Effects of annealing temperature and heat-treatment duration on electrical properties of sol-gel derived indium-tin-oxide thin films

Transparent indium tin oxide (ITO) thin films have been deposited by the dip-coating process on silica substrates using solutions of 2,4-pentanedione, ethanol, indium and tin salts. The films have been first dried in air at 260 °C for 10 min and then annealed in a reducing atmosphere at different temperatures for various durations. The resistivity of ITO layers was found to decrease with increasing the metal concentration of the starting solution or the annealing temperature. Hence, by adjusting both metal concentration in the coating solution and heat-treatment, resistivities lower than 5 × 10^− 3 Ω cm for an annealing temperature of 550 °C and lower than 2 × 10^− 2 Ω cm for an annealing temperature of 300 °C, were obtained. These results are correlated with the density and the size of ITO grains in the films.     

Preparation and characterization of indium zinc oxide thin films by electron beam evaporation technique

In this work, the preparation of In₂O₃-ZnO thin films by electron beam evaporation technique on glass substrates is reported. Optical and electrical properties of these films were investigated. The effect of dopant amount and annealing temperature on the optical and electrical properties of In₂O₃-ZnO thin films was also studied. Different amount of ZnO was used as dopant and the films were annealed at different temperature. The results showed that the most crystalline, transparent and uniform films with lowest resistivity were obtained using 25 wt% of ZnO annealed at 500 °C.     

Properties of Ce-doped ITO films deposited on polymer substrate by DC magnetron sputtering

Ce-doped indium tin oxide (ITO:Ce) films were deposited on flexible polyimide substrates by DC magnetron sputtering using ITO targets containing various CeO₂ contents (CeO₂ : 0, 0.5, 3.0, 4.0, 6.0 wt.%) at room temperature and post-annealed at 200 °C. The crystallinity of the ITO films decreased with increasing Ce content, and it led to a decrease in surface roughness. In addition, a relatively small change in resistance in dynamic stress mode was obtained for ITO:Ce films even after the annealing at high temperature (200 °C). The minimum resistivity of the amorphous ITO:Ce films was 3.96 × 10^− 4 Ωcm, which was deposited using a 3.0 wt.% CeO₂ doped ITO target. The amorphous ITO:Ce films not only have comparable electrical properties to the polycrystalline films but also have a crystallization temperature > 200 °C. In addition, the amorphous ITO:Ce film showed stable mechanical properties in the bended state.     

Structural and opto-electrical properties of the tin-doped indium oxide thin films fabricated by the wet chemical method with different indium starting materials

Tin-doped indium oxide (ITO) thin films were fabricated by the sol-gel spin-coating method with different indium precursor solutions synthesized from In(NO₃)₃ or InCl₃ (denoted as N-ITO and Cl-ITO, respectively). For both N-ITO and Cl-ITO thin films, the increase of mobility/conductivity and the reduction of carrier concentration with increasing annealing temperatures from 400 to 700 °C are related to the increase of crystallization/densification and the annihilation of oxygen vacancies. The refractive index (1.84 at λ = 550 nm), packing density (0.83), conductivity [(234 (Ω-cm)^− 1], and optical band gap (3.95 eV) of N-ITO thin films are higher than that of Cl-ITO thin films, which can be attributed to the higher densification, lower crystallinity, and more free charge carriers of N-ITO thin films. These properties make the indium nitrate-derived ITO thin films have better potential applications for some commercial products.     

Deposition of transparent conductive mesoporous indium tin oxide thin films by a dip coating process

Cetyltrimethyl ammonium bromide (CTAB) templated mesoporous indium tin oxide (ITO) thin films were deposited on quartz plates by an evaporation-induced self-assembly (EISA) process using a dip coating method. The starting solution was prepared by mixing indium chloride, tin chloride, and CTAB dissolved in ethanol. Five to fifty mole percent Sn-doped ITO films were prepared by heat-treatment at 400 °C for 5 h. The structural, adsorptive, electrical, and optical properties of mesoporous ITO thin films were investigated. Results indicate that the mesoporous ITO thin films have an ordered two-dimensional hexagonal (p6mm) structure, with nanocrystalline domains in the inorganic oxide framework. The continuous thin films have highly ordered pore sizes (>20 Å), high Brunauer-Emmett-Teller (BET) surface area up to 340 m²/g, large pore volume (>0.21 cm³/g), outstanding transparency in the visible range (>80%), and show a minimum resistivity of ρ = 1.2 × 10⁻² Ω cm.     

