改进铜铌溅射型QWR超导腔性能的探讨

通过直流偏压二级溅射方法，在无氧铜腔体表面溅射一层铌膜，研制了铜铌溅射型射频超导1/4波长谐振腔(quarter wave resonator,QWR)，该腔主要用于重离子的加速，是北京放射性核束装置中后加速部分的预研项目.目前国际上很多实验室都在研究进一步提高铜铌溅射型QWR超导腔的性能，通过多种方法的实验研究，发现在无氧铜衬底与铌膜之间加入一层氮 化铌（NbN）薄膜，可以使得表面铌膜的超导温度转变点由原来的8.8K提高到了接近9.6K ，该方法有可能成为提高QWR腔加速性能的重要途径，目前进一步研究正 关键词： 溅射 QWR超导腔 氮化铌NbN 超导温度     

Effects of substrate temperature on properties of NbNx films grown on Nb by pulsed laser deposition

NbN_x films were deposited on Nb substrate using pulsed laser deposition. The effects of substrate deposition temperature, from room temperature to 950 °C, on the preferred orientation, phase, and surface properties of NbN_x films were studied by X-ray diffraction, atomic force microscopy, and electron probe micro analyzer. We find that the substrate temperature is a critical factor in determining the phase of the NbN_x films. For a substrate temperature up to 450 °C the film showed poor crystalline quality. With temperature increase the film became textured and for a substrate temperature of 650−850 °C, mix of cubic δ-NbN and hexagonal phases (β-Nb₂N + δ′-NbN) were formed. Films with a mainly β-Nb₂N hexagonal phase were obtained at deposition temperature above 850 °C. The c/a ratio of β-Nb₂N hexagonal shows an increase with increased nitrogen content. The surface roughness of the NbN_x films increased as the temperature was raised from 450 to 850 °C.     

Structure evolution and stoichiometry control of Pb(Zr, Ti)O3 thick films fabricated by electrospray assisted vapour deposition

Well-crystallized and stoichiometric Pb(Zr, Ti)O₃ (PZT) films, typically ∼5 μm thick, with pure perovskite-type rhombohedral structures have been successfully prepared via an electrospray assisted vapour deposition (ESAVD) method. Control of the deposition temperature within a narrow range of 300-400 °C resulted in films with the most desirable phases. PZT films with close stoichiometric match with the expected composition ratio and uniform element distribution were obtained by adding the appropriate levels of excess Pb in the precursor solutions. The annealed films were uniform, dense, compact and adherent to the substrates. The dielectric constant, ?_r, and loss tangent, tan δ, of the fabricated PZT films measured at 10 kHz were 442 and 0.09, respectively. The ESAVD deposited PZT films showed a remanent polarization, P_r, of 15.3 μC/cm² and coercive field, E_c, of 86.7 kV/cm. These results demonstrate the clear potential of the ESAVD method as a promising technique for the fabrication of thick PZT films.     

An AES investigation of aluminum,Al oxide and Al nitride thin films

The aluminum-L₂₃VV Auger spectra for elemental Al, Al oxide and Al nitride have been measured in an assessment of the utility of Auger spectroscopy in characterizing thin oxidized Al films used in model supported-metal catalyst studies. Clearly distinct spectra were found for the three surface chemical states. The oxide spectrum was shown to be similar to published spectra from bulk, single-crystalline Al₂O₃. Complete oxidation of Al films required exposure to O₂ at temperatures above room temperature. Room temperature exposure to hydrazine resulted in the complete nitriding of Al films. The spectrum for the nitride is similar in shape to published spectra from films produced by two alternative methods of nitriding. The hydrazine-exposure method of producing Al nitride films was found to offer an alternative, easily prepared support material for future model catalyst studies.     

On the surface denudation of voids induced by 200 keV C+ ion irradiation

Abstract

Niobium films (120 nm thick) deposited by electron-beam evaporation were implanted near 5 K with 100 keV N₂ ions to maximum fluences of 4 to 7 × 10¹⁷ N/cm². STEM diffraction patterns showed a structural phase transformation from the initial Nb lattice with [110] fiber texture (bcc, a ₀ = 0.330 nm) to randomly oriented δ-NbN (fcc, a ₀ = 0.435–0.439 nm), via an intermediate, highly disordered Nb-(interstitial N) structure (bcc, maximum a ₀ = 0.342 nm). Decreases in transition temperature T _c from 9 K to a minium of 3 K and rapid linear increases in residual resistivity (ρ ₁₀) were observed to fluence of 1.0–1.5 × 10¹⁷ N/cm² and were attributed to the accumulation of radiation-induced defects. Continued implantation resulted in δ-NbN formation and T _c increases to maximum values of 9–10 K which were achieved at fluences from 3.5 to 5.0 × 10¹⁷ N/cm², corresponding to average substoichiometric N/Nb ratios of 0.52–0.75, at which point the phase transformation was complete. The δ-NbN formation was accompanied by significant lattice reordering and grain growth. At still higher fluences T _c gradually declined to 8–9 K and sharp increases in ρ ₁₀ were observed, possibly due to film sputtering.     

