Eco-friendly method of fabricating indium-tin-oxide thin films using pure aqueous sol-gel

An indium-tin-oxide (ITO) thin film with approximately 50 nm thickness was successfully synthesized on glass substrates by using a fully aqueous sol-gel process. The sol was prepared from indium nitrate hydrate and tin fluoride as a precursor. Thermogravimetric analysis confirmed that the sol converted into crystalline ITO at 286 °C. The optical band gap and transmittance of the thin film were observed to increase with annealing temperature and plasma treatment time. X-ray photoelectron spectroscopy and transmittance studies established that the number of oxygen vacancies in the thin film drastically increased with increasing temperature and plasma treatment. The annealing temperature and argon plasma treatment time appear to be key factors in reducing resistivity and increasing the transmittance of the thin film. A considerable decrease in the resistivity of the ITO thin film was observed after Ar plasma treatment. This eco-friendly sol-gel ITO thin film may find potential applications in n-type ohmic electrodes for ink-jet printable electronics.     

Crystallisation kinetics of hydroxyapatite thin films prepared by sol-gel process

Abstract

Abstract

In this study, the crystallisation of nano hydroxyapatite (HA) films on stainless steel 316L was studied. The film was prepared by sol-gel technique. The process was started with preparation of an HA sol. After aging of the sol at room temperature, a stainless steel 316L substrate was dip coated and then was heat treated from 350 to 450°C at different periods of time in air. The crystallisation behaviour and the transformation-temperature-time diagram of HA films were achieved and analysed using the avrami equation. The results showed that the crystallisation of HA began at 250°C and was increased up to 450°C. The obtained HA film showed a nanostructure character with a suitable crystalinity after heat treatment.     

Seed-mediated electrochemical growth of gold nanostructures on indium tin oxide thin films

Two-dimensional gold nanostructures (Au NSs) were fabricated on amine-terminated indium tin oxide (ITO) thin films using constant potential electrolysis. By controlling the deposition time and by choosing the appropriate ITO surface, Au NSs with different shapes were generated. When Au NSs were formed directly on aminosilane-modified ITO, the surface roughness of the interface was largely enhanced. Modification of such Au NSs with n-tetradecanethiol resulted in a highly hydrophobic interface with a water contact angle of 144°. Aminosilane-modified ITO films further modified with colloidal Au seeds before electrochemical Au NSs formation demonstrated interesting optical properties. Depending on the deposition time, surface colors ranging from pale pink to beatgold-like were observed. The optical properties and the chemical stability of the interfaces were characterized using UV-vis absorption spectroscopy. Well-defined localized surface plasmon resonance signals were recorded on Au-seeded interfaces with λ_max = 675 ± 2 nm (deposition time 180 s). The prepared interfaces exhibited long-term stability in various solvents and responded linearly to changes in the corresponding refractive indices.     

Porous indium oxide thin films deposited by electrostatic spray deposition technique

This paper presents the preparation process of porous indium oxide (In₂O₃) films using a novel deposition technique, i.e., electrostatic spray deposition (ESD). The films were deposited on platinum-coated alumina substrates using as precursor solution indium chloride in ethanol and acetic acid. The films were characterized using scanning electron microscopy (SEM), X-ray diffraction (XRD), transmission electron microscopy (TEM) and Raman spectroscopy. The nanocrystalline structure of the films was evidenced by TEM and also by XRD studies. The Raman spectroscopy and XRD measurements revealed the cubic phase of In₂O₃ films. Considering the obtained results, we conclude that the ESD technique is an efficient, cheap and successful method for the preparation of porous indium oxide films.     

Tunable surface plasmon resonance frequencies of monodisperse indium tin oxide nanoparticles by controlling composition,size, and morphology

Monodisperse indium tin oxide nanoparticles (ITO NPs) with high crystallinity have been synthesized by the rapid thermal injection method and the seed-mediated growth method. We demonstrate that the surface plasmon resonance (SPR) frequencies of ITO NPs can be manipulated from 1,600 to 1,993 nm in near-infrared band by controlling the composition, size, and morphology. The doping Sn concentration in ITO NPs could be controlled via changing the %Sn in the initial feed from 0% to 30%. The shortest SPR wavelength at 1,600 nm with 10% Sn doping concentration indicates highest free electron carrier concentration in ITO NPs, which has direct relationship with doping Sn⁴⁺ ions. Furthermore, we demonstrate that the SPR peaks can also be tuned by the size of ITO NPs in the case of uniform doping. Besides, compared with the ITO NPs, single crystalline ITO with nanoflower morphology synthesized through the one-pot method exhibit SPR absorption peak features of red-shifting and broadening.     