Structural properties of indium tin oxide thin films prepared for application in solar cells

Indium tin oxide (ITO) thin films prepared by rf sputtering were annealed in several temperatures. The electrical, optical and structural properties of these films are systematically investigated. The post annealing of the samples lead to considerably higher electrical conductivity, better optical transparency and larger grain size for the films. In an optimum annealing temperature of 400 °C, we have found that a maximized conductivity of films is achieved without a remarkable loss in their transparency. The sheet resistance of 2.3 Ω/□ and average grain size of 30 nm, are the results of the optimized post processing of films. The investigation for microstructure of films investigated by X-ray diffraction measurement (XRD) shows that a preferential crystal growth toward the (2 2 2) orientation takes place when the annealing temperature increases to 400 °C.     

Structural, thermal and optical characterization of TiO2:ZrO2 thin films prepared by sol-gel method

We have studied the structural and optical properties of thin films of TiO₂, doped with 5% ZrO₂ and deposited on glass substrate (by the sol-gel method). The dip-coated thin films have been examined at different annealing temperatures (350 to 450 °C) and for various layer thicknesses (63-286 nm). Refractive index and porosity were calculated from the measured transmittance spectrum. The values of the index of refraction are in the range of 1.62-2.29 and the porosity is in the range of 0.21-0.70. The coefficient of transmission varies from 50 to 90%. In the case of the powder of TiO₂, doped with 5% ZrO₂, and aged for 3 months in ambient temperature, we have noticed the formation of the anatase phase (tetragonal structure with 14.8 nm grains). However, the undoped TiO₂ exhibits an amorphous phase. After heat treatments of thin films, titanium oxide starts to crystallize at the annealing temperature 350 °C. The obtained structures are anatase and brookite. The calculated grain size, depending on the annealing temperature and the layer thickness, is in the range (8.58-20.56 nm).     

Evaluation of the film formation and the charge transport mechanism of indium tin oxide nanoparticle films

The structure formation and charge transfer of thin nanoparticulate indium tin oxide (ITO) films prepared by dip-coating was studied as a function of stabilizer before and after annealing at different temperatures. The analysis of the film structure by optical methods revealed that it is a function of the stability. Suspensions containing an optimum stabilizer concentration of 0.1 mol/l resulted in densely packed films with a peak specific conductivity of 8.3 S cm^− 1 after annealing at 550 °C for 1 h in air and 121 S cm^− 1 after annealing in forming gas at 250 °C for 1 h, respectively. Furthermore, for the densely packed films fluctuation-induced tunnelling was found to be the dominant charge transport mechanism, whereas for the low density films a thermally activated charge transport was observed. That the films of maximum density showed a metallic charge transport behaviour at temperatures above 300 K indicated the optimal contact between ITO particles had been achieved.     

Low temperature ordering of FePt films by in-situ heating deposition plus post deposition annealing

FePt thin films with 40 nm thickness were prepared on thermally oxidized Si (001) substrates by dc magnetron sputtering at the nominal growth temperature 375 °C. The effects of annealing on microstructure and magnetic properties of FePt thin films were investigated. The as-deposited FePt thin films show soft magnetic properties. After the as-deposited FePt thin films were annealed at various temperatures and furnace cooled, it is found that the ordering temperature of L1₀ FePt phase could be reduced to 350 °C. For FePt thin films annealed at 350 °C, the in-plane and out-of-plane coercivities of the films increased to 510 and 543 kA/m, respectively, and the films had hard magnetic properties. A highly (001) orientation was obtained, when FePt thin films were annealed at 600 °C. And the hysteresis loops of FePt thin films annealed at 600 °C show out-of-plane magnetic anisotropy.     