Electrochromic properties of spray-deposited niobium oxide thin films

Niobium oxide thin films were deposited on the glass and fluorine-doped tin oxide (FTO)-coated glass substrates using simple and inexpensive spray pyrolysis technique. Various preparative parameters like nozzle to substrate distance, spray rate, concentration of sprayed solution were optimized to obtain good substrate-adherent and transparent films. Morphological and structural characterizations of the films were carried out using scanning electron microscopy and X-ray diffraction techniques. Electrochemical characterization of the niobium oxide thin films was carried out using cyclic-voltammetry, chronoamperometry and chronocoulometry.     

The competitive growth of cubic domains in Ti1–xAlxN films studied by diffraction anomalous near‐edge structure spectroscopy

Titanium and aluminium nitride films deposited by magnetron sputtering generally grow as columnar domains made of oriented nanocrystallites with cubic or hexagonal symmetry depending on Al content, which are embedded in more disordered grain boundaries. The substitution of Al atoms for Ti in the cubic lattice of the films improves their resistance to wear and oxidation, allowing their use as protective coatings. Ti K‐edge X‐ray absorption spectroscopy, which probes both crystallized and more disordered grain boundaries, and X‐ray diffraction anomalous fine structure, which is sensitive to short‐ and long‐range order within a given crystallized domain, are carried out on a set of Ti_1–xAl_xN films deposited by magnetron sputtering on Si substrates. Attention is paid to the shape of the pre‐edge region, which is sensitive to the symmetry of the site occupied by Ti atoms, either octahedral in face‐centred‐cubic Ti‐rich (TiN, Ti_0.54Al_0.46N) samples or tetrahedral in hexagonal‐close‐packed Al‐rich (Ti_0.32Al_0.68N) films. In order to obain information on the titanium environment in the well crystallized areas, subtraction of the smooth part of the energy‐dependent structure factor for the Bragg reflections is applied to the pre‐edge region of the diffraction anomalous data in order to restore their spectroscopic appearance. A flat pre‐edge is related to the typical octahedral environment of Ti atoms for cubic reflections. The difference observed between pre‐edge spectra associated with face‐centred‐cubic 200 and 111 Bragg reflections of Ti_0.54Al_0.46N is assigned to Ti enrichment of 111 large well ordered domains compared with the more disordered 200 ones. The sharp peak observed in the spectrum recorded from the hexagonal 002 peak of Ti_0.32Al_0.68N can be regarded as a standard for the pure tetrahedral Ti environment in hexagonal‐close‐packed nitride.     

Thin ZnO films prepared by chemical solution deposition on glass and flexible conducting substrate

Thin films of zinc oxide (ZnO) are deposited by a simple method of successive immersion of substrate in (NH₄)₂ZnO₂(0.1 M) chemical solution and in boiling water. Films of a thickness ≈ 500 nm could be deposited on stainless steel and glass by 40 immersions. The composition, structure, optical bandgap and the charge transport mechanism were determined and the results are presented. Films are stoichiometric and have the same hexagonal lattice parameters as for powder samples. Films are formed from grains with a mean size of a few 100 nm. Grains consist of crystallites of mean size 20–30 nm. For films deposited on stainless steel, the crystallites are highly oriented along their c-axis perpendicular to the substrate. Films have a high optical transparency (above 80%) in the visible region and bandgap energy in the range 3.38–3.42 eV. Films are intrinsically n-type and the charge transport across the films is controlled by a shallow trapping level in accordance with the Poole–Frenkel mechanism. The doubly-ionized trapping level has a concentration of 4×10¹¹ cm^-3 and zero-field ionization energy of 110 meV. Adsorption of oxygen by annealing the films in air yields a singly-ionized trap. PACS 81.15.Lm; 81.05.Dz; 68.37.Hk; 73.61.Ga     

非晶态Nb氧化物纳米薄膜可见光区的光玫发光

在低真空及亚高温(200～300℃)下.通过热氧化法在Si单晶基底上合成了呈准直阵列的椎形结构的氧化铌(NbOx)非晶结构纳米薄膜,薄膜经热处理后室温下在可见光区具有很好的光致发光.实验研究了退火温度与发光强度规律,对铌氧化物纳米薄膜的光致发光(PL)机制进行了初步分析和讨论.变功率光致发光(PL)实验有力地支持了初步讨论结果.     

