Phase transitions in iridium oxide films

We report studies of SIROFs by differential thermal analysis (DTA), evolved gas analysis (EGA), and scanning electron microscopy (SEM). SIROFs undergo an irreversible exothermic transition at ≈300°C associated with ≈1 eV energy release and no decomposition. There is a second endothermic transition at ≈700°C, which is associated with dehydration. After undergoing the first transition, SIROFs lose their good electrochromic and electrocatalytic properties.     

HF sputtered indium oxide films doped with tin

Indium-tin-oxide films (ITO films) sputtered in Ar-atmosphere with and without addition of oxygen reveal an irreversible increase in conductivity during annealing in vacuum. This annealing process increases drastically the density of free electrons, while the Hall mobility changes only slightly. Below the annealing temperature the temperature dependence of the conductivity is reversible. In films with low density of free electrons, which behave like non-degenerated semiconductors, two activation energies for the mobility could be found. The irreversible changes, observed during annealing in the vacuum, are explained by diffusion of oxygen from the interior of the film to the surface, followed by desorption of the oxygen from the surface into the vacuum. The excess oxygen in the non-stoichiometric films plays the role of electron traps. The irreversible effects during annealing in the vacuum are partly reversible in the long run. If the annealed films are exposed to oxygen or air their conductivity decreases because of diffusion of oxygen from the surface into the film.     

氧化钒薄膜微观结构的研究

采用直流磁控反应溅射在Si(100)衬底上溅射得到(001)取向的V₂O₅薄膜.x射线衍射(XRD)、扫描电镜(SEM)和傅里叶变换红外光谱(FTIR)的结果表明，氧分压影响薄膜的成分和生长取向，在氧分压0.4Pa时溅射得到(001)取向的纳米V₂O₅薄膜，即沿c轴垂直衬底方向取向生长的薄膜.V₂O₅薄膜经过真空退火得到(001)取向的VO₂薄膜，晶体颗 关键词： 微观结构 氧化钒薄膜 择优取向 直流磁控溅射     

Effect of some preparative parameters on optical properties of spray deposited iridium oxide thin films

Optical properties of iridium oxide films fabricated by the spray pyrolysis technique (SPT) have been investigated. The transmission and reflection spectra of the sprayed films were measured by using a double-beam spectrophotometer in the wavelength range from 200 to 2500 nm. Influences of the preparative parameters; namely, substrate temperature (350-500 °C) and solution molarity (0.005-0.03 M), on the optical characteristics were examined. The solution molarity of the iridium chloride solution was varied so as to prepare iridium oxide thin films with thicknesses ranging from 160 to 325 nm. Some important characteristics of optical absorption, such as optical dispersion energies, the dielectric constant, the ratio of the number of charge carriers to the effective mass, the single oscillator wavelength, and the average value of the oscillator strength, were evaluated. The value of the refractive index was found to depend on the chemical composition as well as the degree of stoichiometry of IrO₂. The values obtained for the high frequency dielectric constant through two procedures are in the range of 2.8-3.9 and 3.3-4.6 over the relevant ranges of the substrate temperature and solution molarity, respectively. Analysis of the energy dispersion curve of the absorption coefficient indicated a direct optical transition with the bandgap energy ranging between 2.61 and 2.51 eV when the substrate temperature increases from 350 to 500 °C.     

Low reflectance sputtered vanadium oxide thin films on silicon

Vanadium oxide thin films on silicon (Si) substrate are grown by pulsed radio frequency (RF) magnetron sputtering technique at RF power in the range of 100–700 W at room temperature. Deposited thin films are characterized by field emission scanning electron microscopy (FESEM), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) techniques to investigate microstructural, phase, electronic structure and oxide state characteristics. The reflectance and transmittance spectra of the films and the Si substrate are recorded at the solar region (200–2300 nm) of the spectral window. Substantial reduction in reflectance and increase in transmittance is observed for the films grown beyond 200 W. Further, optical constants viz. absorption coefficient, refractive index and extinction coefficient of the deposited vanadium oxide films are evaluated.     