Preparation of transparent conductive indium tin oxide thin films from nanocrystalline indium tin hydroxide by dip-coating method

Indium tin oxide (ITO) thin films with well-controlled layer thickness were produced by dip-coating method. The ITO was synthesized by a sol-gel technique involving the use of aqueous InCl₃, SnCl₄ and NH₃ solutions. To obtain stable sols for thin film preparation, as-prepared Sn-doped indium hydroxide was dialyzed, aged, and dispersed in ethanol. Polyvinylpyrrolidone (PVP) was applied to enhance the stability of the resulting ethanolic sols. The transparent, conductive ITO films on glass substrates were characterized by X-ray diffraction, scanning electron microscopy and UV-Vis spectroscopy. The ITO layer thickness increased linearly during the dipping cycles, which permits excellent controllability of the film thickness in the range ~ 40-1160 nm. After calcination at 550 °C, the initial indium tin hydroxide films were transformed completely to nanocrystalline ITO with cubic and rhombohedral structure. The effects of PVP on the optical, morphological and electrical properties of ITO are discussed.     

Porous nanostructured ZnO films deposited by picosecond laser ablation

Porous nanostructured polycrystalline ZnO films, free of large particulates, were deposited by picosecond laser ablation. Using a Zn target, zinc oxide films were deposited on indium tin oxide (ITO) substrates using a picosecond Nd:YVO₄ laser (8 ps, 50 kHz, 532 nm, 0.17 J/cm²) in an oxygen atmosphere at room temperature (RT). The morpho-structural characteristics of ZnO films deposited at different oxygen pressures (150–900 mTorr) and gas flow rates (0.25 and 10 sccm) were studied. The post-deposition influence of annealing (250–550 °C) in oxygen on the film characteristics was also investigated. At RT, a mixture of Zn and ZnO formed. At substrate temperatures above 350 °C, the films were completely oxidized, containing a ZnO wurtzite phase with crystallite sizes of 12.2–40.1 nm. At pressures of up to 450 mTorr, the porous films consisted of well-distinguished primary nanoparticles with average sizes of 45–58 nm, while at higher pressures, larger clusters (3.1–14.7 μm) were dominant, leading to thicker films; higher flow rates favored clustering.     

Phase stabilization and microstructural studies of lead lanthanum titanate thin films

Thin ferroelectric films of PLTx (Pb_1−xLa_xTi_1−x/4O₃) have been prepared by a sol-gel spin coating process. As deposited films were thermally treated for crystallization and formation of perovskite structure. Characterization of these films by X-ray diffraction (XRD) have been carried out for various concentrations of La (x = 0.04, 0.08 and 0.12) on ITO coated corning glass substrates. For a better understanding of the crystallization mechanism, the investigations were carried out on films annealed at temperatures (350, 450, 550 and 650 °C). Characterization of these films by X-ray diffraction shows that the films annealed at 650 °C exhibit tetragonal phase with perovskite structure. Atomic force microscope (AFM) images are characterized by slight surface roughness with a uniform crack free, densely packed structure. Fourier transform infrared spectra (FTIR) studies of PLTx thin films (x = 0.08) deposited on Si substrates have been carried out to get more information about the phase stabilization.     

Preparation, dielectric and ferroelectric properties of Pb5Ge3O11 and Pb5Ge2.85Si0.15O11 thin films fabricated by sol-gel process

Lead germanate-silicate (Pb₅Ge_2.85Si_0.15O₁₁) ferroelectric thin films were successfully fabricated on Pt/Ti/SiO₂/(100)Si substrates by the sol-gel process. The thin films were fabricated by multi-coating at preheating temperatures of 350 and 450 °C. After annealing the thin films at 600 °C, the films exhibited c-axis preferred orientation. The degree of c-axis preferred orientation of the thin films preheated at 350 °C was higher than that of films preheated at 450 °C. Grain growth was influenced by the annealing time. The thin films exhibited a well-saturated ferroelectric P-E hysteresis loop when preheated at 350 °C and annealed at 600 °C for 1.5 h. The values of the remanent polarization (Pr) and the coercive field (Ec) were approximately 2.1 μC/cm² and 100 kV/cm, respectively.     

