Results for “niobium” — Page 3

DOE OSTI2022

Niobium addition improves the corrosion resistance of TiHfZrNb x high-entropy alloys in Hanks’ solution

High-strength TiHfZrNb x high-entropy alloys could become the ideal materials for small-diameter endovascular stents once their corrosion resistance in the physiological milieu is confirmed. Here, this work aims at evaluating the corrosion resistance of a TiHfZrNb x high-entropy-alloys family in Hanks’ solution at 37 °C and revealing the influence of niobium on the mechanisms of dissolution and passivation. The alloys were subjected to a series of static and dynamic electrochemical tests and surface characterization, employing the static/dynamic/cyclic polarizations, impedance spectroscopy, XPS, AFM, and SEM. Results confirm a higher corrosion resistance of the alloys compared to that of CP-Ti and Ti6Al4V. The addition of niobium considerably improves the microstructural homogeneity that ensures a low dissolution rate and a greater resistance of the film due to the lower concentration of point defects. The passive film behaves as an n-type semiconductor and is composed of a mixture of TiO 2 , Nb 2 O 5 , ZrO 2 , and HfO 2 oxides, with the presence of metallic hydroxides on the outermost layer. A detailed description of the niobium influence on the mechanisms of the dissolution and passivation is presented in this work.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Direct evidence of microstructure dependence of magnetic flux trapping in niobium

Abstract Elemental type-II superconducting niobium is the material of choice for superconducting radiofrequency cavities used in modern particle accelerators, light sources, detectors, sensors, and quantum computing architecture. An essential challenge to increasing energy efficiency in rf applications is the power dissipation due to residual magnetic field that is trapped during the cool down process due to incomplete magnetic field expulsion. New SRF cavity processing recipes that use surface doping techniques have significantly increased their cryogenic efficiency. However, the performance of SRF Nb accelerators still shows vulnerability to a trapped magnetic field. In this manuscript, we report the observation of a direct link between flux trapping and incomplete flux expulsion with spatial variations in microstructure within the niobium. Fine-grain recrystallized microstructure with an average grain size of 10–50 µm leads to flux trapping even with a lack of dislocation structures in grain interiors. Larger grain sizes beyond 100–400 µm do not lead to preferential flux trapping, as observed directly by magneto-optical imaging. While local magnetic flux variations imaged by magneto-optics provide clarity on a microstructure level, bulk variations are also indicated by variations in pinning force curves with sequential heat treatment studies. The key results indicate that complete control of the niobium microstructure will help produce higher performance superconducting resonators with reduced rf losses 1 related to the magnetic flux trapping.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2025

Mitigation of Pitting on Nitrogen-Doped Niobium Surfaces through Two-Step Electropolishing

Surface processing of niobium superconducting RF cavities used in particle accelerators is crucial for determining their performance. The nitrogen (N)-doping method, developed at Fermilab, enhances the cavities’ quality factor by doping the cavity’s interior surface with N atoms at 800 °C. After N-doping, electropolishing (EP) is employed to remove the niobium nitride phases and attain the desired concentration of interstitial N atoms. This study explores the effects of EP conditions on N-doped niobium samples. The samples were electropolished at 5 to 40 °C and voltages between 3 and 22 V. Different EP voltage ranges produced two types of pits, classified based on their sizes. Larger pits, linked to higher voltages, are also affected by the reaction rate. Pitting could be reduced at a lower temperature and adequate EP voltage. However, to effectively minimize gas evolution forming large-sized pitting, peeling off the top nitride layer before EP might be beneficial. This was achieved through precise low-voltage etching, forming a two-step EP process. The process involves removing the top 100–200 nm layer at a low voltage, followed by standard EP to remove the required material. This two-step EP process effectively mitigated the pitting risk associated with gas evolution on N-doped surfaces.

43 PARTICLE ACCELERATORS↗

DOE OSTI2022

Studies on the Fundamental Mechanisms of Niobium Electropolishing

To improve the superconducting performance of niobium SRF cavities, electropolishing (EP) with a sulfuric and hydroflouric acid mixture is used. The chemistry of this reaction is complex due to the interactions between diffusion mechanisms, surface oxide structure, and multiple chemical species. Past studies on the EP process have produced a certain set of optimum parameters that have been used successfully for a long time. However, two recent developments have called the efficacy of the existing EP process into question. Since the introduction of nitrogen doping the surface quality of some cavities has been very poor. Also, EP performed at colder than standard temperatures leads to an increase in the cavity performance. To understand these questions, we perform a multivariate study on the EP process using niobium test samples electropolished at different temperatures and potentials. We find that electropolishing at lower potentials leads to rough surface features such as pitting and grain etching. Some of the surface features show similarities to features seen in niobium cavities. The effect of electropolishing temperature is not clear based on the results of this study.