Third-order nonlinear optical properties of thin sputtered gold films

Au films of thickness ranging between 5 and 52 nm were prepared by sputtering on quartz substrates and their third-order nonlinear optical response was investigated by Optical Kerr effect (OKE) and Z-scan techniques using 532 nm, 35 ps laser pulses. All prepared films were characterized by XRD, AFM and UV-VIS-NIR spectrophotometry while their third-order susceptibility χ⁽³⁾ was measured and found to be of the order of 10⁻⁹ esu. The real and imaginary parts of the third-order susceptibility were found in very good agreement with experimental results and theoretical predictions reported by Smith et al. [D.D. Smith, Y. Yoon, R.W. Boyd, Y.K. Cambell, L.A. Baker, R.M. Crooks, M. George, J. Appl. Phys. 86 (1999) 6200].     

Structural and optical properties of sputtered ZnO thin films

Zinc oxide (ZnO) and aluminium-doped zinc oxide (ZnO:Al) thin films were prepared by RF diode sputtering at varying deposition conditions. The effects of negative bias voltage and RF power on structural and optical properties were investigated. X-ray diffraction measurements (XRD) confirmed that both un-doped and Al-doped ZnO films are polycrystalline and have hexagonal wurtzite structure. The preferential 〈0 0 1〉 orientation and surface roughness evaluated by AFM measurements showed dependence on applied bias voltage and RF power. The sputtered ZnO and ZnO:Al films had high optical transmittance (>90%) in the wavelength range of 400-800 nm, which was not influenced by bias voltage and RF power. ZnO:Al were conductive and highly transparent. Optical band gap of un-doped and Al-doped ZnO thin films depended on negative bias and RF power and in both cases showed tendency to narrowing.     

Hard magnetic properties of sputtered Co and Co-P films

Both magnetic properties and microstructure of sputtered Co and Co-4.8 wt% P films ( ≈ 3000 Å) deposited near room temperature are studied as a function of Ar pressure P_Ar ranging from 4×10^-3 to 1.4×10^-1 Torr. The coercive force H_c of the film is a strong function of P_Ar. The coercive force of Co increases from 25 to 270 Oe with increasing P_Ar. With an addition of phosphorus in Co, H_c increases substantially. At high P_Ar ( ≈ 1×10^-1 Torr), a high H_c of 700 Oe and a low squareness of 0.58 are obtained. From observation of the microstructure, it is concluded that the structure of columns is responsible for the high H_c and the low squareness.     

Structural and optical properties of sputtered gadolinium nitride films

Rare-earth (RE) materials have high magnetic moments and form a wide range of magnetic structures. There has been speculation in the literature that rare-earth nitrides may form half-metallic ferromagnetics. This is surprising because, based on a simple ionic model, trivalent rare-earth nitrides would be expected to be insulators with a similar electronic structure to the divalent rare-earth chalcogenides. However if it is the case that they are half-metallic or narrow gap insulators, then they have potential applications in spin-filtering devices. In the present investigation, We have deposited GdN films on glass substrate at room temperature by Ar/N₂ mixed gas plasma-radio frequency (rf) sputtering method. The structure and the complex optical properties as well as the energy gap of GdN thin films as a function of N₂ partial pressure are determined.     

Anodic iridium oxide films: An UPS study of emersed electrodes

Formation of anodic iridium oxide films has been monitored using Ultraviolet Photoemission Spectroscopy (UPS) of the emersed electrodes. The potential dependent valence band spectra clearly show the onset of oxide formation at about 0.6 V versus SCE. The density of states at the Fermi level and the positron of the Fermi level with respect to the maximum of the t_2g band of the oxide indicates a transition from metallic to semiconducting behaviour of the oxide. Protonation of the oxide is associated with increased emission from OH species. A linear correlation between electrode potential and workfunction change is observed for the metal as well as for the oxide. Our results confirm known band theory models and provide a fundamental understanding of the electrochromism of anodic iridium oxide films.     

Structural and optical characterization of DC magnetron sputtered molybdenum oxide films

Thin films of molybdenum trioxide were deposited on glass substrates employing direct current (DC) magnetron sputtering by sputtering of molybdenum at different oxygen partial pressures in the range 8 × 10⁻⁵–1 × 10⁻³ mbar and at a substrate temperature of 473 K. The glow discharge characteristics of magnetron cathode target of molybdenum were studied. The influence of oxygen partial pressure on the structural and optical properties of molybdenum trioxide films was investigated. The films formed at an optimum oxygen partial pressure of 2 × 10⁻⁴ mbar were polycrystalline in nature with orthorhombic α- phase and an optical band gap of 3.16 eV. The refractive index of the films formed at an oxygen partial pressure of 2 × 10⁻⁴ mbar decreased from 2.08 to 1.89 with increase of wavelength from 450 to 1,000 nm, respectively. Paper presented at the Third International Conference on Ionic Devices (ICID 2006), Chennai, Tamilnadu, India, Dec. 7–9, 2006.     