Photocatalytic properties of visible-light enabling layered titanium oxide/tin indium oxide films

Visible-light enabling titanium oxide/tin indium oxide (TiO₂/ITO) thin films deposited on unheated glass slides with prolonged deposition duration were investigated in this study. Structural properties characterized by X-ray diffraction (XRD), Raman spectra and scanning electron microscopy (SEM) showed typical polycrystalline structure with primary anatase phase along with elongated pyramid-like grains lying on the film surface and densely packed columnar structure from cross-sectional profile. The XRD preferential peak of (2 1 1) and the Raman peak intensity at 640 cm⁻¹ dramatically increased without noticeable broadening and shift as the deposition time was prolonged beyond 2 h. This implies that more perfectly crystalline structure, less internal stress, and comparatively larger grains were obtained by this technique. The Ti2p_3/2 and O1s XPS peaks shifted toward higher binding energy suggest that the local chemical state was influenced by the prolonged deposition duration in the film, which resulted in red shift of absorption threshold into visible-light region. Under ultra-violet (UV) and visible-light illumination, the visible-light enabling film exhibited the best photocatalytic activity on MB degradation with the rate-constant of about 0.231 h⁻¹. Hydrophilic conversion rate was estimated to be 8.14 × 10⁻³ deg⁻¹ min⁻¹ and long-term UV-induced hydrophilicity of 10° in the dark storage up to 72 h was observed. In addition to its inherent characteristics of the layered TiO₂/ITO structure on hole/electron separation, all these could be attributed to more perfectly formed crystalline structure, densely packed columnar crystals and the surface roughness along with its enlarged surface area.     

Optimizing the processing conditions of sodium potassium niobate thin films prepared by sol-gel spin coating technique

In the present study, potassium sodium niobate (KNN) thin films were synthesized by means of sol-gel spin coating method. Along with the synthesis, the effects of annealing temperature and various number of coating layers on both the structural and electrical properties were looked into. The results of the study revealed that the annealing temperature had a great impact on the properties of KNN. In addition, the XRD diffractograms and texture coefficient of the synthesized films confirmed that a highly oriented orthorhombic perovskite structure was obtained at 650 °C, whereas at a relatively higher temperature (700 °C), a spurious phase of K₄Nb₆O₁₇ was evolved. In addition, the growth of KNN at 650 °C exhibited a reasonable resistivity value for piezoelectric applications. Looking into the results, it was discovered that the KNN thin films also found to be dependent on a number of coating layers. Field emission scanning electron microscopy (FESEM) showed that KNN with five coating layers was highly crystalline, cracks-free, and had significantly more homogenous surface morphology and the size of grains being uniform, the resistivity of KNN thin films improved with the increasing number of coating layers i.e., up to five.     

Characteristics of carbon films prepared by plasma-based ion implantation

A series of carbon films have been prepared by plasma-based ion implantation (PBII) with C on pure Al and Si. Emphasis has been placed on the effect of implanting voltage on the characteristics of these films. The structures of the films were analyzed by X-ray photoelectron spectroscopy (XPS) and Raman spectroscopy. The morphologies were observed by atomic force microscope (AFM). Surface hardness and electrical resistivity were also measured. The results indicate that the characteristics of these films are strongly dependent on the implanting voltage. An implanting voltage threshold value ranging from 3 to 5 kV starts to form a C-substrate transition layer owing to C⁺ ions implanted into the substrate. The transition layer exhibits a gradual change in composition and structure and effectively connects the carbon film and the substrate. Also, an implanting voltage threshold value ranging from 5 to 10 kV starts to form diamond-like carbon (DLC) films. An increasing voltage causes the resultant DLC films to be smoother and more compact. Moreover, Raman spectrum, chemical state of C1s, surface hardness and electrical resistivity all prove an optimum voltage of approximately 30 kV corresponding to the lowest ratio of sp²/sp³.     

