Niobium Samples Research Articles

XPS studies of nitrogen doping niobium used for accelerator applications

Nitrogen doping study on niobium (Nb) samples used for the fabrication of superconducting radio frequency (SRF) cavities was carried out. The samples’ surface treatment was attempted to replicate that of the Nb SRF cavities, which includes heavy electropolishing (EP), nitrogen doping and the subsequent EP with different amounts of material removal. The surface chemical composition of Nb samples with different post treatments has been studied by XPS. The chemical composition of Nb, O, C and N was presented before and after Gas Cluster Ion Beam (GCIB) etching. No signals of poorly superconducting nitrides NbNx was found on the surface of any doped Nb sample with the 2/6 recipe before GCIB etching. However, in the depth range greater than 30 nm, the content of N element is below the XPS detection precision scope even for the Nb sample directly after nitrogen doping treatment with the 2/6 recipe.

Investigation of Trapped Magnetic Flux in Superconducting Niobium Samples with Neutron Radiography

Investigation of Trapped Magnetic Flux in Superconducting Niobium Samples with Neutron Radiography

A magneto-optical study on magnetic flux expulsion and pinning in high-purity niobium

The magnetic flux trapped inside high-purity niobium samples after field cooling was investigated by indirect magneto-optical imaging using an indicator film. The detected magnetic field was compared with the field present during the phase transition, and the distribution of trapped flux was investigated. The measurements were performed on an untreated sample cut from an ingot and a sample that was heated at 1400 °C for 4 h. For untreated niobium, the trapped flux was found to be homogeneously distributed and almost all applied field during phase transition was trapped. In contrast, the heat treated niobium showed significantly reduced trapping. Neither did the grain boundaries play a major role as pinning centers nor did the crystal orientation influence the amount of trapped flux significantly, which is contrary to recent assumptions. However, niobium hydrides, which formed during the cool-down-stage to cryogenic temperatures, were found to enhance trapping considerably.

Hydrogen Reduction in MEP Niobium Studied by Secondary Ion Mass Spectrometry (SIMS)

Niobium, as pure metal and alloying element, is used in a variety of applications, among them in nuclear industries. Niobium is incorporated into nuclear fission reactors due to its enormous strength and low density. Surface finishing of niobium is often performed in electrochemical polishing processes in view of improving its smoothness, corrosion resistance and its surface cleanability. However, the presently used electropolishing process (EP) is intrinsically linked to the subsurface hydrogenation of niobium, which measurably degrades its properties. This is why the annealing operation is used to remove hydrogen from electropolished niobium that is a costly and time-consuming process. The traditional electrolyte consisting of a mixture of 96% H2SO4/49% HF acids by volume in a 9:1 ratio has been substituted for the new one, being a mixture of 70% methanesulfonic acid with 49% hydrofluoric acid by volume in a 3:1 ratio. Moreover, the additional imposition of a magnetic field during the electropolishing process (MEP) further increases hydrogen removal, when compared to the hydrogen content achieved by the electropolishing process alone. The aim of the study is to reveal a methodic approach and showing decreasing hydrogenation of niobium samples after consecutive steps of electrochemical polishing. Secondary ion mass spectrometry (SIMS) was used to measure the hydrogen content in the surface layer of as-received AR niobium and in the samples after EP and MEP processes.

Synthesis and Comparative Study on Intergranular Corrosion Characteristics of Stabilized 5A Grade Cast Duplex Stainless Steel

Abstract In this paper, stabilization using zirconium and niobium was investigated to reduce the effect of intergranular corrosion (IGC) in 5A grade cast duplex stainless steel. Computational thermodynamic software was used to determine the various heat treatment temperatures according to phase precipitation. Resistance to IGC was investigated by oxalic acid etch test and double-loop electrochemical potentiokinetic reactivation (DL-EPR) technique. The surface of the specimens was observed using optical microscopy, scanning electron microscopy, energy dispersive spectroscopy, and X-ray diffractometry to evaluate the presence of various intermetallic phases prone to IGC. Oxalic acid etch test response has indicated the susceptibility, whereas the DL-EPR test has provided the degree of sensitization. The results revealed that zirconium-stabilized samples are more susceptible to IGC compared to the niobium samples. Earlier formation of niobium compounds led to the reduction of intergranular attack in the niobium-stabilized samples.

