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.     

Structural and optical properties of electrodeposited molybdenum oxide thin films

Electrosynthesis of Mo(IV) oxide thin films on F-doped SnO₂ conducting glass (10-20/Ω/□) substrates were carried from aqueous alkaline solution of ammonium molybdate at room temperature. The physical characterization of as-deposited films carried by thermogravimetric/differential thermogravimetric analysis (TGA/DTA), infrared spectroscopy and X-ray diffraction (XRD) showed the formation of hydrous and amorphous MoO₂. Scanning electron microscopy (SEM) revealed a smooth but cracked surface with multi-layered growth. Annealing of these films in dry argon at 450 °C for 1 h resulted into polycrystalline MoO₂ with crystallites aligned perpendicular to the substrate. Optical absorption study indicated a direct band gap of 2.83 eV. The band gap variation consistent with Moss rule and band gap narrowing upon crystallization was observed.Structure tailoring of as-deposited thin films by thermal oxidation in ambient air to obtain electrochromic Mo(VI) oxide thin films was exploited for the first time by this novel route. The results of this study will be reported elsewhere.     

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.     

Properties of dc magnetron sputtered Cu2O films prepared at different sputtering pressures

The sputtering pressures maintained during the deposition of Cu₂O films, by dc reactive magnetron sputtering, influence the structural, electrical and optical properties. The crystalline orientation mainly depends on the sputtering pressure. The films deposited at a sputtering pressure of 4 Pa showed single-phase Cu₂O films along (1 1 1) direction. The electrical resistivity of the films increased from 1.1 × 10¹ Ω cm to 3.2 × 10³ Ω cm. The transmittance of the films increased from 69% to 88% with the increase of sputtering pressure from 2.5 Pa to 8 Pa.     

反应气压对直流磁控反应溅射制备的氧化银薄膜的结构和光学性质的影响

利用直流磁控反应溅射技术,通过调节反应气压(RP),在250 ℃衬底温度下制备了一系列氧化银 (Ag_xO) 薄膜,并利用X射线衍射谱、能量色散谱和分光光度计重点研究了RP对Ag_xO薄膜的结构和光学性质的影响. 研究结果表明,随着RP从0.5 Pa升高到3.5 Pa,薄膜明显呈现了从两相(AgO+Ag₂O)到单相(Ag₂O)结构再到两相(Ag₂O+AgO)结构的演变. 特 关键词： 氧化银薄膜 直流磁控反应溅射 X射线衍射谱 光学性质     

Evolution of the structural and optical properties of silver oxide films with different stoichiometries deposited by direct-current magnetron reactive sputtering

Nitrogen doping of silver oxide(AgxO) film is necessary for its application in transparent conductive film and diodes because intrinsic AgxO film is a p-type semiconductor with poor conductivity.In this work,a series of AgxO films is deposited on glass substrates by direct-current magnetron reactive sputtering at different flow ratios(FRs) of nitrogen to O2.Evolutions of the structure,the reflectivity,and the transmissivity of the film are studied by X-ray diffractometry and sphectrophotometry,respectively.The specular transmissivity and the specular reflectivity of the film decreasing with FR increasing can be attributed to the evolution of the phase structure of the film.The nitrogen does not play the role of an acceptor dopant in the film deposition.     

Optical and electrical properties of nanocrystal zinc oxide films prepared by dc magnetron sputtering at different sputtering pressures

The nanocrystal thin films of zinc oxide doped by Al (ZnO:Al) were deposited by dc reactive magnetron sputtering on the glass substrates, in the pressure range of 33-51 Pa. From the X-ray diffraction patterns, the nanocrystalline structure of ZnO:Al films and the grain size were determined. The optical transmission spectra depend from the sputtering pressure, but their average value was 90% in the range from 33 Pa to 47 Pa. Also, the sputtering pressure changes the optical band gap of ZnO:Al films, which is highest for films deposited at 37 Pa, 40 Pa and 47 Pa. The obtained films at room temperature have a sheet resistance of 190 Ω/cm² which increases with time, but the films annealed at temperature of 400 °C have constant resistance. The surface morphology of the films was studied by Scanning electron microscopy. XPS spectra showed that the peak of O1s of the as-deposited films is smaller than the peak of the annealed ZnO:Al films.     

