Temperature dependence of the microstructure and resistivity of indium zinc oxide films deposited by direct current magnetron reactive sputtering

Indium zinc oxide (IZO) films were deposited as a function of the deposition temperature using a sintered indium zinc oxide target (In₂O₃:ZnO = 90:10 wt.%) by direct current (DC) magnetron reactive sputtering method. The influence of the substrate temperature on the microstructure, surface roughness and electrical properties was studied. With increasing the temperature up to 200 °C, the characteristic properties of amorphous IZO films were improved and the specific resistivity was about 3.4 × 10^− 4 Ω cm. Change of structural properties according to the deposition temperature was also observed with X-ray diffraction patterns, transmission electron microscopy, X-ray photoelectron spectroscopy, and atomic force microscopy. IZO films deposited above 300 °C showed polycrystalline phases evolved on the amorphous IZO layer. Very flat surface roughness could be obtained at lower than 200 °C of the substrate temperature, while surface roughness of the films was increased due to the formation of grains over 300 °C. Consequently, high quality IZO films could be prepared by DC magnetron sputtering with O₂/Ar of 0.03 and deposition temperature in range of 150-200 °C; a specific resistivity of 3.4 × 10^− 4 Ω cm, and the values of peak to valley roughness and root-mean-square roughness are less than 4 nm and 0.5 nm, respectively.     

High conductivity and transparent ZnO:Al films prepared at low temperature by DC and MF magnetron sputtering

Aluminum-doped zinc oxide thin films have been deposited by DC and MF magnetron sputtering from a ceramic oxide target in argon atmosphere without direct heating of the substrates. The samples were prepared at different predetermined conditions of input power or discharge voltage and the influence upon electronic, optical, and microstructural properties has been investigated. The as-deposited layers show low resistivity, such as 9 × 10^− 4 Ω cm minimum for DC excitation and 1.2 × 10^− 3 Ω cm for MF mode, with growth rates up to 130 nm/min, and resulting substrate temperatures always below 200 °C. Low resistivity of the films is combined with high transmission, 85-90% in the visible wavelength range (400-800 nm). A strong (002) texture perpendicular to the substrate has been found, with lower strain for DC than for MF sputtering.     

Mechanism of biaxial alignment in thin films, deposited by magnetron sputtering

Biaxially aligned TiN layers have been deposited by reactive unbalanced magnetron sputtering. In this work, a mechanism for the resulting microstructure and biaxial alignment of the deposited TiN layers will be discussed. According to the described model, the resulting biaxial alignment is caused by an overgrowth mechanism (zone T) due to an anisotropy in growth rate of the different oriented grains towards the incoming material flux. Hence, the in-plane alignment will mainly depend on two parameters: the mobility during the growth (zone T condition) and the spread on the incoming material flux. This spread on the incoming material flux has been calculated by an earlier published Monte Carlo simulation program of the transport of sputtered particles towards the substrate. The model for the mechanism of biaxial alignment is validated by comparing the experimental and theoretical influence of target-substrate distance and working pressure on the resulting in-plane alignment.     

Structural properties of films grown by magnetron sputtering of a BiFeO3 target

Thin films have been prepared on silicon substrates by pulsed DC magnetron sputtering of a BiFeO₃ target under an Ar/O₂ mixture with various oxygen flow (0-50 sccm) at room temperature. Due to the low deposition-temperature, the as-grown films are amorphous. As a consequence, we have investigated the effect of the annealing temperature (400-900 °C) and atmosphere (100% N₂ or 90% N₂/10% O₂) on the crystallisation. Microstructural investigations (XRD, HREM, Raman and FTIR spectroscopy) have been performed in order to determine the structural properties of the films and to establish the experimental parameters leading to BiFeO₃ films. A temperature-dependent Raman study points to a spin-phonon coupling around the Néel temperature.     

In-situ electrical characterization of ultrathin TiN films grown by reactive dc magnetron sputtering on SiO2

Ultrathin TiN films were grown by reactive dc magnetron sputtering on thermally oxidized Si (100) substrates. The electrical resistance of the films was monitored in-situ during growth in order to determine the minimum thickness of a continuous film. The coalescence thickness has a minimum of 1 nm at a growth temperature of 400 °C after which it increases with growth temperature. The minimum thickness of a continuous film decreases with increasing growth temperature from 2.9 nm at room temperature to 2.2 nm at 650 °C. In-situ resistivity measurements show that films grown at 500 °C and above are resistant to oxidation indicating high density. X-ray photoelectron spectroscopy and X-ray diffraction measurements show that the TiN grain stoichiometry and grain size increases with increasing growth temperature.     

