Search NASA⌕ Search

Engineering topics

Reece, Charles E.

Publications and source records attributed to Reece, Charles E..

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↗

Methods of controllable interstitial oxygen doping in niobium

A method for vacuum heat treating Nb, such as is used in superconducting radio frequency cavities, to engineer the interstitial oxygen profile with depth into the surface to conveniently optimize the low-temperature rf surface resistance of the material. An example application is heating of 1.3 GHz accelerating structures between 250-400° C. to achieve a very high quality factor of 5×1010 at 2.0 K. With data supplied by secondary ion mass spectrometry measurements, application of oxide decomposition and oxygen diffusion theory was applied to quantify previously unknown parameters crucial in achieving the oxygen alloy concentration profiles required to optimize the rf surface resistance. RF measurements of vacuum heat treated Nb superconducting radio frequency cavities confirmed the minimized surface resistance (higher Q0) previously expected only from 800° C. diffusive alloying with nitrogen.

Palczewski, Ari D.↗

Analysis of furnace contamination on superconducting radio frequency niobium using secondary-ion mass spectrometry

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”). Here 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.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Effect of substrate temperature on the growth of Nb 3 Sn film on Nb by multilayer sputtering

Here, we report on the fabrication of niobium tin (Nb 3 Sn) films by multilayer sequential sputtering on niobium at substrate temperatures ranging from room temperature to 250 °C. The multilayers were then annealed inside a separate vacuum furnace at 950 °C for 3 h. The material properties of the films were characterized by X-ray diffraction, scanning electron microscopy, energy-dispersive X-ray spectroscopy, atomic force microscopy, and transmission electron microscopy. The superconducting properties of the films were studied by four-point probe resistivity measurements from room temperature to below the superconducting critical temperature T c . The highest film T c was 17.76 K, obtained when the multilayers were deposited at room temperature. When the deposition temperature was raised to 250 °C, a significant reduction in voids was achieved while the film's T c was 17.58 K.

36 MATERIALS SCIENCE↗

Finite Element Modeling of Electrochemical Polishing of Niobium in Hydrofluoric-Sulfuric Acid Electrolyte

Niobium (Nb) used in superconducting radio-frequency cavities requires smooth surface to achieve optimal performance. In this work, a finite element model that coupled electrochemistry, heat transfer, and fluid dynamics was developed to investigate the electrochemical polishing mechanisms of Nb, using experimentally measured polarization results of coupon samples as validations. The current and potential distribution, oxide growth kinetics of Nb in a complex cavity geometry was investigated as a function of temperature and coolant flow. A low temperature coolant with intermediate flow rate was found to reduce surface current and ensure oxide uniformity. These results could shed light on the design of future particle accelerators.

SRF accelerator cavity↗

Improved quantitation of SIMS depth profile measurements of niobium via sample holder design improvements and characterization of grain orientation effects

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.

43 PARTICLE ACCELERATORS↗

Effect of substrate temperature on the growth of Nb$_3$Sn film on Nb by multilayer sputtering

Nb3Sn films were fabricated by multilayer sequential sputtering on Nb substrates at substrate temperatures ranging from room temperature to 250 °C. The film material properties were characterized by X-ray diffraction, scanning electron microscopy, energy-dispersive X-ray spectroscopy, atomic force microscopy, and transmission electron microscopy. The films’ superconducting properties were studied by four-point probe resistivity measurements from room temperature to below the superconducting critical temperature Tc. The highest Tc was17.76 K, when the multilayers were deposited at room temperature. A superconducting Nb3Sn thin film with a smoother surface morphology but a lower Tc of 17.58 K was obtained on the film deposited at a substrate temperature of 250 °C.

Sayeed, Md. Nizam↗

Advances in secondary ion mass spectrometry for N-doped niobium

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. Furthermore, 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.

47 OTHER INSTRUMENTATION↗

Properties of Nb3Sn films fabricated by magnetron sputtering from a single target

Superconducting Nb3Sn films were fabricated on sapphire and fine grain Nb substrates by magnetron sputtering from a single stoichiometric Nb3Sn target. The structural, morphological and superconducting properties of the films annealed for 24 h at temperatures of 800-1000 {\deg}C were investigated. The effect of the annealing time at 1000 {\deg}C was examined for 1, 12, and 24 h. The film properties were characterized by X-ray diffraction, scanning electron microscopy, atomic force microscopy, energy dispersive X-ray spectroscopy, and Raman spectroscopy. The DC superconducting properties of the films were characterized by a four-point probe measurement down to cryogenic temperatures. The RF surface resistance of films was measured over a temperature range of 6-23 K using a 7.4 GHz sapphire-loaded Nb cavity. As-deposited Nb3Sn films on sapphire had a superconducting critical temperature of 17.21 K, which improved to 17.83 K when the film was annealed at 800 {\deg}C for 24 h. For the films annealed at 1000 {\deg}C, the surface Sn content was reduced to ~11.3 % for an annealing time of 12 h and to ~4.1 % for an annealing time of 24 h. The Raman spectra of the films confirmed the microstructural evolution after annealing. The RF superconducting critical temperature of the as-deposited Nb3Sn films on Nb was 16.02 K, which increased to 17.44 K when the film was annealed at 800 {\deg}C for 24 h.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

