Trialkyl-dihalotantalum and niobium compounds Patent
Organometallic compounds of niobium and tantalum useful for film deposition
Juvinall, G. L.↗
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Reclamation of niobium compounds from ionic liquid electrochemical polishing of superconducting radio frequency cavities
Recent research has shown that choline chloride (vitamin B4)-based solutions can be used as a greener alternative to acid-based electrochemical polishing solutions. This study demonstrated a successful method for electrochemical deposition of niobium compounds onto the surface of copper substrates using a novel choline chloride-based ionic liquid. Niobium ions present in the ionic liquid solution were dissolved into the solution prior to deposition via electrochemical polishing of solid niobium. A black coating was clearly visible on the surface of the Cu following deposition. This coating was analyzed using scanning electron microscopy (SEM), electron dispersive X-ray spectroscopy (EDX), atomic force microscopy (AFM), and X-ray fluorescence spectroscopy (XRF). This ionic liquid-based electrochemical deposition method effectively recycles previously dissolved niobium from electrochemical polishing of superconducting radio frequency (SRF) cavities.
36 MATERIALS SCIENCE↗
Electron-Activated Carbon Diffusion in Niobium Compounds for RF Superconductivity
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Garwin, E.↗
Sigma-bonded alkyl compounds of niobium and tantalum - trimethyldichloroniobium and trimethyldichlorotantalum.
Synthesis and formula determination of sigma bonded trimethyldichloroniobium and trimethyldichlorotantalum
TANTALUM COMPOUND↗
Thermoelectric properties of Nb3SbxTe7-x compounds
Niobium antimony telluride, Nb3Sbx,Te7-x, was synthesized and tested for thermoelectric properties in the Thermoelectrics group at the Jet Propulsion Laboratory. The forty atoms per unit cell of Nb3Sb2Te5 and its varied mixture of atoms yield acomplicated structure, suggesting that Nb3Sb2Te5 and related compounds may exhibit low thermal conductivity and hence a higher ZT value. Nb3SbxTe7-x, compounds were synthesized and subsequently analyzed for their Seebeck voltage, heat conduction, and electrical resistivity. Results indicate that Nb3Sb2Te5 is a heavily doped semiconductor whose thermoelectric properties are compromised by compensating n-type and p-type carriers. Attempts to dope in favor of either carrier by varying the Sb:Te ratio yielded samples containing secondary metallic phases that dominated the transport properties of the resulting compounds.
thermoelectric power generation segmented↗
Study of properties of high-field superconductors at elevated temperatures Final technical report, 27 Apr. - 26 Aug. 1966
Properties of high field superconductors at high temperatures - magnetization experiments on niobium and niobium compounds
NIOBIUM COMPOUND↗
Structural characterization and Curie temperature determination of a sodium strontium niobate ferroelectric nanostructured powder
The Curie temperature and its correlation with the magnitude of the displacement of the niobium atom from the center of [NbO{sub 6}] octahedra in NaSr{sub 2}Nb{sub 5}O{sub 15} nanostructured powder were investigated. A single powder was prepared by high-energy ball milling. A powder with an average crystallite size of 37 nm was prepared by calcining the precursor at 1423 K. The refinement of the structural parameters was carried out by the Rietveld method. NaSr{sub 2}Nb{sub 5}O{sub 15} exhibits tetragonal symmetry with the tungsten bronze structure (a=b=12.3495 (6) A, c=3.8911 (2) A, V=593.432 (5) A{sup 3}, and Z=2). The site occupancy of the Na{sup +} and Sr{sup 2+} cations and the interatomic distances between the niobium and oxygen atoms were derived. The [NbO{sub 6}] octahedron undergoes both rotation and tilting depending on the crystallographic site. The Curie temperature of the powder was derived using both the impedance