Temperature dependence of InN film deposition by an RF plasma-assisted reactive ion beam sputtering deposition technique

Indium nitride (InN) films were deposited on Si(100) substrates using a radiofrequency (RF) plasma-assisted reactive ion beam sputtering deposition technique at various substrate temperatures. The X-ray diffraction patterns of the InN films suggest that the InN films deposited at substrate temperatures up to 370 °C were cubic crystalline InN; and at 500 °C, the InN film was hexagonal crystalline InN. In a scanning electron microscope image of the InN film surface, facets of cubic single-crystalline InN grains were clearly observed on the InN film deposited at 370 °C. The inclusion of metallic indium appeared on the InN film deposited at 500 °C.     

Refractive index, optical bandgap and oscillator parameters of organic films deposited by vacuum evaporation technique

In this work, the organic thin films of 8-hydroxyquinoline aluminum (Alq₃), 9,10-bis-(β-naphthyl)-anthrene (ADN), and aluminum (III) bis-(2-methyl-8-quninolinato)-4-phenylphenolate (BAlq) were deposited by vacuum evaporation technique, and the optical and dielectric properties of the films were investigated. The optical constants such as refractive index, extinction coefficient, dielectric constant and dissipation factor were determined from the measured transmittance spectra using the envelope method. Meanwhile, the dispersion behavior of the refractive index was studied in terms of the single-oscillator Wemple-DiDomenico (W-D) model, and the physical parameters of the average oscillator strength, average oscillator wavelength, average oscillator energy, the refractive index dispersion parameter and the dispersion energy were achieved. Furthermore, the optical bandgap values were calculated by W-D model and Tauc model, respectively, and the values obtained from W-D model are in agreement with those determined from the Tauc model. These results provide some useful references for the potential application of the thin films in optoelectronic devices.     

Friction and adhesion properties of fluorocarbon polymer thin films prepared by magnetron sputtering

Fluorocarbon polymer thin films were deposited onto a SUS302 substrate with a poly(tetrafluoroethylene) (PTFE) target by three different types of r.f. magnetron sputtering systems with strong, weak and unbalanced magnetic fields. Friction and adhesion properties of these polymer thin films were evaluated.Friction coefficient of polymer thin films prepared with strong magnetic field, unbalanced magnetron and without magnetron (r.f. sputtering) was almost the same level, however, that prepared with the weak magnetic field was slightly lower than those of other thin films. Wear durability of polymer thin film increased with increase of the magnetic field.Adhesion strength between these thin films and SUS302 substrate and shear stress were measured by SAICAS. Both of the adhesion strength and shear stress of polymer thin films prepared with r.f. sputtering (without magnetron) were slightly higher than those prepared by magnetron sputtering systems.     

Substrate temperature dependent morphology and resistivity of pulsed laser deposited iridium oxide thin films

Iridium oxide (IrO₂) thin films were deposited on Si (100) substrates by means of pulsed laser deposition technique at various substrate (deposition) temperatures ranging from 250 to 500 °C. Effects of substrate temperature on the crystalline nature, morphology and electrical properties of the deposited films were analyzed by using X-ray diffraction, Raman spectroscopy, Scanning electron microscopy and four-point probe method. It was found that the above properties were strongly dependent on the substrate temperature. The as-deposited films at all substrate temperatures were polycrystalline tetragonal IrO₂ and the preferential growth orientation changed with the substrate temperature. IrO₂ films exhibited fairly homogeneous thickness and good adhesion with the substrate, the average feature size increases with the substrate temperature. The room-temperature resistivity of IrO₂ films decreased with the increase of substrate temperature and the minimum resistivity of (42 ± 6) μΩ cm was obtained at 500 °C. The resistivity of IrO₂ films correlated well with the corresponding film morphology changes.     

Compositional analysis and optical properties of Ag-doped ITO films

ITO and Ag-ITO composite films were deposited on glass substrates by DC magnetron sputtering. Scanning electron microscope images indicated that Ag existed in the form of nanoparticles. X-ray photoelectron spectroscopic analysis illustrated that both Ag doping and heat treatment had obvious influence on the composition and element chemical state of the films. Ag doping dramatically decreased the transmittance of the film. But after being annealed, Ag-ITO films exhibited the high average transmittance of 80-90% in visible wavelength range. By using the spectroscopic ellipsometry optimization, the optical constants were extracted from the transmittance spectra. The results suggested the potential use of Ag-ITO films for antireflection coating system.     

