitrogen Absorption Rate and Nitride Growth on SRF Cavity Grade RRR Niobium as a Function of Furnace Temperature

The current state of the art processing of niobium superconducting radio frequency cavities with nitrogen diffusion is performed at 800 C 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 for this recipe. These measurements have been successfully modelled by extrapolating data from nitride growth studies performed at atmospheric pressure and temperatures above 1000 C.1 One open question is whether there is a diffusion-only zone at lower temperature in the ~20 mTorr range 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 which is what has been shown down to 600 C at atmospheric pressures on long time scales. A systematic study of absorption vs. temperature and correlated SIMS measurements is required to answer this question. We report on measurements of the parabolic rate constant vs. temperature from 400 C to 900 C of cavity grade niobium with metallurgically flat witness samples. Depth profiles of witness samples using SIMS are presented together with SEM imaging for nitride crystals and correlated with N absorption.

Reece, Charles↗

Investigation of Low-Level Nitrogen in Niobium by Secondary Ion Mass Spectrometry

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.

Tuggle, Jay↗