and infrared spectroscopy methods. -- Graphical abstract: Representation of the unit cell of the NaSr2Nb5O15 powder. Nb{sup 5+} cations are differentiated as Nb(I) and Nb(II). [Nb(I)O6] octahedral sites are represented by yellow color and [Nb(II)O6] by blue ones. Display Omitted highlights: > Spontaneous polarization has been based on the off-center displacement of atoms. > Distortion of the [Nb(II)O{sub 6}] octahedra occurs due to both to [NbO{sub 6}] octahedron rotation and tilting. > Newest another equation to derive the parameter Curie's temperature. > The ferroelectric transition in the NaSr{sub 2}NaNb{sub 5}O{sub 15} powder is of displacive type.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Ga lithography in sputtered niobium for superconductive micro and nanowires
This work demonstrates the use of focused ion beam (FIB) implanted Ga as a lithographic mask for plasma etching of Nb films. Using a highly collimated Ga beam of a FIB, Nb is implanted 12 nm deep with a 14 nm thick Ga layer providing etch selectivity better than 15:1 with fluorine based etch chemistry. Implanted square test patterns, both 10 μm by 10 μm and 100 μm by 100 μm, demonstrate that doses above than 7.5 × 10{sup 15 }cm{sup −2} at 30 kV provide adequate mask protection for a 205 nm thick, sputtered Nb film. The resolution of this dry lithographic technique is demonstrated by fabrication of nanowires 75 nm wide by 10 μm long connected to 50 μm wide contact pads. The residual resistance ratio of patterned Nb films was 3. The superconducting transition temperature (T{sub c}) = 7.7 K was measured using a magnetic properties measurement system. This nanoscale, dry lithographic technique was extended to sputtered TiN and Ta here and could be used on other fluorine etched superconductors such as NbN, NbSi, and NbTi.
77 NANOSCIENCE AND NANOTECHNOLOGY↗
Nonresonant valence-to-core x-ray emission spectroscopy of niobium
The valence-to-core (V2C) portion of x-ray emission spectroscopy (XES) measures the electron states close to the Fermi level. These states are involved in bonding, thus providing a measure of the chemistry of the material. For this paper, we show the V2C XES spectra for several niobium compounds. The Kβ" peak in the V2C XES results from the transition of a ligand 2s electron into the 1s core-hole of the niobium, a transition allowed by hybridization with the niobium 4p . This location in energy of this weak peak shows a strong ligand dependence, thus providing a sensitive probe of the ligand environment about the niobium.
36 MATERIALS SCIENCE↗
Preparation, crystal structure, and superconductive characteristics of new oxynitrides (Nb{sub 1-x}M{sub x})(N{sub 1-y}O{sub y}) where M=Mg, Si, and x{approx}y
New niobium oxynitrides containing either magnesium or silicon were prepared at 1000 deg. C by ammonia nitridation of oxide precursors obtained via the citrate route. The products had rock-salt type crystal structures. Crystallinity was improved by annealing in 0.5 MPa N{sub 2} and the final compositions were (Nb{sub 0.95}Mg{sub 0.05})(N{sub 0.92}O{sub 0.08}) at 1500 deg. C and (Nb{sub 0.87}Si{sub 0.09{open_square}0.04})(N{sub 0.87}O{sub 0.13}) at 1200 deg. C. The magnesium and oxide ions partially co-substitute the niobium and nitride ions in the octahedral sites of the {delta}-NbN lattice, respectively. Silicon ions were also successfully doped together with oxide ions into the rock-salt type NbN lattice. The Si doped product exhibited relatively large displacement at the octahedral sites and was accompanied by a small amount of cation vacancies. Superconductivity was improved by annealing to obtain critical temperatures/volume fractions of T{sub c}=17.6 K/100% for Mg- and T{sub c}=16.2 K/95% for the Si-doped niobium oxynitrides. - Graphical Abstract: Doped silicon ions substituting Nb in (Nb{sub 0.87}Si{sub 0.09{open_square}0.04})(N{sub 0.87}O{sub 0.13}) introduced a large displacement at the 4a site mainly because of the