Influence of oxygen partial pressure on the structure and photoluminescence of direct current reactive magnetron sputtering ZnO thin films

The effects of oxygen partial pressure on the structure and photoluminescence (PL) of ZnO films were studied. The films were prepared by direct current (DC) reactive magnetron sputtering with various oxygen concentrations at room temperature. With increasing oxygen ratio, the structure of films changes from zinc and zinc oxide phases, single-phase ZnO, to the (002) orientation, and the mechanical stresses exhibit from tensile stress to compressive stress. Films deposited at higher oxygen pressure show weaker emission intensities, which may result from the decrease of the oxygen vacancies and zinc interstitials in the film. This indicates that the emission in ZnO film originates from the oxygen vacancy and zinc interstitial-related defects. From optical transmittance spectra of ZnO films, the plasma edge shifts towards the shorter wavelength with the improvement of film stoichiometry.     

Thickness dependence of structure and optical properties of silver films deposited by magnetron sputtering

A series of silver films with different thickness were prepared under identical conditions by direct current magnetron sputtering. The optical properties of the silver films were measured using spectrophotometric techniques and the optical constants were calculated from reflection and transmission measurements made at near normal incidence. The results show that the optical properties and constants are affected by films' thickness. Below the critical thickness of 17 nm at which Ag film forms a continuous film, the optical properties and constants vary significantly as the thickness of films increases and then tends to a stable value which is reached at 41 nm. X-ray diffraction measurements were carried out to examine the structure and stress evolution of the Ag films as a function of films' thickness. It was found that the interplanar distance of (111) orientation decreases when the film thickness increases and tends to be close to that of bulk material. The compressive strains also decrease with increasing thickness.     

Low temperature deposition of ITO on organic films by using negative ion assisted dual magnetron sputtering system

In a magnetron sputter type negative metal ion deposition, the influence of positive bias voltage (V_b) on the surface morphology, electrical resistivity, optical transmittance, and microhardness of ITO prepared on organic polycarbonate films has been investigated. In this study, the V_b increased from 0 to 250 V to attract secondary negative In and Sn metal ions, which were produced from ITO target by surface negative ionization with intense Cs ion bombardments. During deposition although reactive oxygen gas was not introduced into the chamber, by adjusting V_b at 100 V, ITO films on polycarbonate substrate with resistivity as low as 6.1×10⁻⁴ Ω cm and transmittance over 90% at 550 nm have been obtained without intentional substrate heating.AFM measurement also shows that surface roughness varied significantly with V_b. However, too intense ion bombardment originated by high V_b (>100 V) condition increased surface roughness and as a result deteriorated the electrical and optical property of ITO films.     

Characterization of (Al, Si)N films deposited by balanced magnetron sputtering

Hard and transparent nanocomposite (Al, Si)N films are attractive for optical applications. In this paper, experimental results will be reported on nanocomposite (Al, Si)N films prepared by balanced magnetron sputtering. Microstructure and properties of the films were systematically characterized as a function of Si content of the films. It is shown that the (Al, Si)N films are transparent and exhibit no absorption in a wide range of wavelengths from ~ 0.3 to ~ 9 µm, i.e. from ultraviolet to mid-infrared region. Maximum hardness exceeding 25 GPa has been obtained when the Si content of the films is above 25 at.% and the microstructure of the films undergoes a transformation from nanocrystalline to amorphous states. It is demonstrated that the microstructure detail of the films is different, as compared with that of the films prepared by using unbalanced magnetron sputtering, and the reasons for this discrepancy is discussed.     

Plasma influence on the properties and structure of indium tin oxide films produced by reactive middle frequency pulsed magnetron sputtering

Reactive pulsed magnetron sputtering was used to produce conductive and transparent tin-doped indium oxide (ITO) films with low thickness inhomogeneity. Due to the parallel operation of two magnetrons, the deposition system allows in situ investigations of the plasma influence on the film properties. The distribution of the film resistivity, refractive index, structure and stoichiometry along the substrate are presented and related to the spatial distribution of the plasma flow escaping the magnetrons, and the substrate temperature. A higher plasma flow likely causes a localized relaxation of the distorted In-O bonds in amorphous phase which prevails in ITO films prepared at unheated substrates. This leads to a decrease of the film resistivity due to free electrons density and mobility enhancement. The free electron density increase is caused likely by generation of oxygen vacancies. Deposition on a heated substrate (T_s / T_m = 0.3) leads to a change of the film growth mode due to enhanced surface diffusion of the adatoms which results in a textured low resistivity film. This also causes significant improvements of the homogeneity of the film properties that is important for ITO applications.     