43 PARTICLE ACCELERATORS↗

DOE OSTI2022

Preliminary Results from Magnetic Field Scanning System for a Single-Cell Niobium Cavity

One of the building blocks of modern particle accelerators is superconducting radiofrequency (SRF) cavities. Niobium is the material of choice to build such cavities, which operate at liquid helium temperature (2 - 4 K) and have some of the highest quality factors found in Nature. There are several sources of residual losses, one of them is trapped magnetic flux, which limits the quality factor in SRF cavities. The flux trapping mechanism depends on different niobium surface preparations and cool-down conditions. Suitable diagnostic tools are not yet available to study the effects of such conditions on magnetic flux trapping. A magnetic field scanning system (MFSS) for SRF cavities using Hall probes and Fluxgate magnetometer has been designed, built, and is commissioned to measure the local magnetic field trapped in 1.3 GHz single-cell SRF cavities at 4 K. In this contribution, we will present the preliminary results from MFSS for a single cell niobium cavity.

Ciovati, G.↗

DOE OSTI2022

Thermal Conductivity of Electroplated Copper Onto Bulk Niobium at Cryogenic Temperatures

Superconducting radio-frequency (SRF) cavities made of high-purity bulk niobium are widely used in modern particle accelerators. The development of metallic outer coatings with high thermal conductivity would have a beneficial impact in terms of improved thermal stability, reduced material cost and for the development of conduction-cooled, cryogen-free SRF cavities. Several high-purity, fine-grain Nb samples have been coated with 2-4 mm thick copper by electroplating. Measurements of the thermal conductivity of the bimetallic Nb/Cu samples in the range 2 ? 7 K showed values of the order of 1 kW/(m K) at 4.3 K. Very good adhesion between copper and niobium was achieved by depositing a thin Cu layer by cold spray on the niobium, prior to electroplating the bulk Cu layer.

Dhakal, P.↗

DOE OSTI2023

INVESTIGATION OF THE MULTILAYER SHIELDING EFFECT THROUGH NbTiN-AlN COATED BULK NIOBIUM

Superconducting radio frequency (SRF) cavities, composed of bulk niobium (Nb), are extensively utilized in particle accelerators. To optimize their performance and extend their operational range, thin films of superconducting materials are applied to the Nb surfaces. This study focuses on investigating the magnetic field penetration characteristics of NbTiN-AlN coating on bulk niobium. The experimental setup involves measuring the magnetic field penetration across flat superconducting samples at cryogenic temperatures. One key parameter of interest is the field just before the first flux penetration, Bp which enables the observation of the multilayer shielding effect on bulk niobium under high magnetic fields. The study reveals a significant enhancement in Bp of the NbTiN-AlN coated Nb samples compared to bare Nb samples. This property holds critical importance for achieving high field performance in SRF cavities. Furthermore, the study explores the relationship between coating thickness and Bp corroborating the theoretical predictions.

Senevirathne, I. H.↗

DOE OSTI2023

THERMODYNAMIC PROPERTIES OF SRF NIOBIUM

Bulk and thin films of niobium are the materials of choice in fabricating superconducting radio frequency (SRF) cavities for modern particle accelerators and quantum computing applications. The thermodynamic properties of Nb are of particular interest in heat management in cryogenic environments. Here, we report the results of measurements of the thermodynamic properties of niobium used in the fabrication of SRF cavities. The temperature and magnetic field dependence of thermal conductivity, Seebeck coefficient, and specific heat capacity was measured on bulk niobium samples.