Study on physical properties of indium-doped zinc oxide deposited by spray pyrolysis technique

Transparent conducting indium doped zinc oxide (IZO) thin films have been deposited on soda-lime glass substrates by the spray pyrolysis technique. The structural, electrical, and optical properties of these films were investigated as a function of substrate temperature. In this work the substrate temperature was varied between 350 °C and 500 °C. X-ray diffraction pattern reveals that at 350 °C dominant peak is (100) orientation. By increasing substrate temperature from 350 °C to 450 °C, sheet resistance decreases, from 302 Ω/□ to 26 Ω/□, then at 500 °C increases to 34 Ω/□. In the useful range for deposition (i.e. 450 °C to 500 °C), the orientation of the films was predominantly (002). The lowest sheet resistance (26Ω/□) is obtained at substrate temperature of about 450 °C with the transmittance of about 75%. Study of scanning electron microscopy images shows that films deposited at 400 °C, have grain size as large as 574 nm, while with increasing substrate temperature to 450 °C, grain size becomes smaller and reaches to a value of about 100 nm with spherical shape. At 500 °C grain size value would be around 70 nm with the same spherical shape.     

The influence of annealing temperature on the structural, electrical and optical properties of ion beam sputtered CuInSe2 thin films

CuInSe₂ (CIS) thin films were prepared by ion beam sputtering deposition of copper layer, indium layer and selenium layer on BK7 glass substrates followed by annealing at different temperatures for 1 h in the same vacuum chamber. The influence of annealing temperature (100-400 °C) on the structural, optical and electrical properties of CIS thin films was investigated. X-ray diffraction (XRD) analysis revealed that CIS thin films exhibit chalcopyrite phase and preferential (112) orientation when the annealing temperature is over 300 °C. Both XRD and Raman show that the crystalline quality of CIS thin film and the grain size increase with increasing annealing temperature. The reduction of the stoichiometry deviation during the deposition of CIS thin films is achieved and the elemental composition of Cu, In and Se in the sample annealed at 400 °C is very near to the stoichiometric ratio of 1:1:2. This sample also has an optical energy band gap of about 1.05 eV, a high absorption coefficient of 10⁵ cm⁻¹ and a resistivity of about 0.01 Ω cm.     

Electrical and optical properties of Zn-In-Sn-O transparent conducting thin films

Indium tin oxide (ITO) is one of the widely used transparent conductive oxides (TCO) for application as transparent electrode in thin film silicon solar cells or thin film transistors owing to its low resistivity and high transparency. Nevertheless, indium is a scarce and expensive element and ITO films require high deposition temperature to achieve good electrical and optical properties. On the other hand, although not competing as ITO, doped Zinc Oxide (ZnO) is a promising and cheaper alternative. Therefore, our strategy has been to deposit ITO and ZnO multicomponent thin films at room temperature by radiofrequency (RF) magnetron co-sputtering in order to achieve TCOs with reduced indium content. Thin films of the quaternary system Zn-In-Sn-O (ZITO) with improved electrical and optical properties have been achieved.The samples were deposited by applying different RF powers to ZnO target while keeping a constant RF power to ITO target. This led to ZITO films with zinc content ratio varying between 0 and 67%. The optical, electrical and morphological properties have been thoroughly studied. The film composition was analysed by X-ray Photoelectron Spectroscopy. The films with 17% zinc content ratio showed the lowest resistivity (6.6 × 10^− 4 Ω cm) and the highest transmittance (above 80% in the visible range). Though X-ray Diffraction studies showed amorphous nature for the films, using High Resolution Transmission Electron Microscopy we found that the microstructure of the films consisted of nanometric crystals embedded in a compact amorphous matrix. The effect of post deposition annealing on the films in both reducing and oxidizing atmospheres were studied. The changes were found to strongly depend on the zinc content ratio in the films.     