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     

A study of the optical properties of titanium oxide films prepared by dc reactive magnetron sputtering

TiO₂ thin films were deposited on the glass substrates by dc reactive magnetron sputtering technique at different sputtering pressures (2 × 10⁻³ to 2 × 10⁻² mbar). The films prepared at low pressures have an anatase phase, and the films prepared at high pressures have an amorphous phase. The optical properties were studied by measuring the transmittance and the ellipsometric spectra. The optical constants of the films in the visible range were obtained by fitting the transmittance combined with the ellipsometry measurements using the classical model with one oscillator. The refractive index of the films decreases from 2.5 until 2.1 as the sputtering pressure increases from 2 × 10⁻³ to 2 × 10⁻² mbar. The films prepared at the pressure higher than 6 × 10⁻³ mbar show a volume inhomogeneity. This volume inhomogeneity has been calculated by fitting the transmittance and the ellipsometric spectra. The volume inhomogeneity of the film prepared at the highest sputtering pressure is about 10%. Although the films prepared at high pressures show a large volume inhomogeneity, they have low extinction coefficients. It is suggested that the anatase phase results in more light scattering than amorphous phase does, and then a high extinction coefficient.     

Development of structural and optical properties of WOx films upon increasing oxygen partial pressure during reactive sputtering

WO_x films were prepared by reactive dc magnetron sputtering using tungsten target. Sputtering was carried out at a total pressure of 1.2 Pa using a mixture of argon plus oxygen in an effort to determine the influence of the oxygen partial pressure on structural and optical properties of the films. The deposition rate decreases significantly as the surface of the target is oxidized. X-Ray diffraction revealed the amorphous nature of all the films prepared at oxygen partial pressures higher than 1.71×10⁻³ Pa. For higher oxygen partial pressures, fully transparent films were deposited, which showed a slight increase in optical band gap with increasing oxygen partial pressure, while the refractive index was simultaneously decreased.     

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.     

Microstructure, optical and electrical properties of nitrogen doped sp-rich a-C thin films grown by facing-target magnetron sputtering

N atoms were incorporated into sp²-rich a-C networks using DC facing-target reactive sputtering at various N₂ fraction (P_N2) and their structure and opto-electrical properties were investigated systematically. As P_N2 increases, the fraction of CN bonded carbons (or the N content) increases primarily at the expense of the CC bonded carbons and then reaches its saturated value at P_N2 > 40%. The incorporated N preferentially forms different kinds of non-aromatic CN phase, leading to more localization of π electrons and the loss of the connectivity of nanographite fragments in the films, which is different from the case in N-doped sp³-rich a-CN_x films. Hence, with increasing P_N2, the a-C(:N) film converts from a semiconductor with a narrower optical band gap to an insulator-like material with a wider gap. Additionally, the variation of optical constants (n and k) and spin defects are related to the enhancement of the non-aromatic CN phase.     

Influence of substrate bias voltage on the properties of magnetron sputtered Cu2O films

Thin films of cuprous oxide (Cu₂O) were deposited on glass substrates at various bias voltages using DC reactive magnetron sputtering technique. The effects of substrate bias voltage on structural, electrical and optical properties were systematically analyzed. The crystallographic structure and orientation of the crystallites were strongly influenced by the bias voltage.     

