Preparation and characterization of Ce-doped BaTiO3 thin films by pulsed laser deposition

Thin films of BaTiO₃ doped with 5.5 mol%CeO₂ have been deposited on Pt/Si substrate by pulsed laser deposition. These films crystallize on the tetragonal BaTiO₃ structure without any preferential orientation. Ce-doped BaTiO₃ films deposited by PLD at 675°C in 30 Pa ambient oxygen exhibits a smooth surface: mean surface roughness (Rms) of 48 nm, mean size of grain of 40 Å, average size of aggregates of 315 nm. Thin films as prepared presented good dielectric characteristics: dielectric constant and dielectrics loss (tan ) at a frequency of 1 KHz were 220 and 0.2, respectively. The temperature dependence of dielectric constant exhibited a diffuse ferroelectric to paraelectric phase transition at about 0–10°C. The ferroelectric nature of Ce-doped BaTiO₃ film was confirmed by the hysteresis of the C-V curves.     

Preparation of Fe-N films by r.f. sputtering

Fe-N films over a wide compositional range have been prepared by the reactive sputtering method. Fe-N sputtered films were composed of a single or two phases such as-Fe₂N,-Fe_3.02N,-Fe_3.82N,-Fe₄N and-Fe; however, an unknown phase was observed at a higher nitrogen pressure. A remarkable preferred orientation of the-Fe_3.02N (110) plane parallel to the film surface was observed. The Curie temperature of the sputtered -Fe_3.82N sample was 490° C, which was almost the same as that of-Fe₄N prepared by metal nitriding. The saturation magnetization, _s, of the sputtered Fe-N samples decreased from 151.8 to 42.4 e.m.u.g^–1 with increasing nitrogen content from 7.94 to 24.87 at%, and its coercive force,₁ H _c was found to lie in the range 150 to 600 Oe in the powder form at room temperature.     

Structural properties of TiO2–WO3 thin films prepared by r.f. sputtering

TiO₂–WO₃ thin films were prepared by radio frequency (r.f.) reactive sputtering from metallic target. Structural and morphological properties of the thin films have been studied through X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM). The influence of the annealing on the phase composition TiO₂–WO₃ system was studied. The binding energies of titanium and tungsten are characteristic for Ti⁴⁺ and W⁶⁺. The influence of tungsten on anatase–rutile phase transition in TiO₂ was observed. The structural modeling has been performed to account the preferred orientation in tungsten doped titanium oxide.     

Piezoelectric ZnO films by r.f. sputtering

Piezoelectric zinc oxide films are used in microelectromechanical systems (MEMS) applications, where they can be used in sensors to detect, e.g., pressure or acceleration. Beside sensors, ZnO films are applied in activation devices, where force is needed. Conductive-doped zinc oxide (most often with aluminum) is also used in optoelectronics. Piezoelectric films including AlN and ZnO are more difficult to produce than the corresponding conductive materials. In order to achieve good piezoelectricity in ZnO films, they have to possess high purity, a (0 0 1) orientation (ZnO has hexagonal crystal structure), high resistivity, and fine columnar microstructure perpendicular to the substrate. We have used r.f. magnetron (13.56 MHz) sputtering from a ZnO target in an oxygen atmosphere to achieve the piezoelectric ZnO. The aim of this work has been to develop an r.f. sputtering process for ZnO to achieve highly piezoelectric thin films. As a test vehicle to measure the piezoelectricity of the ZnO films we have fabricated resonators and passband filters in the 1–2 GHz range using standard microelectronics photolithography, deposition, and etching techniques on 100-mm diameter Corning glass or silicon wafers. The influence of the sputtering-process parameters on the film properties has been studied by X-ray diffraction, scanning electron microscopy, atomic force microscopy, and electrical measurements. In this study, the effects of the process parameters on the final material properties of the ZnO film are discussed in detail.     

ZnO:Ga透明导电膜的低温制备及特性研究

采用射频磁控溅射法在玻璃衬底上低温制备出高质量的镓掺杂氧化锌(ZnOGa)透明导电膜,对薄膜的结构和光电特性以及制备参数对薄膜性能的影响进行了研究.制备的ZnOGa是具有六角纤锌矿结构的多晶薄膜,最佳择优取向为(002)方向.薄膜的最低电阻率达到了3.9×10-4Ωcm,方块电阻～4.6Ω/□,薄膜具有良好的附着性,在可见光区的平均透过率达到90%以上.     