Effect of surface roughness and surface modification of indium tin oxide electrode on its potential response to tryptophan

The effect of surface modification of indium tin oxide (ITO) electrode on its potential response to tryptophan was investigated for ITO substrates with different surface roughness. It was found that a small difference in surface roughness, between ∼1 and ∼2 nm of R_a evaluated by atomic force microscopy, affects the rest potential of ITO electrode in the electrolyte. A slight difference in In:Sn ratio at the near surface of the ITO substrates, measured by angle-resolved X-ray photoelectron spectrometry and Auger electron spectroscopy is remarkable, and considered to relate with surface roughness. Interestingly, successive modification of the ITO surface with aminopropylsilane and disuccinimidyl suberate, of which essentiality to the potential response to indole compounds we previously reported, improved the stability of the rest potential and enabled the electrodes to respond to tryptophan in case of specimens with R_a values ranging between ∼2 and ∼3 nm but not for those with R_a of ∼1 nm. It was suggested that there are optimum values of effective work function of ITO for specific potential response to tryptophan, which can be obtained by the successive modification of ITO surface.     

Structural,thermal, micromechanical and electrical study of polyimide composite thin films incorporating indium tin oxide

Studies of composite films incorporating inorganic materials are of immense importance for current technological applications. Polyimide (PI) composite thin films incorporating indium tin oxide (ITO) at various weight ratios were processed using an in situ generation approach. The resultant product was imidized up to 350 °C to test the ability of the material to endure high temperatures without affecting the host matrix. The morphological behaviour of the PI/ITO composite films was investigated using Fourier transform infrared, scanning electron microscopy and atomic force microscopy characterization techniques. The degrees of crystallinity and ITO particle size within the PI matrix were studied using X‐ray diffraction. The thermal, structural and electrical properties were analysed using thermogravimetric analysis, differential scanning calorimetry, UV‐visible spectroscopy and the four‐probe technique. The micromechanical properties of the composites were evaluated in terms of tensile strength, tensile modulus and elongation. An overall improvement in the properties of the composite films was observed in comparison to those of pure PI. The synergistic improvement in the composite films is associated with the interaction mechanism between ITO and PI, where ITO becomes dispersed and interacts within the PI matrix. This leads to a decrease in available free‐space volume and increases the surface enrichment providing reinforcement to the matrix. Copyright © 2010 Society of Chemical Industry     

Preparation of ITO/Ag nanohybrid particles by a reverse micellar layer-by-layer coating

Silver (Ag) nanoparticles were adsorbed preferentially on indium tin oxide (ITO) surface to form composite particles using a reverse micellar layer-by-layer deposition. The micellar process stabilized the Ag particles by an anionic sodium bis(2-ethylhexyl) sulfosuccinate (AOT) surfactant in isooctane solvent. The ITO particles surface was mediated by a cationic poly(allylamine hydrochloride) (PAH) polyelectrolyte. The heterogeneous deposition was rendered by both electrostatic attraction and hydrophilic/hydrophobic interaction, and was carried out in multiple coating cycles. The resulting hybrid particles were characterized by zeta-potential measurement, electron microscopy, X-ray diffractometry, and inductively coupled plasma analysis, respectively. Optical transmittance of the ITO/Ag composite films was found to decrease substantially with the Ag deposition over the visible wavelengths range, arising mainly from scattering induced by the Ag nanoparticles.     