Crystal structure and tribological properties of molybdenum disulfide films prepared by magnetron sputtering technology

Molybdenum disulfide (MoS₂) is widely used in practice due to its excellent lubricating properties. However, research on the tribological properties of magnetron sputtering for depositing MoS₂ films remains limited. Herein, the tribological properties of MoS₂ films were investigated in detail through a series of characterization and friction coefficient tests. MoS₂ films were deposited onto silicon substrates by magnetron sputtering under different radio-frequency powers (P_rf). With increased P_rf, the crystallinity of the films gradually increases, whereas the friction coefficient initially decreases and then increases. P_rf also affects the chemical composition, surface morphology, and grain size of MoS₂ films. At P_rf = 300 W, the film surface is dense and smooth, the grain distribution is uniform. Moreover, the films have superior tribological properties and low friction coefficient, which can be attributed to the weak van der Waals force among MoS₂ layers and the microscopic morphology of the films. All these results indicate that by reasonably controlling the preparation parameters, MoS₂ films with excellent tribological properties can be prepared by magnetron sputtering.     

Study of the effect of the oxygen partial pressure on the properties of rf reactive magnetron sputtered tin-doped indium oxide films

The influence of the oxygen partial pressure on the properties of indium tin oxide films deposited by rf reactive magnetron sputtering has been studied. The oxygen partial pressure was varied from 3.2 × 10⁻⁴ to 1.0 × 10⁻³ mbar. It has been found that the 4 × 10⁻⁴ mbar of oxygen partial pressure is a critical point. When the oxygen partial pressure is lower than 4 × 10⁻⁴ mbar, the deposition rate of the films is high; the films have low transmittance and electrical resistivity; the X-ray diffraction shows that the films have a random orientation and the images of the scanning electron microscopy show that the films surface are smooth without structure. When the pressure is higher than 4 × 10⁻⁴ mbar, the deposition rate is low and does not change as the oxygen partial pressure is further increased; the transmittance and the electrical resistivity are both high; the films show the preferred orientation along the (440) direction; the films surface show a clear structure and as the pressure is increased further, the films become porous. Considering both the factor of transmittance and resistivity, the optimum oxygen partial pressure will be 3.6 × 10⁻⁴ mbar. The films prepared at this pressure have 80% transmittance and 9 × 10⁻⁴ Ω cm resistivity.     

Growth, structural, and magnetic properties of iron nitride thin films deposited by dc magnetron sputtering

FeN thin films were deposited on glass substrates by dc magnetron sputtering at different Ar/N₂ discharges. The composition, structure and the surface morphology of the films were characterized using X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), and atomic force microscopy (AFM). Films deposited at different nitrogen pressures exhibited different structures with different nitrogen contents, and the surface roughness depended on the mechanism of the film growth. Saturation magnetization and coercivity of all films were determined using superconducting quantum interference device, which showed that if N₂/(Ar+N₂) flow ratio was equal to or larger than 30% the nonmagnetic single-phase γ″-FeN appeared. If N₂/(Ar+N₂) flow ratio was less than 10%, the films consisted of the mixed phases of FeN_0.056 and γ′-Fe₁₆N₂, whose saturation magnetizations were larger than that of -Fe. If N₂/(Ar+N₂) flow ratio was 10%, the phases of γ′-Fe₄N and -Fe₃N appeared, whose saturation magnetizations were lower than that of -Fe.     

Enhanced electrical stability of flexible indium tin oxide films prepared on stripe SiO2 buffer layer-coated polymer substrates by magnetron sputtering

The electrical stability of flexible indium tin oxide (ITO) films fabricated on stripe SiO₂ buffer layer-coated polyethylene terephthalate (PET) substrates by magnetron sputtering was investigated by the bending test. The ITO thin films with stripe SiO₂ buffer layer under bending have better electrical stability than those with flat SiO₂ buffer layer and without buffer layer. Especially in inward bending text, the ITO thin films with stripe SiO₂ buffer layer only have a slight resistance change when the bending radius r is not less than 8 mm, while the resistances of the films with flat SiO₂ buffer layer and without buffer layer increase significantly at r = 16 mm with decreasing bending radius. This improvement of electrical stability in bending test is due to the small mismatch factor α in ITO-SiO₂, the enhanced interface adhesion and the balance of residual stress. These results indicate that the stripe SiO₂ buffer layer is suited to enhance the electrical stability of flexible ITO film under bending.     