Dhakal, Pashupati↗

DOE OSTI2021

Study of the niobium oxide structure and microscopic effect of plasma processing on the Nb surface

A study of the niobium oxide structure is presented here, focusing on the niobium suboxides. Multiple steps of argon sputtering and XPS measurements were carried out until the metal surface was exposed. Subsequently, the sample was exposed to air for different time intervals and the oxide regrowth was studied. In addition, three Nb samples prepared with different surface treatments were studied before and after being subjected to plasma processing. The scope is investigating the microscopic effect that the reactive oxygen contained in the glow discharge may have on the niobium surface. This study suggests that the Nb 2 O 5 thickness may increase. Nevertheless, since the Nb 2 O 5 is dielectric, its thickening would not negatively affect the cavity performance.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Study of the Niobium Oxide Structure and Microscopic Effect of Plasma Processing on the Nb Surface

A study of the niobium oxide structure is presented here, focusing on the niobium suboxides. Multiple steps of argon sputtering and XPS measurements were carried out until the metal surface was exposed. Subsequently, the sample was exposed to air for different time intervals and the oxide regrowth was studied. In addition, three Nb samples prepared with different surface treatments were studied before and after being subjected to plasma processing. The scope is investigating the microscopic effect that the reactive oxygen contained in the glow discharge may have on the niobium surface. This study suggests that the Nb 2 O 5 thickness may increase. Nevertheless, since the Nb 2 O 5 is dielectric, its thickening would not negatively affect the cavity performance.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Thermal Conductivity of Electroplated Copper Onto Bulk Niobium at Cryogenic Temperatures

Superconducting radio-frequency (SRF) cavities made of high-purity bulk niobium are widely used in modern particle accelerators. The development of metallic outer coatings with high thermal conductivity would have a beneficial impact in terms of improved thermal stability, reduced material cost and for the development of conduction-cooled, cryogen-free SRF cavities. Several high-purity, fine-grain Nb samples have been coated with 2-4 mm thick copper by electroplating. Measurements of the thermal conductivity of the bimetallic Nb/Cu samples in the range 2 ? 7 K showed values of the order of 1 kW/(m K) at 4.3 K. Very good adhesion between copper and niobium was achieved by depositing a thin Cu layer by cold spray on the niobium, prior to electroplating the bulk Cu layer.

Dhakal, P.↗

DOE OSTI2023

Demonstration of Niobium Tin in 218 MHz Low-beta Quarter Wave Accelerator C

A 218 MHz quarter wave niobium cavity has been fabricated for the purpose of demonstrating Nb3Sn technology on a low-beta accelerator cavity. Niobium-tin has been established as a promising next generation SRF material, but development has focused primarily in high- beta elliptical cell cavities. This material has a significantly higher TC than niobium, allowing for design of higher frequency quarter wave cavities (that are subsequently smaller) as well as for significantly lowered cooling requirements (possibly leading to cryocooler based designs). The fabrication, initial cold testing, and Nb3Sn coating are discussed as well as test plans and details of future applications.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗

DOE OSTI2025

Identifying the connections between grain growth and flux expulsion in low RRR niobium SRF cavities

The SRF community has shown that high temperature annealing can improve the flux expulsion of niobium cavities during cooldown. The required temperature will vary between cavities and different batches of material, typically around 800 C and up to 1000 C. However, for niobium with a low residual resistance ratio (RRR), even 1000 C is not enough to improve its poor flux expulsion. The purpose of this study is to observe the grain growth behavior of low RRR niobium coupons subjected to high temperature annealing to identify the mechanism for improving flux expulsion. We observe that low RRR material experiences less grain growth than high RRR when annealed at the same temperature. We search for the limitations to grain growth in low RRR material and develop a diagnostic based on grain structure to determine the appropriate recipe for good flux expulsion. The results of this study have the potential to unlock a new understanding on SRF materials and enable the next generation of high Q/high gradient surface treatments.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗

DOE OSTI2025

Identifying the Connections between Grain Growth and Flux Expulsion in Low RRR Niobium SRF Cavities

The SRF community has shown that high temperature annealing can improve the flux expulsion of niobium cavities during cooldown. The required temperature will vary between cavities and different batches of material, typically around 800 C and up to 1000 C. However, for niobium with a low residual resistance ratio (RRR), even 1000 C is not enough to improve its poor flux expulsion. The purpose of this study is to observe the grain growth behavior of low RRR niobium coupons subjected to high temperature annealing to identify the mechanism for improving flux expulsion. We observe that low RRR material experiences less grain growth than high RRR when annealed at the same temperature. We search for the limitations to grain growth in low RRR material and develop a diagnostic based on grain structure to determine the appropriate recipe for good flux expulsion. The results of this study have the potential to unlock a new understanding on SRF materials and enable the next generation of high Q/high gradient surface treatments.