Electrical and optical properties of reactive dc magnetron sputtered silver-doped indium oxide thin films: role of oxygen

Silver-doped indium oxide thin films have been prepared on glass and quartz substrates at room temperature (300 K) by a reactive dc magnetron sputtering technique using an alloy target of pure indium and silver (80:20 at. %). During sputtering, the oxygen flow rates are varied in the range 0.00–2.86 sccm keeping the magnetron power constant at 40 W. The resistivity of these films is in the range 10⁰–10^-3 Ω cm and they show a negative temperature coefficient of resistivity. The films exhibit p-type conductivity at an oxygen flow rate of 1.71 sccm. The work function of these silver–indium oxide films has been measured by a Kelvin probe technique. The refractive index of the films (at 632.8 nm) varies in the range 1.13–1.20. Silver doping in indium oxide narrows the band gap of indium oxide (3.75 eV). PACS 73.30.+y; 81.15.Cd; 78.20.Ci; 73.61.Le     

DC magnetron sputtered Mo-Ti oxide films for color neutral electrochromic devices

Mo-Ti oxide films with compositions ranging from MoO₃ to TiO₂ were prepared by reactive DC magnetron sputtering using a newly developed high-rate technique with interacting plasma zones. Optical and electrochemical measurements showed that an increase of the Ti content yielded increased electrochemical stability, decreased coloration efficiency, and increased potential for electrochromic coloration. The films have interesting properties for color-neutral electrochromic devices. Paper presented at the 2nd Euroconference on Solid State Ionics, Funchal, Madeira, Portugal, Sept. 10–16, 1995     

Magnetic properties of dc magnetron sputtered and evaporated amorphous films

Compositions of Fe₈₁B_13.5Si_3.5C₂, Fe₆₇Co₁₈Si₁B₁₄ and Fe_5.85Co_72.15Mo₂B₁₅Si₅ were deposited on to rigid and flexible substrates for the first time using a dc sputtering source as part of a novel Rotating Cryostat (RC). The films sputtered on silicon and glass show only isotropic magnetisation, whereas those sputtered on a polyimide (Kapton^TM) substrate exhibited either isotropic or anisotropic magnetisation depending upon composition. Similar findings were obtained for equivalent evaporated films. Received 23 October 2001 and Received in final form 29 January 2002     

Vibrational spectroscopy characterization of magnetron sputtered silicon oxide and silicon oxynitride films

Vibrational (infrared and Raman) spectroscopy has been used to characterize SiO_xN_y and SiO_x films prepared by magnetron sputtering on steel and silicon substrates. Interference bands in the infrared reflectivity measurements provided the film thickness and the dielectric function of the films. Vibrational modes bands were obtained both from infrared and Raman spectra providing useful information on the bonding structure and the microstructure (formation of nano-voids in some coatings) for these amorphous (or nanocrystalline) coatings. X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM) analysis have also been carried out to determine the composition and texture of the films, and to correlate these data with the vibrational spectroscopy studies. The angular dependence of the reflectivity spectra provides the dispersion of vibrational and interference polaritons modes, what allows to separate these two types of bands especially in the frequency regions where overlaps/resonances occurred. Finally the attenuated total reflection Fourier transform infrared measurements have been also carried out demonstrating the feasibility and high sensitivity of the technique. Comparison of the spectra of the SiO_xN_y films prepared in various conditions demonstrates how films can be prepared from pure silicon oxide to silicon oxynitride with reduced oxygen content.     