Positron Annihilation Studies of the Near-Surface Regions of Niobium before and after Wear Treatment

The positron annihilation studies of well-annealed niobium samples after dry sliding or sandblasting are reported. These treatments modify surface and subsurface regions introducing crystalline defects, which are extended beneath the surface of the sample at a depth of about 140 µm for the highest applied load of 50 N. These defects can be identified as dislocations with jogs or vacancies near dislocations. The obtained depth profile of mean positron lifetime reflects the defect depth distribution and exhibits the characteristic plateau near the worn surface, which disappears when lowering of the applied load. A similar depth profile was obtained also for niobium samples after sandblasting. Slow positron beam studies revealed that at the surface of the samples after dry sliding or other treatments some defects that localize positrons are present. Additionally, a large value of positron diffusion length of about 266(33) nm was found for well annealed niobium.

A Model for the Formation of Niobium Structures by anodization

The fluoride use for anodizing electrolytes has been primarily responsible for the formation of nanoporous oxides at valve metals, except aluminum, since it causes a dissolution process. This study presents the formation of an oxide model according to the following anodizing parameters: 100 V, 12.73 mA/cm², room temperature and the niobium samples anodized in niobium oxalate and oxalic acid electrolytes without and with the addition of HF for 5, 30 and 60 min. The anodized samples were analyzed morphologically by scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), atomic force microscopy (AFM) and the hydrophobicity of the samples was assessed by the sessile drop method. The presence of fluor in the niobium oxalate electrolyte formed oxides with lower a dissolution and a low hydrophobicity compared to the one formed in oxalic acid was attributed to the incorporation of niobium and oxalate ions. Thereby, the model proposed in this paper showed that during anodization the migration of the fluoride ion into the oxide occurs at high speed, which results in the formation of microcones, leading to the formation of discrete layers of porous oxide.

Optical investigation of niobium properties: Electrical- and physical constants

In this paper, we report optical (reflectance) measurements and investigations of optical properties of electropolished (EP), buffered chemical polished (BCP), and as-received (AR) from vendor niobium (Nb) samples typically used for fabrication of superconducting radio frequency (SCRF) cavities. Optical conductivity (σ(0), approximated near zero frequency) of EP (σ(0) ∼ 9 × 103Ω−1 cm−1) sample is one order of magnitude higher than that of BCP (σ(0) ∼ 7 × 102Ω−1 cm−1) and AR (σ(0) ∼ 3 × 102Ω−1 cm−1) niobium samples. Furthermore, physical constants of electropolished Nb-SCRF materials such as concentration of conduction electrons ( ∼ 1.8 × 1022electrons/cm3), average velocity ( ∼ 5.9 × 107cm/s) of the electrons on the Fermi surface, and mean free path ( ∼ 0.53 nm) were also found to be considerably higher than that of the BCP and the AR samples. The depth of electric field penetration (in low frequency region) in the electropolished Nb sample ( ∼ 80 nm) is appreciably lesser than the BCP ( ∼ 450 nm) and the AR ( ∼ 400 nm) samples.