Howard, Katrina N. [Chicago U.] (ORCID:00000003256↗

DOE OSTI2025

Development of Niobium-based alloys for Turbine Applications: 20/CJ000/08/09 (ULTIMATE Phase I project)

Current Ni-based alloys used in turbine blade applications are operating at 1100°C which is approximately 90% of the solidus of Ni-based alloys. Further increases in temperature can be achieved only through the use of alloys with higher solidus temperatures such as refractory alloys which include Mo, Nb, W, Ta alloys. Niobium has a unique combination of physical properties that include a high melting point (2468°C), lowest density (8.57 g/cc), and the lowest modulus amongst refractory alloys, a good thermal conductivity that increases from 45 W/mK at room temperature to 62 W/mK at 1093°C, good ductility with fabricability using traditional techniques, high strength, good creep resistance, and general chemical inactivity. Hence niobium alloys offer many advantages for use at the desired temperature of 1300°C. One of the major deterrents to the use of niobium and its alloys at high temperatures is achieving good oxidation resistance. In addition, achieving balanced properties of room temperature strength, ductility, fracture toughness, high temperature strength, and creep resistance required for 1300°C operation at a density of 9 g/cm 3 is extremely challenging since the addition of W which is a potent strengthener increases the density of the alloy. This project seeks to enable the development of a tri-layered turbine blade that can operate continuously at 1300°C with the core of the turbine blade providing good creep resistance, the second layer providing improved oxidation resistance over the core layer, and the third layer being an environmental barrier providing oxidation resistance. The objective of this Phase 1 project was to use computational modeling and advanced characterization tools to develop two classes of Nb alloys which could be used as the core layer and the transition layer.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Identifying the Connections between Grain Growth and Flux Expulsion in Low RRR Niobium SRF Cavities

The SRF community has shown that high temperature annealing can improve the flux expulsion of niobium cavities during cooldown. The required temperature will vary between cavities and different batches of material, typically around 800 C and up to 1000 C. However, for niobium with a low residual resistance ratio (RRR), even 1000 C is not enough to improve its poor flux expulsion. The purpose of this study is to observe the grain growth behavior of low RRR niobium coupons subjected to high temperature annealing to identify the mechanism for improving flux expulsion. We observe that low RRR material experiences less grain growth than high RRR when annealed at the same temperature. We search for the limitations to grain growth in low RRR material and develop a diagnostic based on grain structure to determine the appropriate recipe for good flux expulsion. The results of this study have the potential to unlock a new understanding on SRF materials and enable the next generation of high Q/high gradient surface treatments.

Howard, Katrina [Chicago U.] (ORCID:00000003256133↗

DOE OSTI2026

Identifying the connections between grain growth and flux expulsion in low RRR niobium SRF cavities

The SRF community has shown that high temperature annealing can improve the flux expulsion of niobium cavities during cooldown. The required temperature will vary between cavities and different batches of material, typically around 800 C and up to 1000 C. However, for niobium with a low residual resistance ratio (RRR), even 1000 C is not enough to improve its poor flux expulsion. The purpose of this study is to observe the grain growth behavior of low RRR niobium coupons subjected to high temperature annealing to identify the mechanism for improving flux expulsion. We observe that low RRR material experiences less grain growth than high RRR when annealed at the same temperature. We search for the limitations to grain growth in low RRR material and develop a diagnostic based on grain structure to determine the appropriate recipe for good flux expulsion. The results of this study have the potential to unlock a new understanding on SRF materials and enable the next generation of high Q/high gradient surface treatments.

Howard, K. [Chicago U.] (ORCID:0000000325613308)↗

DOE OSTI2026

Understanding the connections between grain growth and flux expulsion in low RRR niobium SRF cavities

The SRF community has shown that high temperature annealing can improve the flux expulsion of niobium cavities during cooldown. The required temperature will vary between cavities and different batches of material, typically around 800 C and up to 1000 C. However, for niobium with a low residual resistance ratio (RRR), even 1000 C is not enough to improve its poor flux expulsion. The purpose of this study is to observe the grain growth behavior of low RRR niobium coupons subjected to high temperature annealing to identify the mechanism for improving flux expulsion in low RRR cavities. We anneal the low RRR material up to 1200 C to understand the limits of flux expulsion performance. We observe that low RRR material experiences less grain growth than high RRR when annealed at the same temperature. We search for the limitations to grain growth in low RRR material and develop a diagnostic based on grain structure to determine the appropriate recipe for good flux expulsion. The results of this study have the potential to unlock a new understanding on SRF materials and enable the next generation of high Q/high gradient surface treatments.

Howard, K. [Chicago U.]↗