accompanied vacancy. The silicon ions may also be slightly shifted from the regular octahedral 4a site (green) towards the interstitial tetrahedral site (red) statistically in the rock-salt type lattice. Highlights: > New superconducting niobium oxynitrides containing either magnesium or silicon were prepared. > Their annealed products had chemical compositions of (Nb{sub 0.95}Mg{sub 0.05})(N{sub 0.92}O{sub 0.08}) and (Nb{sub 0.87}Si{sub 0.09{open_square}0.04})(N{sub 0.87}O{sub 0.13}) in the rock-salt type structure. > Their superconductivities were T{sub c}/volume fraction=17.6 K/100% and 16.2 K/95%, respectively.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Production of High Purity Niobium Ingots at CBMM
CBMM is a fully integrated company, from the mine to the end line of the production chain, supplying different niobium products to the world market: ferroniobium, nickelniobium, niobium pentoxide and high purity metallic niobium. This high purity metallic niobium has long been known to exhibit superconductivity below 9.25 Kelvin. This characteristic has the potential to bring technological benefits for many different areas such as medicine, computing and environment. This paper presents the raw material requirements as well as CBMM experience on producing high purity niobium ingots. The results prove that CBMM material can be the best solution for special applications such as low cost superconductive radiofrequency cavities.
36 MATERIALS SCIENCE↗
Modulation periodicity dependent structure, stress, and hardness in NbN/W{sub 2}N nanostructured multilayer films
NbN/W{sub 2}N nano-multilayer films with a modulation periodicity, {Lambda}, ranging from 5.1 to 157.4 nm have been deposited on a Si(100) substrate by reactive magnetron sputtering in Ar/N{sub 2} mixtures. The {Lambda} dependent structural and mechanical properties for the resulting NbN/W{sub 2}N multilayers have been evaluated by means of low-angle x-ray reflectivity, x-ray diffraction, high-resolution transmission electron microscope, and nanoindentation measurements. The finding is that for films with {Lambda}{<=} 10.6 nm, fcc NbN layers are coherent with cubic W{sub 2}N layers, resulting in NbN layers and W{sub 2}N layers that are in the compressive and tensile states, respectively. In contrast, as {Lambda} is larger than 10.6 nm, a phase transition from W{sub 2}N to W occurs in the W{sub 2}N layer, which is a result of the coherent interface strain relaxation. For this case, all layers are in the compressive state, and the coherent interface disappears. The intrinsic compressive stress evolution with {Lambda} can be interpreted in terms of interface stress. The formation of coherent interface at small {Lambda} ({<=}10.6 nm) is helpful for releasing point defects in layers, leading to a low compressive stress ({<=}1.1 GPa). The hardness for the obtained multilayer film increases with decreasing {Lambda}, and approaches a maximum value of 43.7 GPa when {Lambda} is 7.4 nm. The maximum strengthen at lower {Lambda} is mainly attributed to coherent interface stresses and the modulus difference between the NbN and W{sub 2}N layers. The increase in hardness with a decrease in {Lambda} is interpreted by the Lehoczky model.
36 MATERIALS SCIENCE↗
Self-selection bipolar resistive switching phenomena observed in NbON/NbN bilayer for cross-bar array memory applications
In this letter, to integrate bipolar resistive switching cells into cross bar array (CBA) structure, we study one-selector (1S) and one-resistor (1R) behavior of a niobium oxynitride (NbON) and niobium nitride (NbN) bilayer for the applications of resistive random access memory (RRAM). In this structure, a NbN layer exhibits bipolar switching characteristics while a NbON layer acts as the selector. The NbN-based 1S1R devices within a single RRAM memory cell can be directly integrated into a CBA structure without the need of extra diodes; this can significantly reduce the fabrication complexity.