Influence of annealing on characteristics of tin disulfide thin films by vacuum thermal evaporation

In this paper, we reported on an approach to prepare tin disulfide (SnS₂) thin films on soda-lime glass substrates by vacuum thermal evaporation using SnS₂ powders as a source. The influence of annealing on the chemical composition, crystal structure, surface morphology, and optical band gap of the SnS₂ thin films was systemically investigated. The as-grown SnS₂ thin film was amorphous, homogeneous, smooth, nearly stoichiometric, with no pinhole and crack free, and with an optical band gap of 2.41 eV. After the SnS₂ thin film was annealed at 300 °C, the crystallization of SnS₂ was demonstrated by X-ray diffraction and scanning electron microscope with a characteristic of a preferred orientation along (001) plane with hexagonal phase and the sheet appearance of the SnS₂ crystals. At the annealing temperature of 350 °C, some SnS₂ crystallites and a few pinholes appeared on the surface of the SnS₂ thin films, though the SnS₂ thin film was not oxidized. When the annealing temperature was increased to 400 °C, SnS₂ was gradually oxidized into an approximate spherical shape of SnO₂ from the top to the bottom of the SnS₂ thin film by trace O₂ in the furnace. Therefore, our experiment suggested that the annealing temperature of the SnS₂ thin film using the vacuum thermal evaporation should not be over 300 °C as a window layer in compound thin film solar cells.     

Influence of post-annealing temperature on the properties exhibited by ITO, IZO and GZO thin films

In this work we present a study on the effect of annealing temperatures on the structural, morphological, electrical and optical characteristics of gallium doped zinc oxide (GZO), indium zinc oxide (IZO) and indium-tin-oxide (ITO) films. GZO and IZO films were deposited at room temperature by r.f. magnetron sputtering, whereas the ITO films were commercial ones purchased from Balzers. All films were annealed at temperatures of 250 and 500 °C in open air for 1 h. The GZO and ITO films were polycrystalline. The amorphous structure of as-deposited IZO films becomes crystalline on high temperature annealing (500 °C). The sheet resistivity increased with increase in annealing temperature. GZO films showed an increase of 6 orders of magnitude. The optical transmittance and band gap of as-deposited films varied with annealing. The highest transmittance (over 95 %) and maximum band gap (3.93 eV) have been obtained for ITO films.     

Epitaxial growth and surface morphology of aluminum films deposited on mica studied by transmission electron microscopy and atomic force microscopy

The bulk structure and epitaxial growth of aluminum films deposited on mica substrates by thermal evaporation in a wide temperature range (16-550 °C) in high vacuum were investigated by transmission electron microscopy and transmission electron diffraction. The surface morphology of the films was observed and analyzed by atomic force microscopy. The films prepared at room temperature consist of single crystals having a diameter of 90 ± 40 nm with (111) planes. The surface of the films comprises spherical grains with morphology that is caused by self-shadowing during the deposition. The surface of the films becomes smoother as the temperature increases, and atomically-smooth surfaces with a root-mean-square roughness of about 0.45 nm over an area of 1 μm² are obtained at 250-350 °C. The crystals are oriented randomly along the [111] direction perpendicular to the substrate. The surface of the films consists of larger (> 300 nm) grains with terraces, and the surface becomes rough above 400 °C. Films with well-oriented single crystals along the [111] direction perpendicular to the substrate are obtained above 520 °C. The films grown epitaxially at 520-550 °C are characterized by the isolated grains with a diameter of 1220 ± 450 nm.     

Comparative study of ITO and FTO thin films grown by spray pyrolysis

Tin doped indium oxide (ITO) and fluorine doped tin oxide (FTO) thin films have been prepared by one step spray pyrolysis. Both film types grown at 400 °C present a single phase, ITO has cubic structure and preferred orientation (4 0 0) while FTO exhibits a tetragonal structure. Scanning electron micrographs showed homogeneous surfaces with average grain size around 257 and 190 nm for ITO and FTO respectively.The optical properties have been studied in several ITO and FTO samples by transmittance and reflectance measurements. The transmittance in the visible zone is higher in ITO than in FTO layers with a comparable thickness, while the reflectance in the infrared zone is higher in FTO in comparison with ITO. The best electrical resistivity values, deduced from optical measurements, were 8 × 10⁻⁴ and 6 × 10⁻⁴ Ω cm for ITO (6% of Sn) and FTO (2.5% of F) respectively. The figure of merit reached a maximum value of 2.15 × 10⁻³ Ω⁻¹ for ITO higher than 0.55 × 10⁻³ Ω⁻¹ for FTO.