TESLA's High Gradient March: Thirty years anniversary of TESLA Technology Collaboration (TTC)

In 2020, the TTC (TESLA Technology Collaboration) celebrates 30 years of collaborative efforts on SRF technologies. The first international TESLA workshop on a TeV Energy Superconducting Linear Accelerator was held at Cornell University on July 23-26, 1990. The purpose of the meeting was to work on a parameter list for a superconducting high energy physics collider in the Teravolt energy region and to explore ideas on how to increase the gradients and lower the costs for the accelerator structures. It was clear from the beginning that the needed technological progress would require a large international collaboration. This meeting was indeed the origin of a long preparation effort toward a future ILC (International Linear Collider), which eventually led to the realization of the TTF (TESLA Test Facility, since 2005 operated as the DESY user facility FLASH) and the European XFEL also at DESY, and created the conditions supporting the proposals for several large SRF-based research facilities like SNS, LCLS-II, ESS, PIP-II and SHINE, as well as a growing number of smaller facilities around the world. Highlights of this 30-year international collaboration are presented and celebrated.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗

Analysis of RF losses and material characterization of samples removed from a Nb 3 Sn-coated superconducting RF cavity

Nb 3 Sn (T c ≈18 K and H sh ≈400 mT) is a prospective material to replace Nb (T c ≈9 K and H sh ≈200 mT) in SRF accelerator cavities for significant cost reduction and performance enhancement. Because of its material properties, Nb3Sn is best employed as a thin film (coating) inside an already built RF cavity structure. A particular test cavity noted as C3C4 was a 1.5 GHz single-cell Nb cavity, coated with Nb3Sn using Sn vapor diffusion process at Jefferson Lab. Cold measurements of the coated cavity indicated the superconducting transition temperature of about 18 K. Subsequent RF measurements indicated field-dependent surface resistance both at 4.3 K and 2.0 K. After initial cold measurements, the cavity RF loss distribution was studied with a thermometry mapping system. Loss regions were identified with thermometry and were cut out for material analysis. The presence of significantly thin patchy regions and other carbon-rich defects is associated with strong local field-dependent surface resistance. This paper summarizes RF and thermometry results correlated with material science findings.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Progress with Nb Hipims Films on 1.3 GHz Cu Cavities

In recent years, efforts have been invested to leverage the different processes involved in energetic condensation to tailor Nb film growth in sequential steps. The resulting Nb/Cu films display high quality material properties and show promise of high RF performance. The lessons learned are now applied to 1.3 GHz Nb on Cu cavity deposition via high power impulse magnetron sputtering (HiPIMS). RF performance is measured at different temperatures. Particular attention is given to the effect of cooldown and sensitivity to external applied magnetic fields. The results are evaluated in light of the Nb film material and superconducting properties measured with various microscopy and magnetometry techniques in order to better understand the contributing factors to the residual and flux induced surface resistances. This contribution presents the insights gained in exploiting energetic condensation as a path towards RF Q-slope mitigation for Nb/Cu films, correlating film material characteristics with RF performance.

Burton, Matthew C.↗

Growth of Nb 3 Sn coating in tin vapor-diffusion process

The potential of Nb 3 Sn for superconducting radio frequency (SRF) cavities is widely recognized and renewed R&D efforts continue to bring new insights about the material's structure and properties. Here, we have systematically coated niobium with Nb 3 Sn for different durations, and several of them were coated over ("overcoat") multiple times, to elucidate the growth kinetics of Nb 3 Sn during tin vapor diffusion process. Analysis of coated samples is consistent with the model in which tin diffuses via grain boundaries to the Nb 3 Sn-Nb interface, where the growth of Nb 3 Sn into the Nb bulk takes place. Similar scaling laws were found for Nb 3 Sn grain growth and layer thickness. Non-parabolic layer growth is consistent with significant grain growth, which reduces the number of Sn transport channels. Examination of patchy region in Nb 3 Sn coating, revealing large single crystalline grains, points to impeded Nb 3 Sn layer growth due to low grain boundary density, resulting in a significantly thinner coating in those areas.