Surface acoustic wave device properties of (B, Al)N films on 128° Y-X LiNbO3 substrate

A c-axis orientated aluminium nitride (AlN) film on a 128° Y-X lithium niobate (LiNbO₃) surface acoustic wave (SAW) device which exhibit a large electromechanical coupling coefficient (k²) and a high SAW velocity property, is needed for future communication applications. In this study, a c-axis orientated (B, Al)N film (with 2.6 at.% boron) was deposited on a 128° Y-X LiNbO₃ substrate by a co-sputtering system to further boost SAW device properties. The XRD and TEM results show that the (B, Al)N films show highly aligned columns with the c-axis perpendicular to the substrate. The hardness and Young's modulus of (B, Al)N film on 128° Y-X LiNbO₃ substrates are at least 17% and 7% larger than AlN films, respectively. From the SAW device measurement, the operation frequency characteristic of (B, Al)N film on 128° Y-X LiNbO₃ is higher than pure AlN on it. The SAW velocity also increases as (B, Al)N film thickness increases (at fixed IDT wavelength). Furthermore, the k² of (B, Al)N on the IDT/128° Y-X LiNbO₃ SAW device shows a higher value than AlN on it.     

Effect of nitrogen partial pressure on Al–Ti–N films deposited by arc ion plating

AlTiN films with different nitrogen partial pressures were deposited using arc ion plating (AIP) technique. In this study, we systematically investigated the effect of the nitrogen partial pressure on composition, deposition efficiency, microstructure, macroparticles (MPs), hardness and adhesion strength of the AlTiN films. The results showed that with increasing the nitrogen partial pressure, the deposition rate exhibited a maximum at 1.2 Pa. Results of X-ray photoelectron spectroscopy (XPS) analysis revealed that AlTiN films were comprised of Ti–N and Al–N bonds. XRD results showed that the films exhibited a (1 1 1) preferred growth, and AlTi₃N and TiAl_x phases were observed in the film deposited at 1.7 Pa. Analysis of MPs statistics showed MPs decreased with the increase in the nitrogen partial pressure. In addition, the film deposited at 1.2 Pa possessed the maximum hardness of 38 GPa and the better adhesion strength.     

Influence of vacuum annealing on structures and mechanical properties of Al–Ti–N films deposited by multi-arc ion plating

The Al–Ti–N films deposited by multi-arc ion plating have been annealed in vacuum within the range of 700–1100 °C. X-ray diffraction results showed that the structure of the films underwent the formation of coherent c-TiN and c-AlN for the annealing temperatures were up to 900 °C. A new phase AlTi_x (x = 0.50, 0.56, 3) was observed after annealing. The X-ray photoelectron spectroscopy results showed the intensity of Ti–Al bonds decreased as annealing temperatures increased, indicating the decomposition of (Al, Ti)N into c-TiN and c-AlN were at the expense of Ti–Al bonds. Differential scanning calorimetry experiments were used to investigate the dynamic behavior of the films during annealing process and the results showed that the N₂ formed as a consequence of the phase transformation process. The release of the N₂ resulted in the peeling of the films from the substrates. The film exhibited a maximum hardness of 39 GPa after 900 °C annealing due to the formation of coherent c-TiN and c-AlN phases. In addition, we also investigated the influence of vacuum annealing on adhesive strength.     

Fabrication,characterization and biocompatibility of TiO2 nanotubes via anodization of Ti6Al7Nb

Ti6Al7Nb has been used as an implant material because of its good corrosion resistance and high mechanical properties. However, the presence of aluminium (Al), which may lead to ostemalacia, anaemia and nervous system disorders, limited its wide clinical use. In this study, a titanium oxide (TiO₂) nanoporous layer was fabricated on a Ti6Al7Nb alloy using an electrochemical anodic oxidation method. The structure of the TiO₂ nanoporous layer was examined by scanning electron microscopy. The chemical compositions of the samples were analysed by X-ray photoelectron spectroscopy (XPS). Biocompatibility was evaluated by culturing rat osteoblast cells. The result showed that TiO₂ nanoporous layers comprise a mixed oxide containing TiO₂ and a small amount of nobium oxides (Nb₂O₅) and almost no elemental aluminium. The outer layer of the TiO₂ nanoporous layer comprises highly ordered nanotubes and the inner layer forms disordered nanopores. The TiO₂ nanoporous layer could support the adhesion, proliferation, differentiation and gene expression of osteoblast cells. Therefore, a TiO₂ nanoporous layer could enhance the biocompatibility of Ti6Al7Nb alloy and is as a promising candidate for Ti6Al7Nb alloy implants.     

Absorption optique du niobium en couches minces entre 0,32 ET 5,5 eV. interpretation par la theorie des bandes d'energie

Niobium optical conductivity has been determined from reflexion and transmission data measured, at room temperature, on polycrystalline thin films in the 0.32–5.50 eV spectral range. The films have been deposited in ultra high vacuum and the measurements carried out in situ. Structures are observed at -.55, 2.3, 3.0 and 4.4 eV and tentatively identified with interband transitions in fairly good agreement with the band structure calculated by Mattheiss. In addition, we compare our results with recent experiments on niobium.     