The effect of argon pressure on the structural and photocatalytic characteristics of TiO2 thin films deposited by d.c. magnetron sputtering

TiO₂ thin films of 200-300 nm thickness were deposited by d.c. magnetron sputtering onto glass substrates from a semiconducting TiO_2−x target in pure Ar using pressures between 0.1 and 1.0 Pa. The obtained TiO₂ coatings are transparent and have refractive indices between 2.5 and 1.9. Post deposition heat treatment at different temperatures was performed to achieve crystallization of anatase TiO₂. The as-deposited and heat treated films were examined with UV-VIS (transmission), SEM and XRD to investigate the influence of the argon pressure during deposition on the structural development during heat treatment. Additionally, the photocatalytic activity of the films was tested by measuring the decomposition rate of ethanol in a controlled gas atmosphere simulating air, and was related to their respective microstructures.     

Investigation of antiperovskite Mn3CuNx film prepared by DC reactive magnetron sputtering

Antiperovskite Mn₃CuN_x film was prepared by dc reactive magnetron sputtering. It is the first time to report an antiperovskite ternary nitride film. The composition and crystal structure were characterized by energy dispersive spectroscope (EDS), X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD). From the XRD pattern, it displays a (1 0 0) preferential orientation. A comparative study on the properties of Mn₃CuN_x film and the bulk sample was presented. The film exhibits an antiferromagnetic to paramagnetic transition around 135 K, similar with the bulk sample. With temperature, the resistivity of the film shows semiconductor-like behavior throughout the measured temperature region, whereas there is an abrupt drop around the magnetic transition for the bulk. The variable temperature XRD results indicate that the film did not display any structure transition and shows a normal linear thermal expansion property around the magnetic transition.     

Effect of substrate temperature on the physical properties of In2O3:Mo films: Prepared by an activated reactive evaporation

Transparent and high conductive molybdenum doped indium oxide (IMO) thin films have been deposited on glass substrates by activated reactive evaporation. The effect of substrate temperature on the structure, surface morphology, electrical, optical and photoluminescence properties of these films were systematically examined and it was found that crystallinity and growth orientation of the films were significantly influenced by substrate temperature. In addition the films exhibited a low electrical resistivity of 5.2 × 10⁻⁴ Ω cm with an optical transmittance 90% in the visible region of the solar spectrum at a substrate temperature of 573 K. Intensive blue PL bands at 415 and 440 nm were observed in the photoluminescence spectrum at room temperature.     

Effects of hydrogen gas on properties of tin-doped indium oxide films deposited by radio frequency magnetron sputtering method

Tin-doped indium oxide (ITO) films were deposited at ∼ 70 °C of substrate temperature by radio frequency magnetron sputtering method using an In₂O₃-10% SnO₂ target. The effect of hydrogen gas ratio [H₂ / (H₂ + Ar)] on the electrical, optical and mechanical properties was investigated. With increasing the amount of hydrogen gas, the resistivity of the samples showed the lowest value of 3.5 × 10^− 4 Ω·cm at the range of 0.8-1.7% of hydrogen gas ratio, while the resistivity increases over than 2.5% of hydrogen gas ratio. Hall effect measurements explained that carrier concentration and its mobility are strongly related with the resistivity of ITO films. The supplement of hydrogen gas also reduced the residual stress of ITO films up to the stress level of 110 MPa. The surface roughness and the crystallinity of the samples were investigated by using atomic force microscopy and x-ray diffraction, respectively.     

Influence of DC magnetron sputtering parameters on the properties of amorphous indium zinc oxide thin film

Amorphous or crystalline indium zinc oxide (IZO) thin films, which are highly transparent and conducting, were deposited by DC magnetron sputtering. X-Ray diffraction technique was used for analyzing microstructures of the films, and also differential thermal analysis was performed for observing their crystallization behavior. The IZO thin films prepared were crystallized at much higher temperature than ITO films were. The crystallized samples showed (222) preferred orientations. By varying process parameters, the optimum conditions for the highest electrical conductivity and optical transmittance, and the lowest surface roughness were found. The resistivity of IZO films decreased as the deposition temperature increased until 250 °C, but sharp rise occurred at or above 300 °C. The extinction coefficients diminished in the films prepared with the conditions of higher deposition temperature, sputtering gas of light mass, and heat treatment. However, excessive amount of oxygen flow during deposition brought about the increase of the extinction coefficients. The variations of extinction coefficients mainly influenced the transmittance of the samples. On the basis of X-ray photoelectron spectroscopy analysis, atomic force microscopy measurement, spectroscopic ellipsometry and spectrophotometer measurement, several characteristics of IZO thin films were discussed comparing with those of ITO thin films. Very low surface roughness of IZO thin films could satisfy the requirement for organic light-emitting diode.