射频磁控溅射制备TiO2-xNx薄膜及其光催化特性研究

利用射频磁控溅射在玻璃衬底上制备了透明TiO2 和 TiO2-x Nx 薄膜样品,通过 X 射线衍射(XRD)、原子力显微镜(AFM)及 UV Vis分光光度计等测试手段表征了样品的结构、形貌和光催化性能。结果表明制备的薄膜为锐钛矿相结构。随着 N2/Ar气流比的增大薄膜样品出现新的物相,吸收光谱向可见光方向展宽,在N2/Ar流量比为 3∶100 时,制备的薄膜在可见光区具有很好的光催化性能。     

直流溅射沉积氧化镍薄膜及结构表征

采用直流溅射并结合热处理工艺制备氧化镍薄膜,利用X射线衍射仪(XRD)、扫描电镜(SEM)、能谱仪(EDX)考察退火温度对薄膜结构、形貌和组成的影响,并通过恒流充放电技术初步考察薄膜的电化学性能.研究结果表明,在400℃～500℃退火温度下制备了表面光滑、结构致密的NiO薄膜;随着退火温度的升高,薄膜的晶粒尺寸逐渐增大,晶形趋于完整;其中,500℃下退火2 h获得的NiO薄膜具有良好的电化学循环稳定性,有望成为高性能的全固态薄膜镡电池阳极材料.     

Voltaic cells of (ZnxCuy)Oz thin films deposited by r.f. sputtering

The growth of (Zn₂₈₋₄₂Cu₃₉₋₂₅)O₃₃ thin films deposited by r.f. sputtering was studied. Voltaic elements with an ITO/(Zn, Cu)O/Al structure (where ITO is indium tin oxide) were fabricated. The open-circuit voltage and short-circuit current at temperatures of 0–45 °C were 0.5–1.25 V and 0.3–1.5 μA cm^-2 respectively. The composition of the films was studied by Auger analysis.     

D.c. properties of ZnO thin films prepared by r.f. magnetron sputtering

In the development of ZnO-based varistors the electrical properties of ZnO/Bi₂O₃ junctions and of the two individual oxides are being investigated. Following our recent work on a.c. conductivity in Al---ZnO---Al sandwich structures we currently report d.c. measurements. The structures were prepared by r.f. magnetron sputtering in an argon/oxygen mixture in the ratio 4:1. Capacitance-voltage data confirm that the Al/ZnO interface does not form a Schottky barrier and measurements of the dependence of capacitance on film thickness indicate that the relative permittivity of the films is approximately 9.7. With increasing voltage the current density changed from an ohmic to a power-law dependence with exponent n≈3. Furthermore measurements of current density as a function of reciprocal temperature showed a linear dependence above about 240 K, with a very low activation energy below this temperature consistent with a hopping process. The higher temperature results may be explained assuming a room-temperature electron concentration n₀ and space-charge-limited conductivity, dominated by traps exponentially distributed with energy E below the conduction band edge according to N = N₀exp(−E/kT_t), where k is Boltzmann's constant. Typical derived values of these parameters are: n₀ = 7.2 × 10¹⁶ m⁻³, N₀ = 1.31 × 10⁴⁵ J⁻¹ m⁻³ and T_t = 623 K. The total trap concentration and the electron mobility were estimated to be 1.13 × 10²⁵ m⁻³ and (5.7−13.1) ×10⁻³m²V⁻¹s⁻¹ respectively.     

Preparation and properties of r.f.-sputtered polymer-metal thin films

The ability to produce polymer-metal thin films by co-sputtering from a composite target was investigated using polytetrafluoroethylene (PTFE) (Teflon) and Ekonol polymers. The preparation of PTFE-metal thin films by sputtering was found to be limited by target cross-contamination possibly caused by negative ion re-sputtering processes. The Ekonol-metal films were found to have microstructure and conductivity properties similar to other metal-insulator composites.     

Preparation of fatigue-free SrBi2Ta2O9 thin films by r.f. magnetron sputtering and their ferroelectric properties

Fatigue-free bismuth-layered SrBi₂Ta₂O₉ (SBT) films were deposited on Pt/Ti/SiO₂/Si substrates by r.f. magnetron sputtering at room temperature. The variation of structure and electrical properties were studied as a function of annealing temperatures from 750–850 °C. The films annealed at 800 °C had a composition ratio of Sr:Br:Ta = 0.7:2.0:2.0. X-ray photoelectron spectroscopy signals of bismuth show an oxygen-deficient state within the SBT films. The films annealed at 800 °C have a thickness of 200 nm and a relatively dense microstructure. The remanent polarization (2P _r), and the coercive field (2E _c), obtained for the SIBT films, were 9.1 C cm^–2 and 85 kV cm^–1 at an applied voltage of 3 V, respectively. The films showed fatigue-free characteristics up to 10¹⁰ cycles under 5 V bipolar square pulses. The leakage current density was about 7 × 10^–7 A cm^–2 at 150 kV cm^–1. The SBT films prepared by r.f. magnetron sputtering were attractive for application to non-volatile memories.     