Superconductivity of vapour quenched beryllium and beryllium-based alloys

The properties of Be films, quench-condensed upon a³He cooled substrate, have been investigated by resistance and tunneling measurements. The superconducting transition temperature,T _c , of Be films increased with thickness and a thick film limit of 9.95 K could be estimated. Alloying with Al or Pb decreasedT _c. The ratios between energy gaps andT _c 's indicated that Be is a weak coupling superconductor, and no phonon induced structure could be traced in tunneling curves neither in pure Be nor in the Be based alloys. Resistance change during annealing as well as superconducting data indicated that the vapour quenched Be films were amorphous as deposited.     

Low-nickel stainless steel passive film in simulated concrete pore solution: A SIMS study

Low-nickel and AISI 304 austenitic stainless steel (SS) passive films were studied using secondary ion mass spectrometry (SIMS). An alkaline Ca(OH)₂ saturated test solution containing different chloride additions was used at room temperature. The passive film formed consists mainly of an inner chromium-rich oxide layer and an outer iron-rich oxide layer. The chemistry of the passive film depends strongly on the chloride content in the alkaline solution. Under these exposure conditions nickel was detected in the outer part of the oxide, whereas chloride ions were not found in the passive film for either the low-nickel or AISI 304 SS alloys.     

Synthesis and electrochemical characteristics of Ta-N thin films fabricated by cathodic arc deposition

Ta-N thin films were deposited on AISI 317L stainless steel (SS) substrates by cathodic arc deposition (CAD) at substrate biases of −50 and −200 V. The as-deposited films were characterized using X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and energy dispersive X-ray analysis (EDX). The results show that stoichiometric TaN with hexagonal lattice (3 0 0) preferred orientation was achieved at the bias of −200 V. On the other hand, Ta-rich Ta-N thin film deposited at −50 V shows amorphous nature. According to the XPS result, Ta element in the films surface exist in bonded state, including the Ta-N bonds characterized by the doublet (Ta 4f_7/2 = 23.7 eV and Ta 4f_5/2 = 25.7 eV). Electrochemical properties of the Ta-N coated stainless steel systems were investigated using potentiodynamic polarization and electrochemical impedance spectroscope (EIS) in Hank's solution at 37 °C. For the Ta-N coated samples, the corrosion current (i_corr) is two or three orders of magnitude lower than that of the uncoated ones, indicating a significantly improved corrosion resistance. Growth defects in the Ta-N thin films produced by CAD, however, play a key role in the corrosion process, especially the localised corrosion. Using the polarization fitting and the EIS modelling, we compared the polarization resistance (R_p) and the porosity (P) of the Ta-N coatings deposited at different biases. It seems that Ta-N film with comparatively lower bias (−50 V) shows better corrosion behavior in artifical physiological solution. That may be attributed to the effect of ion bombarding, which can be modulated by the substrate bias.     

Electronic properties of thin films of laser-ablated Al2O3

Laser ablation coupled to mass quadrupole spectrometry (LAMQS) has been used to prepare thin films of aluminum oxide deposited on Si substrates starting from commercial Al₂O₃ polycrystalline targets. X-ray photoemission (XPS) and reflection electron energy loss spectroscopy (REELS) have allowed the investigation of the electronic properties of the produced films. In particular, it was found that the Al/O atomic ratio assumes a value very near to 0.7 (stoichiometric ratio) only for films deposited normally with respect to the target surface, while films grown at larger deposition angles are more rich in oxygen content.The composition, the mass density, the optical energy gap, the complex dielectric function and refraction index of the films have been calculated and compared with the results obtained from our starting target material and with the literature. The morphology of the deposited samples has been analyzed by the AFM technique.     

Improving mechanical properties of a-CNx films by Ti-TiN/CNx gradient multilayer

Amorphous carbon nitride (a-CN_x) films with functional gradient Ti-TiN/CN_x underlayer were deposited by direct current magnetron sputtering. Microstructure and composition of the films were characterized by means of X-ray diffraction (XRD), Raman spectroscopy, atomic force microscope (AFM) and transmission electron microscopy (TEM). Mechanical and tribological properties were investigated by nanoindenter, scratch and ball-on-disk tribometer. The a-CN_x-based films suffer a graphitization process with the increasing deposition temperature, thus the hardness and elastic modulus decrease. With the design of the Ti-TiN/CN_x gradient underlayers, some important advantages of relatively thick CN_x films can be achieved, such as increased hardness, improved adhesion strength, and the wear resistance of the a-CN_x-based films can be also improved significantly.