Equilibrium properties of superconducting niobium at high magnetic fields: A possible existence of a filamentary state in type-II superconductors

The standard interpretation of the phase diagram of type-II superconductors was developed in 1960s and has since been considered a well-established part of classical superconductivity. However, upon closer examination a number of fundamental issues arise that leads one to question this standard picture. To address these issues we studied equilibrium properties of niobium samples near and above the upper critical field Hc2 in parallel and perpendicular magnetic fields. The samples investigated were very high quality films and single crystal discs with the Ginzburg-Landau parameters 0.8 and 1.3, respectively. A range of complementary measurements have been performed, which include dc magnetometry, electrical transport, muSR spectroscopy and scanning Hall-probe microscopy. Contrarily to the standard scenario, we observed that a superconducting phase is present in the sample bulk above Hc2 and the field Hc3 is the same in both parallel and perpendicular fields. Our findings suggest that above Hc2 the superconducting phase forms filaments parallel to the field regardless on the field orientation. Near Hc2 the filaments preserve the hexagonal structure of the preceding vortex lattice of the mixed state and the filament density continuously falls to zero at Hc3. Our work has important implications for the correct interpretation of properties of type-II superconductors and can also be essential for practical applications of these materials.

Emissivity of Elgiloy and pure niobium at high temperature for the Solar Orbiter mission

The science payload of the Solar Orbiter mission that will be launched in 2018 comprises the RPW (Radio and Plasma Waves) experiment that will perform in situ and remote-sensing measurements (magnetic and electric fields). Some parts of this instrument will be made of Elgiloy for the antennas and must be protected from the intense solar radiation by a heat shield made in niobium. Emissivity of both materials is important to know in order to correctly model before launch the heat transfer in the instrumentation. Hemispherical emissivity results in the two following wavelength ranges 0.6–2.8 and 0.6–40 μm are presented at temperatures up to 1500 K for these two materials according to their surface roughness particularly for the niobium samples and at room temperature in the wavelength range 0.25–25 μm. New original data are obtained for both the materials at high temperature.

Attempts to test an alternative electrodynamic theory of superconductors by low-temperature scanning tunneling and atomic force microscopy

We perform an experiment to test between two theories of the electrodynamics of superconductors: the standard London theory and an alternative proposed by J. E. Hirsch [Phys. Rev. B 69, 214515 (2004)]. The two alternatives give different predictions with respect to the screening of an electric field by a superconductor, and we try to detect this effect using atomic force microscopy on a niobium sample. We also perform the reverse experiment, where we demonstrate a superconductive tip mounted on a qPlus force sensor. Due to limited accuracy, we are able neither to prove nor to disprove Hirsch's hypothesis. Within our accuracy of 0.17 N/m, the superconductive transition does not alter the atomic-scale interaction between tip and sample.

Reflected electron-energy-loss spectra, differential inverse inelastic mean free paths, and angular resolved X-ray photoelectron spectra of a niobium sample

A technique for recovering the differential inverse inelastic mean free paths (DIIMFP) of electrons in Nb from the reflected electron energy loss spectra (REELS) at initial energies of 5 to 40 keV using a threelayer model of the sample surface is presented. The recovered DIIMFP are used for analyzing X-ray photoelectron spectra measured at different viewing angles. Comparison with experimental data is carried out.

First Results of Cavitation Erosion Behavior of Plasma Nitrided Niobium: Surface Modification

This work presents the first results of the plasma nitriding study performed in pure niobium in order to increase its cavitation erosion resistance. Samples were prepared from 98.9% purity and 90% reduction cold-rolled niobium bars. Annealing treatment of the cold-worked niobium samples was carried out in vacuum furnace at 1.33 Pa pressure, in the temperature of 1000 °C, for a time of 60 min. Annealed samples showing hardness of 80 HV were cut to dimensions of 20 × 30 × 4 mm3. Nitriding treatment was conducted at 1080 °C, gas mixture of 90% N2 + 10% H2, flow rate of 5 × 10–6 Nm3s–1, and pressure of 1200 Pa (9 Torr), for a total time of 4 h comprised by two treatment steps of 2 h each. For comparison purpose, results for nitrided and non-nitrided niobium are confronted. Samples were characterized by XRD, nanoindentation, microhardness, SEM, and 2D surface topography and 3D interferometry profile analysis techniques. Cavitation testing was conducted according to ASTM G32-09. Comparatively, promising results based on the formation of niobium nitride phases in treated surfaces are presented and discussed in the present work.