On the properties of AlN thin films grown by low temperature reactive r.f. sputtering

In this paper we report on the growth of c-axis-oriented AlN thin films by low temperature reactive r.f. sputtering and the results of their examination and analysis in a variety of ways. In addition to using other substrates, we fabricated c-axis- oriented AlN films on aluminium film substrates. A hexagonal column structure was observed in the morphology of replicas of the natural surfaces of films. As well as the dielectric constant ε, the resistivity ϱ, the breakdown field E_p and the refractive index n, curves of ε versus frequency f, ε versus temperature T and conductivity σ versus T were measured. The IR absorption spectrum of an AlN film sputtered at low temperature coincides with that of an AlN film sputtered onto a high temperature substrate and of a bulk crystal, which remains unchanged after annealing. The band gap E_g = 5.9–6.0 eV, which remains unchanged after annealing in N₂ at 900°C. Theoretical calculation of the dispersion curve of surface acoustic waves by an AlN/glass structure shows that the curve is very level in the range hk = 0.2–0.6. The capacitance-voltage curve of an Al/AlN/Si structure is given in this paper.     

Preparation and characterization of r.f.-sputtered multilayered TiN---Au films

TiN---Au films with multiple intermediate layers deposited by r.f. sputtering are suggested as a solution to the problem of adhesion of gold films to TiN coatings. Their optical and mechanical properties are investigated and compared with those of conventional electroplated gold films. Various analysis techniques have been used: Auger electron spectroscopy to determine the composition profiles, the direct tensile test for adhesion characteristics, optical rub test for scratch characteristics, salt spray test for corrosion characteristics and the selected ordinate method to identify the color of resultant films. It is shown that poor adhesion of gold films of TiN coatings can be overcome. Resultant multilayered TiN---Au films show the same color as that of commercially available electroplated gold films and their reflectivity reaches 98% of that of gold films over the wavelength range studied. For further applications, electrical properties of multilayered TiN---Au have also been studied. The sheet resistance of these TiN---Au films on n-Si and p-Si is in the range 0.54ω/□–6.12ω/□. Thus these multilayered structures may be used as durable contacts for microelectronic applications.     

Synthesis of Al-Cr-O-N thin films in corundum and f.c.c. structure by reactive r.f. magnetron sputtering

Advanced PVD coatings for metal cutting applications must exhibit a multifunctional property profile including high hardness, chemical inertness and high temperature stability. Recently, ternary Al-Cr-O thin films with mechanical properties similar or superior to conventional aluminium oxide thin films have been suggested as potential materials meeting such demands. These coatings can be deposited at moderate temperatures in PVD processes. In this work, new quaternary Al-Cr-O-N coatings are suggested as alternative for offering thin film materials of high strength, hardness and even toughness. A combinatorial approach to the synthesis of Al-Cr-O-N thin films by means of reactive r.f. magnetron sputtering is presented. A thorough phase analysis of deposited coatings covering a wide range of elemental compositions revealed a well-defined phase transition from a corundum-type α-(Al_1 − x,Cr_x)_2 + δ(O_1 − y,N_y)₃ structure to a CrN-type f.c.c.-(Al_1 − x,Cr_x)_1 + θ(O_1 − y,N_y) structure as a function of the Al/Cr ratio and the nitrogen gas flow ratio. Detailed results on the coatings composition, constitution and microstructure are discussed compared to ternary Al-Cr-O thin films deposited by reactive r.f. magnetron sputtering under nearly identical conditions.     

Optical and structural characterization of r.f. sputtered CeO2 thin films

The optical and structural properties of r.f. sputtered CeO2 thin films deposited on Pyrex substrates have been studied as a function of substrate temperature during deposition. The refractive index, n, extinction coefficient, k, and bandgap of the films were calculated from reflectance, R, and transmittance, T, spectra in the wavelength range 340–900 nm. The refractive index of CeO2 films at 550 nm comprises values from about 2.25–2.4 depending on the substrate temperature during deposition. The extinction coefficient was negligible for wavelength values higher than 400 nm. The value obtained for the bandgap was 3.1 eV. The X-ray diffraction patterns showed the same (f c c) cubic structure with preferential orientation depending on substrate temperature during deposition. The scanning force microscope measurements showed that the roughness and grain size of the CeO2 films increase with increasing substrate temperature. This revised version was published online in November 2006 with corrections to the Cover Date.     

Electrical properties of dielectric thin films of the tantalum oxide-quartz system prepared by r.f. reactive sputtering

It has been reported by many workers that tantalum oxide is one of the most useful materials for thin film capacitors. However, improvements in the design of such capacitors continue to be made; for example, in the development of TMM or TSM capacitors consisting of a film of tantalum oxide or another oxide sandwiched between electrodes.In this paper the electrical properties of mixed tantalum oxide-quartz films, prepared by reactive sputtering from tantalum-quartz composite targets with various area ratios at the target surface, are described.