71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
Synthesis, structure and electrical properties of Cu{sub 3.21}Ti{sub 1.16}Nb{sub 2.63}O{sub 12} and the CuO{sub x}-TiO{sub 2}-Nb{sub 2}O{sub 5} pseudoternary phase diagram
Subsolidus phase relations in the CuO{sub x}-TiO{sub 2}-Nb{sub 2}O{sub 5} system were determined at 935 deg. C. The phase diagram contains one new phase, Cu{sub 3.21}Ti{sub 1.16}Nb{sub 2.63}O{sub 12} (CTNO) and one rutile-structured solid solution series, Ti{sub 1-3x}Cu{sub x}Nb{sub 2x}O{sub 2}: 0<x<0.2335 (35). The crystal structure of CTNO is similar to that of CaCu{sub 3}Ti{sub 4}O{sub 12} (CCTO) with square planar Cu{sup 2+} but with A site vacancies and a disordered mixture of Cu{sup +}, Ti{sup 4+} and Nb{sup 5+} on the octahedral sites. It is a modest semiconductor with relative permittivity {approx}63 and displays non-Arrhenius conductivity behavior that is essentially temperature-independent at the lowest temperatures. - Graphical abstract: The CuO{sub x}-TiO{sub 2}-Nb{sub 2}O{sub 5} phase diagram was determined at 935 deg. C and contains one new phase, Cu{sub 3.21}Ti{sub 1.16}Nb{sub 2.63}O{sub 12}, pictured, a modest semiconductor with {epsilon}{sub r}{approx}63, and one rutile-structured solid solution series, Ti{sub 1-3x}Cu{sub x}Nb{sub 2x}O{sub 2}. Highlights: > Subsolidus phase relations in the CuO{sub x}-TiO{sub 2}-Nb{sub 2}O{sub 5} system were determined at 935 deg. C. > A new phase, Cu{sub 3.21}Ti{sub 1.16}Nb{sub 2.63}O{sub 12} (CTNO), was found with a CaCu{sub 3}Ti{sub 4}O{sub 12}-like crystal structure. > We discovered one rutile-structured solid solution series, Ti{sub 1-3x}Cu{sub x}Nb{sub 2x}O{sub 2}: 0<x<0.2335 (35). > CTNO has square planar Cu{sup 2+}, A site vacancies and Cu{sup +}, Ti{sup 4+} and Nb{sup 5+} disordered on octahedral sites. > CTNO is a modest semiconductor with relative permittivity {approx}63.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Transport properties in semiconducting NbS{sub 2} nanoflakes
The electronic transport properties in individual niobium disulphide (NbS{sub 2}) nanoflakes mechanically exfoliated from the bulk crystal with three rhombohedral (3R) structure grown by chemical vapor transport were investigated. It is found that the conductivity values of the single-crystalline nanoflakes are approximately two orders of magnitude lower than that of their bulk counterparts. Temperature-dependent conductivity measurements show that the 3R-NbS{sub 2} nanoflakes exhibit semiconducting transport behavior, which is also different from the metallic character in the bulk crystals. In addition, the noncontinuous conductivity variations were observed at the temperature below 180 K for both the nanoflakes and the bulks, which is attributed to the probable charge density wave transition. The photoconductivities in the semiconducting nanoflakes were also observed under the excitation at 532 nm wavelength. The probable mechanisms resulting in the different transport behaviors between the NbS{sub 2} nanostructure and bulk were discussed.