Porous titanium and Ti-35Nb alloy: effects on gene expression of osteoblastic cells derived from human alveolar bone.

Tests on titanium alloys that possess low elastic modulus, corrosion resistance and minimal potential toxicity are ongoing. This study aimed to evaluate the behavior of human osteoblastic cells cultured on dense and porous Titanium (Ti) samples comparing to dense and porous Ti-35 Niobium (Ti-35Nb) samples, using gene expression analysis. Scanning electronic microscopy confirmed surface porosity and pore interconnectivity and X-ray diffraction showed titanium beta-phase stabilization in Ti-35Nb alloy. There were no differences in expression of transforming growth factor-β, integrin-β1, alkaline phosphatase, osteopontin, macrophage colony stimulating factor, prostaglandin E synthase, and apolipoprotein E regarding the type of alloy, porosity and experimental period. The experimental period was a significant factor for the markers: bone sialoprotein II and interleukin 6, with expression increasing over time. Porosity diminished Runt-related transcription factor-2 (Runx-2) expression. Cells adhering to the Ti-35Nb alloy showed statistically similar expression to those adhering to commercially pure Ti grade II, for all the markers tested. In conclusion, the molecular mechanisms of interaction between human osteoblasts and the Ti-35Nb alloy follow the principal routes of osseointegration of commercially pure Ti grade II. Porosity impaired the route of transcription factor Runx-2.

Study of impurity distribution in mechanically polished, chemically treated and high vacuum degassed pure niobium samples using the TOFSIMS technique

The performance of superconducting radio frequency (SRF) cavities is strongly influenced by various impurities within the penetration depth (∼50 nm) of niobium (Nb), which in turn depends on the applied surface treatments. The effect of these surface treatments on the impurities of Nb has been explored using various surface analytical techniques. However, the results are still inadequate in many aspects and the effect of sequential SRF treatments on the impurity distribution has not been explored. The present study analyzes various impurities within the penetration depth of Nb samples, treated by SRF cavity processing techniques such as colloidal silica polishing (simulating centrifugal barrel polishing), buffer chemical polishing (BCP), high pressure rinsing (HPR) and degassing under a high vacuum (HV) condition at 600 °C for 10 h. Static, dynamic and slow sputtering modes of the time of flight secondary ion mass spectrometry (TOFSIMS) technique were employed to study the effect of the above treatments on interstitial impurities, hydrocarbons, oxides, acidic residues, reaction products and metallic contaminations. The study confirms that the impurity distribution in Nb is not only sensitive to the surface treatments, but also to their sequence. Varying the treatment sequence prior to HV degassing treatments affected the final impurity levels in HV degassed bulk Nb samples. The HV degassing treatment was capable of reducing hydrogen contamination, but oxygen, carbon and metallic impurities were introduced into bulk Nb due to poor isolation from furnace contamination. On the other hand, BCP treated samples exhibited minimum hydrocarbon and metallic contamination along with the thinnest oxide layer at ∼2.8 nm, but led to extensive contamination of the oxide layer with residuals and reaction products of acids used in the BCP solution. HPR treatment, on the other hand, was effective in reducing the acidic impurities on the top surface. Variability of the distribution of impurities on samples as a function of SRF treatments was also discussed.

Syntesis of Niobium Nitride Using Cryogenic Milling

In the present paper a preliminary study was performed on the influence of mechanical milling on the synthesis of niobium nitrade. The niobium metal powder sample, passing # 635 mesh sieve, was processed by mechanical milling in SPEX mill for 8 hours using a ball-to-powder ratio of 7:1 and a nitrogen atmosphere. The powder was annealed at different temperatures, 900 °C, 1000 °C, 1100 °C and 1200 °C for 1 hour in a hydrogen and argon atmosphere to study their crystallization, which then were formed into blanks for analysis of the compressibility curves. These samples were also subjected to X-ray diffraction and the data were compared between the annealing temperatures. The compressibility curves of niobium samples with and without grinding were also evaluated, showing high compacting capacity. These samples were subjected to X-ray diffraction and X-ray fluorescence. As the formation of nitrides (Nb2N) was observed in SPEX type mill, the interest in studying the synthesis of nitrides came up, using mechanical milling in Attritor type mill. Same previous results of Attritor processing indicate a Nb2N and NbN synthesis after annealing treatments.