The influence of using different substrates on the structural and optical characteristics of ZnO thin films

ZnO thin films with thikness d = 100 nm were deposited onto different substrates such as glass, kapton, and silicon by radio frequency magnetron sputtering. The structural analyses of the films indicate they are polycrystalline and have a wurtzite (hexagonal) structure.The ZnO layer deposited on kapton substrate shows a stronger orientation of the crystallites with (0 0 2) plane parallel to the substrate surface, as compared with the other two samples of ZnO deposited on glass and silicon, respectively.All three layers have nanometer-scale values for roughness, namely 1.7 nm for ZnO/glass, 2.4 nm for ZnO/silicon, and 6.8 nm for ZnO/kapton. The higher value for the ZnO layer deposited on kapton substrate makes this sample suitable for solar cells applications. Transmission spectra of these thin films are strongly influenced by deposition conditions. With our deposition conditions the transparent conducting ZnO layer has a good transmission (78-88%) in VIS and NIR domains. The values of the energy gap calculated from the absorption spectra are 3.23 eV for ZnO sample deposited onto glass substrate and 3.30 eV for the ZnO sample deposited onto kapton polymer foil substrate. The influence of deposition arrangement and oxidation conditions on the structural, morphological, and optical properties of the ZnO films is discussed in the present paper.     

Effects of oxygen partial pressure and substrate temperature on the structure and optical properties of MgxZn1−xO thin films prepared by magnetron sputtering

Deposited with different oxygen partial pressures and substrate temperatures, Mg_xZn_1−xO thin films were prepared using a Mg_0.6Zn_0.4O ceramic target by magnetron sputtering. The structural and optical properties of the prepared thin films were investigated. The X-ray diffraction spectra reveal that all the films on quartz substrate are grown along (2 0 0) orientation with cubic structure. The lattice constant decreases and the crystallite size increases with the increase of substrate temperature. Both energy dispersive X-ray spectroscopy and calculated results suggest the ratio of Mg/Zn increases with increasing substrate temperature. The thin film deposited with T_s = 500 °C has a minimal rms roughness of 7.37 nm. The transmittance of all the films is higher than 85% in the visual region. The optical band gap is not sensitive to the oxygen partial pressure, while it increases from 5.63 eV for T_s = 100 °C to 5.95 eV for T_s = 700 °C. In addition, the refractive indices calculated from transmission spectra are sensitive to the substrate temperature. The photoluminescence spectra of Mg_xZn_1−xO thin films excited by 330 nm ultraviolet light indicate that the peak intensity of the spectra is influenced by the oxygen partial pressure and substrate temperature.     

Effect of oxygen partial pressure on the structural and optical properties of ZnO film deposited by reactive sputtering

Effects of variation of the oxygen partial pressure on the structural and optical properties of zinc oxide (ZnO) thin films prepared by reactive radio-frequency sputtering were investigated. Measurements by X-ray diffraction (XRD) and atomic force microscopy (AFM) indicated that the crystallinity and the surface morphology were sensitive to the oxygen partial pressure. The interfacial and optical properties of the targeted films were investigated by spectroscopic ellipsometry (SE) characterization. Based on Tauc-Lorentz (TL) model, the optical constants of ZnO films were tentatively extracted in the photon energy ranging from 1.5 to 6.0 eV. Analyses by XRD and SE revealed that the oxygen partial pressure had effect on the orientation of the ZnO films, the surface morphology, the packing density, and the interfacial layers. And the relationship between crystallinity and interfacial layer, as well as the relationship between surface roughness and packing density was discussed. All these had a significant impact on the optical properties illustrated by SE analysis.