77 NANOSCIENCE AND NANOTECHNOLOGY↗
Superconductivity in quaternary niobium oxynitrides containing main group elements (M=Mg, Al, Si)
Niobium compounds continue to be an interesting family of superconductors, with the recent addition of oxynitrides to it, which can be categorized as low-T{sub c} superconductors (LTS) because they exhibit superconductivity below T{sub c}{approx}17 K. In this paper, we report the superconducting properties of three members of the family of niobium oxynitrides, viz. (Nb{sub 0.89}Al{sub 0.11})(N{sub 0.84}O{sub 0.16}), (Nb{sub 0.95}Mg{sub 0.05})(N{sub 0.92}O{sub 0.08}) and (Nb{sub 0.87}Si{sub 0.09}{open_square}{sub 0.04})(N{sub 0.87}O{sub 0.13}). Low temperature dc and ac magnetization measurements have been performed. In addition, heat capacity has been recorded at low temperature under applied magnetic fields. A detailed analysis of the data is presented. - Graphical abstract: The doped Si oxide accompanied with some amount of cation vacancy in cubic NbN lattice induces relatively large magnetic hysteresis on isothermal hysteresis loops at 5 K of the dc magnetization up to 5 T among the four niobium oxynitrides containing main group elements, Nb{sub 1.00}(N{sub 0.98}O{sub 0.02}); (Nb{sub 0.95}Mg{sub 0.05})(N{sub 0.92}O{sub 0.08}); (Nb{sub 0.89}Al{sub 0.11})(N{sub 0.84}O{sub 0.16}), and (Nb{sub 0.87}Si{sub 0.09}{open_square}{sub 0.04})(N{sub 0.87}O{sub 0.13}). Highlights: Black-Right-Pointing-Pointer Three Nb-oxynitrides doped either with Si, Al, Mg were bulk superconductors below {approx}17 K. Black-Right-Pointing-Pointer The cation vacancies induced by doping silicon act as pinning centers. Black-Right-Pointing-Pointer The Si-doped sample had strong electron correlations.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Exfoliation and thermal transformations of Nb-substituted layered titanates
Single-layer Nb-substituted titanate nanosheets of ca. 1 nm thickness were obtained by exfoliating tetrabutylammonium (TBA)-intercalated Nb-substituted titanates in water. AFM images and turbidity measurements reveal that the exfoliated nanosheets crack and corrugate when sonicated. Upon heating, the thermal transformation into anatase and further to rutile is retarded. This suppression of the phase transition upon higher valent substitution may promote technological applications of anatase thin films, hereunder development of films with TCO properties. Depending on the oxygen partial pressure during the transformation, the Nb-substitution into TiO{sub 2} provokes different defect situations and also electronic properties. At reducing conditions, Nb is incorporated as Nb{sup V} and an equivalent amount of Ti{sup IV} is transformed to Ti{sup III} as evidenced by XPS. Magnetic susceptibility data show accordingly paramagnetic behavior. For samples heated in air Ti{sup IV} and Nb{sup V} cations prevail, the latter is compensated by cation vacancies. {sup 93}Nb MAS NMR data prove that Nb is finely dispersed into the transformed (Ti,Nb)O{sub 2} oxide matrices without sign of Nb{sub 2}O{sub 5} (nano)precipitates. The Nb-O-Ti bonds and defects at cation sites are considered key factors for increasing the transformation temperatures for conversion of the nanosheets to anatase and finally into rutile. It is further tempting to link the delay in crystallization to morphology limitations originating from the nanosheets. The present work shows that layered Nb-titanates are appropriate precursors for formation of highly oriented Nb-substituted anatase thin films via delamination, reconstruction and subsequent heat treatment. - Graphical abstract: Layered Nb-titanates are appropriate precursors for formation of highly oriented Nb-substituted anatase thin films via delamination, reconstruction and subsequent heat treatment. Highlights: Black-Right-Pointing-Pointer Single layer Nb-substituted nanosheets were obtained by exfoliation of layered titanates. Black-Right-Pointing-Pointer Nb(V) successfully introduced into anatase and rutile solid solutions. Black-Right-Pointing-Pointer Anatase obtained from reconstructed nanosheets exhibit enhanced thermal stability. Black-Right-Pointing-Pointer Oxygen partial pressure influences the valence of Nb in heat-treated samples. Black-Right-Pointing-Pointer Deposition of oriented thin Ti(Nb)O{sub 2} layers by spray coating was demonstrated.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