Influence of electropolishing and anodic oxidation on morphology, chemical composition and corrosion resistance of niobium

The work presents results of the studies performed on electropolishing of pure niobium in a bath that contained: sulphuric acid, hydrofluoric acid, ethylene glycol and acetanilide. After the electropolishing, the specimens were subjected to anodic passivation in a 1moldm−3 phosphoric acid solution at various voltages. The surface morphology, thickness, roughness and chemical composition of the resulting oxide layers were analysed. Thusly prepared niobium samples were additionally investigated in terms of their corrosion resistance in Ringer's solution. The electropolished niobium surface was determined to be smooth and lustrous. The anodisation led to the growth of barrier-like oxide layers, which were enriched in phosphorus species.

Temperature dependence of clusters with attracting vortices in superconducting niobium studied by neutron scattering

We investigated the intermediate mixed state of a superconducting niobium sample using very small angle neutron scattering. We show that this state is stabilized through a sequence where a regular vortex lattice appears, which then coexists with vortex clusters before vanishing at low temperature. Vortices in clusters have a constant periodicity regardless of the applied field and exhibit a temperature dependence close to the one of the penetration depth. The clusters disappear in the high temperature limit. All the results agree with an explanation in terms of vortex attraction due to non-local effects and indicate a negligible role for pinning. Phase coexistence between the Abrikosov vortex lattice and vortex clusters is reported, showing the first-order nature of the boundary line.

Magnetic field distribution and characteristic fields of the vortex lattice for a clean superconducting niobium sample in an external field applied along a three-fold axis

The field distribution in the vortex lattice of a pure niobium single crystal with an external field applied along a three-fold axis has been investigated by the transverse-field muon-spin-rotation (TF-$\mu$SR) technique over a wide range of temperatures and fields. The experimental data have been analyzed with the Delrieu's solution for the form factor supplemented by phenomenological formulas for the parameters. This has enabled us to experimentally establish the temperatures and fields for the Delrieu's, Ginzburg-Landau's, and Klein's regions of the vortex lattice. Using the numerical solution of the quasiclassical Eilenberger's equation the experimental results have been reasonably understood. They should apply to all clean BCS superconductors. The analytical Delrieu's model supplemented by phenomenological formulas for its parameters is found to be reliable for analyzing TF-$\mu$SR experimental data for a substantial part of the mixed phase. The Abrikosov's limit is contained in it.

Formation of laser-induced periodic surface structures on niobium by femtosecond laser irradiation

The surface morphology of a Niobium sample, irradiated in air by a femtosecond laser with a wavelength of 800 nm and pulse duration of 100 fs, was examined. The period of the micro/nanostructures, parallel and perpendicularly oriented to the linearly polarized fs-laser beam, was studied by means of 2D Fast Fourier Transform analysis. The observed Laser-Induced Periodic Surface Structures (LIPSS) were classified as Low Spatial Frequency LIPSS (periods about 600 nm) and High Spatial Frequency LIPSS, showing a periodicity around 300 nm, both of them perpendicularly oriented to the polarization of the incident laser wave. Moreover, parallel high spatial frequency LIPSS were observed with periods around 100 nm located at the peripheral areas of the laser fingerprint and overwritten on the perpendicular periodic gratings. The results indicate that this method of micro/nanostructuring allows controlling the Niobium grating period by the number of pulses applied, so the scan speed and not the fluence is the key parameter of control. A discussion on the mechanism of the surface topology evolution was also introduced.