液相共沉淀法制备氧化铟锡超细粉体材料的研究进展

介绍了液相共沉淀法制备氧化锢超细锡粉体材料的工艺,分析了沉淀剂、反应物的浓度、煅烧的温度和时间、分散剂等四个因素对制备过程及产物的影响。按照三氧化铟和二氧化锡的质量比为9∶1选用铟盐和锡盐；用氨水、尿素或碳酸铵作沉淀剂,并且沉淀剂不同,反应时应控制的pH值和反应时间也不同；反应物In~(3+)的浓度0．2mol／L时可得到接近纳米级的超细氧化铟锡粉体材料；700～800℃煅烧3～5h,可使前驱物成为球状,其团聚现象也可以得到综合平衡；分散剂为硫酸铵、硅烷偶联剂KH570等,对其分散机理作了简要的分析。     

Nonlinear growth of zinc tin oxide thin films prepared by atomic layer deposition

Zinc tin oxide (ZTO) thin films can be deposited by atomic layer deposition (ALD) with adjustable electrical, optical and structural properties. However, the ternary ALD processes usually suffer from low growth rate and difficulty in controlling film thickness and elemental composition, due to the interaction of ZnO and SnO₂ processes. In this work, ZTO thin films with different Sn levels are prepared by ALD super cycles using diethylzinc, tetrakis(dimethylamido)tin, and water. It is observed that both the film growth rate and atom composition show nonlinear variation versus [Sn]/([Sn]+[Zn]) cycle ratio. The experimental thickness measured by spectroscopic ellipsometry and X-ray reflectivity are much lower than the expected thickness linearly interpolated from pure ZnO and SnO_x films. The [Sn]/([Sn]+[Zn]) atom ratios estimated by X-ray photoelectron spectroscopy have higher values than that expected from the cycle ratios. Hence, to characterize the film growth behavior versus cycle ratio, a numerical method is proposed by simulating the effect of reduced density and reactivity of surface hydroxyls and surface etching reactions. The structure, electrical and optical properties of ZTO with different Sn levels are also examined by X-ray diffraction, atomic force microscope, Hall measurements and ultraviolet–visible–infrared transmittance spectroscopy. The ZTO turns out to be transparent nanocrystalline or amorphous films with smooth surface. With more Sn contents, the film resistivity gets higher (>1 Ω cm) and the optical bandgap rises from 3.47 to 3.83 eV.     

Structural,morphological, and optical properties of W-doped VO2 thin films prepared by sol-gel spin coating method

Thermochromic VO₂ thin films were deposited on soda-lime glass via sol-gel method. Doping was done through adding tungstic acid solution to the vanadium solution precursor. Grazing incidence x-ray diffractometer (GIXRD) results showed that VO₂ and V₆O₁₃ phases were formed together in the heat-treated sample. According to the GIXRD result of the W-doped sample, only VO₂ remained. Field-emission scanning electron microscopy (FESEM) micrographs showed that the VO₂ grain size decreased from about 70 to about 25 nm for undoped film and 2 wt% W-doped films, respectively. Atomic force microscopy (AFM) results showed that the root mean square roughness for the film with 180 nm thickness was about 18 nm, and 2 wt% W-doped film had a smoother surface. Diffuse reflectance spectroscopy (DRS) results showed that the band gap energy for undoped, 1 wt% W- doped, and 2 wt% W-doped VO₂ thin films was 1.7, 1.3, and 0 eV, respectively. Four-point probe resistivity measurements showed a significant decrement, from approximately 1 MΩ at 15°C to <100 Ω at 80°C. Regarding Vis-NIR spectroscopy results, maximum optical transmission for undoped and W-doped films was approximately 75% and 35%, respectively.     

High recoverable energy storage density in (1-x)Bi0.5(Na0.8K0.2)0.5TiO3-xSrZrO3 thin films prepared by a sol-gel method

Lead-free (1-x)Bi_0.5(Na_0.8K_0.2)_0.5TiO₃-xSrZrO₃ (abbreviated as BNKT-100xSZ) thin films were deposited on Pt(111)/Ti/SiO₂/Si using sol-gel/spin coating method. With the addition of SZ, the long-range ferroelectric order dominant in BNKT is disrupted, which boosts the ferroelectric relaxor behavior. Consequently, a high recoverable energy density of 34.69?J/cm³ combined with an efficiency of 59.32% was achieved at the optimal composition of BNKT-15SZ under a high electric field of 2100?kV/cm, which can be ascribed to the slim P-E loops induced by strong relaxor behavior (γ?=?1.93) and the enhanced breakdown strength. Moreover, BNKT-15SZ thin film capacitor presents a good thermal stability with minimal variations of the energy density (<10%) and the energy storage efficiency (<5%) over a wide temperature range of 30–100?°C. The results indicated that the BNKT-100xSZ thin films may be a promising environmental-friendly material for energy storage applications.     