Effect of oxygen partial pressure on the structural and optical properties of dc reactive magnetron sputtered molybdenum oxide films

Molybdenum oxide films (MoO₃) were deposited on glass and crystalline silicon substrates by sputtering of molybdenum target under various oxygen partial pressures in the range 8 × 10⁻⁵–8 × 10⁻⁴ mbar and at a fixed substrate temperature of 473 K employing dc magnetron sputtering technique. The influence of oxygen partial pressure on the composition stoichiometry, chemical binding configuration, crystallographic structure and electrical and optical properties was systematically studied. X-ray photoelectron spectra of the films formed at 8 × 10⁻⁵ mbar showed the presence of Mo⁶⁺ and Mo⁵⁺ oxidation states of MoO₃ and MoO_3−x. The films deposited at oxygen partial pressure of 2 × 10⁻⁴ mbar showed Mo⁶⁺ oxidation state indicating the films were nearly stoichiometric. It was also confirmed by the Fourier transform infrared spectroscopic studies. X-ray diffraction studies revealed that the films formed at oxygen partial pressure of 2 × 10⁻⁴ mbar showed the presence of (0 k 0) reflections indicated the layered structure of α-phase MoO₃. The electrical conductivity of the films decreased from 3.6 × 10⁻⁵ to 1.6 × 10⁻⁶ Ω⁻¹ cm⁻¹, the optical band gap of the films increased from 2.93 to 3.26 eV and the refractive index increased from 2.02 to 2.13 with the increase of oxygen partial pressure from 8 × 10⁻⁵ to 8 × 10⁻⁴ mbar, respectively.     

Electrochemical properties of undoped CVD diamond films

The electrochemical properties of undoped diamond polycrystalline films grown on tungsten wire substrates using methanol as a precursor are described. The diamond film quality was changed by introducing sp²-bonded non-diamond carbon impurity through adjustment of the methanol-to-hydrogen (C/H) source gas ratio used for diamond growth.The electrodes were characterized by Raman spectroscopy, scanning electronic microscopy (SEM) and cyclic voltammetry (CV).Diamond coated tungsten wires were then used as a working electrode to ascertain their electrochemical behavior in electrolytic medium. Electrochemical windows of these films were found to be suitable in the potential range of [−2.5 V, +2.2 V] vs. Ag/AgCl in acid medium (0.1 M KCl).The electrochemical behavior was evaluated also using the Fe(CN)₆^3−/4−redox couple.The results demonstrate that the grain boundaries and sp²-hybridized carbon impurity can have a significant influence on electrochemical window of undoped diamond electrodes. It was observed that with increasing sp² carbon impurity concentration the electrochemical window decreases.     

Effect of substrate temperature on the structural, optical and electrical properties of dc magnetron sputtered tantalum oxide films

dc reactive magnetron sputtering technique was employed for deposition of tantalum oxide films on quartz and silicon substrates by sputtering of pure tantalum target in the presence of oxygen and argon gases under various substrate temperatures in the range 303-973 K. The variation of cathode potential with the oxygen partial pressure was systematically studied. The influence of substrate temperature on the chemical binding configuration, crystal structure and optical properties was investigated. X-ray photoelectron spectroscopic studies indicated that the films formed at oxygen partial pressures ≥1 × 10⁻⁴ mbar were stoichiometric. The Fourier transform infrared spectroscopic studies revealed that the films formed up to substrate temperatures <673 K showed a broad absorption band at 750-1000 cm⁻¹ and a sharp band at 630 cm⁻¹ indicated the presence of amorphous phase while at higher substrate temperatures the appearance of bands at about 810 and 510 cm⁻¹ revealed the polycrystalline nature. The effect of substrate temperature on the electrical characteristics of Al/Ta₂O₅/Si structure was investigated. The dielectric constant values were in the range 17-29 in the substrate temperature range of 303-973 K. The current-voltage characteristics showed modified Poole-Frenkel conduction mechanism with a tendency for reduction of the compensation level. The optical band gap of the films decreased from 4.44 to 4.25 eV and the refractive index increased from 1.89 to 2.25 with the increase of substrate temperature from 303 to 973 K.     

Temperature dependence of the optical properties of ion-beam sputtered ZrN films

The reflectivity of sputtered Zirconium nitride films on glass substrate has been investigated in the spectral energy range of 0.8–6.1 eV as a function of deposition temperature varying between 373 and 723 K. Optical constants of the prepared films have been determined using the Drude analysis. Experimental results showed strong dependency of optical properties of the films, such as optical resistivity on the substrate temperature. The temperature increase of the substrate has shown an increase in both the plasmon frequency and electron scattering time. The electrical behavior of the films showed a good agreement between their optical and electrical resistivity.