36 MATERIALS SCIENCE↗

Structural and superconducting properties of Nb 3 Sn films grown by multilayer sequential magnetron sputtering

Nb 3 Sn thin films are fabricated by sequential sputtering followed by annealing at 850–1200°C in vacuum. The effects of the annealing temperature and time on the formation of Nb 3 Sn were examined. The film crystal structure, morphology, surface topography and composition were distinguished by X-ray diffraction, field-emission scanning electron microscopy, atomic force microscopy, and energy dispersive X-ray spectroscopy analysis. The superconducting properties of the films were characterized by measuring the surface resistivity by the four-point probe method. The highest critical temperature T c = 17.86 K was observed for the Nb 3 Sn films annealed at 950°C for 3 h. When the films were annealed above 1000°C for 3 h, Sn evaporation resulted in a Nb-rich film, degrading the superconducting performance. Annealing at 1200°C for 3 h resulted in evaporation of Sn leaving less than 1% Sn on the surface, as detected by energy dispersive spectroscopy, and for that film a T c of 7.9 K was observed.

36 MATERIALS SCIENCE↗

Initial growth of tin on niobium for vapor diffusion coating of Nb 3 Sn

Nb 3 Sn offers significant potential to exceed the performance of niobium for superconducting radio frequency accelerator cavities. The most promising path toward deployment is by tin vapor diffusion coating of Nb cavity interiors via a two step nucleation-then-growth sequence. Reported here is a materials science study of the nucleation process. We manipulated the accessible range of process variables and determined the effect on composition and microstructure using an array of materials characterization tools. Broadly, nucleation deposits tin as a thin surface phase and, under some conditions, as near-micron sized particles as well, resembling Stranski–Krastanov growth. Conditions that impair nucleation promote the formation of defects, such as patches, in subsequent coating growth. Furthermore no significant effect on the subsequently grown coating was found for structures produced during nucleation.

36 MATERIALS SCIENCE↗

RF Results of Nb Coated SRF Accelerator Cavities via HiPIMS

Bulk Niobium (Nb) SRF (superconducting radio frequency) cavities are currently the preferred method for acceleration of charged particles at accelerator facilities around the world. However, bulk Nb cavities have poor thermal conductance and impose material and design restrictions on other components of a particle accelerator. Since the SRF phenomena occurs within a shallow depth of 40 nm (for Nb), a proposed solution to this problem has been to deposit a superconducting Nb thin film on the interior of a cavity made of a suitable alternative material such as copper or aluminum. While this approach has been attempted in the past using DC magnetron sputtering (DCMS), such cavities have never performed at the bulk Nb level. However, new energetic condensation techniques for film deposition offer the opportunity to create suitably thick Nb films with improved density, microstructure and adhesion compared to traditional DCMS. One such technique that has been developed somewhat recently is ?High Power Impulse Magnetron Sputtering? (HiPIMS). Here we report early results from various thin film coatings carried out on 1.3 GHz Cu cavities, a 1.5 GHz Nb cavity, and small Cu coupon samples coated at Jefferson Lab using HiPIMS.

Burton, Matthew Creed↗

New Progress with HF-free Chemical Finishing for Nb SRF Cavities

Jefferson Lab has implemented a bipolar pulsed electropolishing system for final chemical processing of niobium SRF cavities. This FARADAYIC bi-polar electropolishing (BPEP) has been applied to single cells, a 7-cell CEBAF C100 cavity, and to 9-cell TESLA-style cavities.* As a mechanistic characterization of the process emerges, the critical role played by the local current density during each cathodic pulse is becoming clear. This influences system and operational parameter refinement. We present current process parameters, removal characterization, and rf performance of the processed cavities. This is the fruit of collaborative work between Jefferson Lab and Faraday Technology, Inc. directed toward the routine commercialization and industrialization of niobium cavity processing. We also present supporting data from controlled-parameter coupon studies.

Tian, Hui↗

Secondary ion mass spectrometry for superconducting radiofrequency cavity materials

Historically, many advances in superconducting radio frequency (SRF) cavities destined for use in advanced particle accelerators have come empirically, through the iterative procedure of modifying processing and then performance testing. However, material structure is directly responsible for performance. Understanding, the link between processing, structure, and performance will streamline and accelerate the research process. In order to connect processing, structure, and performance, accurate and robust materials characterization methods are needed. Here in this paper, one such method, SIMS, is discussed with focus on analysis of SRF materials. In addition, several examples are presented, showing how SIMS is being used to further understanding of materials based SRF technologies.

43 PARTICLE ACCELERATORS↗