High recoverable energy storage density and large piezoelectric response in (Bi0.5Na0.5)TiO3-PbTiO3 thin films prepared by a sol-gel method

Low-lead-content (1-x)(Bi_0.5Na_0.5)TiO₃-xPbTiO₃ (x = 0, 0.05, 0.10, 0.15, 0.25) (hereafter abbreviated as BNT-xPT) thin films were prepared by a sol-gel method, and their crystal structure, dielectric properties, recoverable energy-storage density and piezoelectric response were investigated as a function of PT concentration. Combining the XRD patterns and Raman spectroscopy indicate the phase structures go through rhombohedral (R) – rhombohedral + tetragonal (R + T) – tetragonal (T) evolution with increasing of PT content. A high recoverable energy storage density of 13.02 ± 0.39 J/cm³ was achieved in the BNT-0.10PT thin films due to the high field endurance and significantly enhanced polarizability. Moreover, a superior piezoelectric response (d₃₃^* = 120 ± 5 pm/V) was also obtained in the 10% PT-modified BNT films, which can be attributed to easy polarization rotation due to low polarization anisotropy on the R-T phase boundary. These properties indicate that BNT-0.10PT films might be promising multifunctional materials for piezoelectric micro-actuator and energy storage embedded capacitor applications.     

The phase formation process of Bi0.5(Na0.8K0.2)0.5TiO3 thin films prepared using the sol-gel method

Lead-free Bi_0.5(Na_0.8K_0.2)_0.5TiO₃ (abbreviated as BNKT) thin films were grown on Pt(111)/Ti/SiO₂/Si substrates using a sol-gel/spin coating technique and were then annealed at different temperatures (350 °C, 550 °C, 750 °C and 850 °C). Analysis of the XRD patterns and FT-IR spectra were used to determine the main reactions and the phase formation process of BNKT thin films during the sol-gel process. The results show that the dielectric constant of the thin films attains a maximum at a set temperature and then decreases at higher annealing temperatures, which can be attributed to phase formation and transformation. Moreover, the morphologies of the BNKT thin films improve with the increase in grain size and the formation of distinct grain boundaries. Furthermore, through increasing the pH of the precursor solutions, the size of the sol-gel colloidal particles increases slightly and the grains formed from the corresponding solutions tend to be small and uniform.     

Characterization of non-stoichiometric Ga2O3-x thin films grown by radio-frequency powder sputtering

We report the synthesis and characterization of non-stoichiometric Ga₂O_3-x thin films deposited on sapphire (0001) substrates by radio-frequency powder sputtering. The chemical and electronic states of the non-stoichiometric Ga₂O_3-x thin films were investigated. By sputtering in an Ar atmosphere, the as-grown thin films become non-stoichiometric Ga₂O_2.7, due to the difference in sputtering yield between Ga and O species of the Ga₂O₃ target. The electronic states of the thin films consist of ~85% Ga³⁺ and ~15% Ga¹⁺, corresponding to Ga₂O₃ and Ga₂O, respectively. The films have the electrical characteristics of a semiconductor, with electrical conductivity of approximately 5.0 × 10^-4 S cm^-1 and a carrier concentration of 4.5 × 10¹⁴ cm^-3 at 300 K.     

Field emission enhancement of amorphous carbon films by nitrogen-implantation

Effect of nitrogen-implantation on electron field emission properties of amorphous carbon films has been examined. Raman and X-ray photoelectron spectroscopy measurements reveal different types of C-N bonds formed upon nitrogen-implantation. The threshold field is lowered from 14 to 4 V/μm with increasing the dose of implantation from 0 to 5 × 10¹⁷ cm⁻² and the corresponding effective work function is estimated to be in the range of 0.01-0.1 eV. From the perspective of tetrahedron bond formation, a mechanism for the nitrogen-lowered work function is proposed, suggesting that both the nitrogen nonbonding (lone pair) and the lone-pair-induced carbon antiboding (dipole) states are responsible for lowering the work function and hence the threshold field.