Properties of thin In2O3 and SnO2 films prepared by corona spray pyrolysis, and a discussion of the spray pyrolysis process

Thin films of doped In₂O₃ and SnO₂ were prepared by the “corona spray pyrolysis” technique with a deposition efficiency of 80%. The electrical and optical properties of the films were determined. A transmission of 88% in the visible region and an IR reflection of more than 90% were the maximum values obtainable for a doped In₂O₃ film.

A detailed discussion of the physical and chemical processes that occur during spray pyrolysis is presented to aid the understanding of this coating technique.

A minimum temperature of about 350°C for the formation of In₂O₃ was empirically confirmed.

Furthermore the powdery precipitate obtained during deposition of In₂O₃ was clearly identified as polycrystalline In₂O₃ formed by a homogeneous reaction.     

Ozone sensing using In2O3-modified Ga2O3 thin films

It is shown that at elevated temperatures the conductance of an In ₂O₃-modified Ga₂O₃ thin film depends significantly and reversibly on the ozone concentration in the ambient air. This ozone sensitivity is much greater than with pure Ga ₂O₃ or In₂O₃ thin films, respectively. The ozone sensitivity of the In₂O₃-modified Ga₂O₃ thin film is characterized by an impressive selectivity, and is maximal at an operation temperature of about 600°C. The cross sensitivities to other gases present in ambient conditions are small compared to the ozone sensitivity, thus opening the way to use this system for ambient ozone monitoring. The results are discussed using an electron injection model     

Indium tin oxide thin films for metallization in microelectronic devices

The use of sputtered indium tin oxide (ITO) thin films as metal layers in silicon-based electronic circuits has been investigated. The ITO films were sputtered directly from In₂O₃/SnO₂ targets under inert ambient in an r.f. sputtering system. The films were characterized as functions of process parameters such as r.f. power, substrate temperature and post-deposition annealing treatments. The properties studied included sheet resistance, transparency, thickness uniformity, composition and structure, step coverage, and etchability. In addition, the suitability of these ITO films as interconnects in microelectronic devices was examined by fabricating MOSFET devices using fine line patterned ITO for the metallization.     

The influence of film structure on In2O3 gas response

This paper reports the influence of In₂O₃ film structure on gas-sensing characteristics measured in steady state and transient modes. Films were deposited by spray pyrolysis from InCl₃–water solutions. Correlation between gas-sensing parameters and structural parameters such as film thickness (20–400 nm), grain size (10–70 nm), refractive index and film texture (I(400)/I(222)) were established. It was shown that grain size and porosity are the parameters of In₂O₃ films that best control gas response to ozone. In the detection of reducing gases, the influence of film structure is less important. Decreases in film thickness, grain size and degree of texture are the best way to decrease time constants of the gas response of In₂O₃-based gas sensors.     

ZnO/In2O3纳米异质结的合成及其光催化性能的研究

通过热水解法成功制备出了形貌均一的ZnO/In₂O₃异质结光催化材料, 采用场发射扫描电子显微镜(FESEM)、X射线衍射仪(XRD)以及透射电子显微镜(TEM)对样品的形貌及结构进行表征。结果表明: ZnO/In₂O₃异质结是由直径约200~300 nm、厚度约40~60 nm的六边形纳米片镶嵌着In₂O₃纳米小颗粒组成。对比纯ZnO、纯In₂O₃和该光催化材料对罗丹明B(RhB)的可见光降解效率, 发现ZnO/In₂O₃异质结光催化材料对RhB具有较高的光催化效率, 其原因是窄带系半导体In₂O₃能够有效地吸收可见光, 当ZnO与In₂O₃ 形成异质结时, In₂O₃能带上被可见光激发的电子会迁移到ZnO的导带上, 而光激发的空穴仍保留在In₂O₃价带, 这样有助于光生电子和空穴的分离, 降低其复合几率, 从而有效地提高了ZnO的光催化效率。     

Investigation of a new In2O3-based selective H2 gas sensor with low power consumption

The nanometer-size In₂O₃ was synthesized via a reverse microemulsion. A new catalytic combustion-type In₂O₃-based H₂ gas sensor was developed based on the technology for fabricating the direct-heating-type sensor and a surface-modifying process. A dense SiO₂ layer near the surface of the sensor was formed by chemical vapor deposition (CVD) of hexamethyldisiloxane (HMDS). The SiO₂ layer, which acted as a molecular sieve, reduced the penetration of large molecular, such as C₂H₅OH, CH₄, i-C₄H₁₀, into the sensing layer, resulting in the improvement of selectivity to H₂. The sensitive properties and the working mechanism of the sensor were presented. The In₂O₃ nanoparticles prepared by microemulsion were characterized by transmission electron microscopy and X-ray diffraction.     

SnO2-Fe2O3复合材料应用于碳纳米管集流体对锂离子电池性能的影响

水热合成法制备纳米SnO₂-Fe₂O₃复合材料,以SnO₂-Fe₂O₃为活性物质,多壁碳纳米管（MWCNTs）导电纸代替传统铜箔作为负极集流体制作锂离子电池。采用XRD、SEM进行表征,结果显示,SnO₂-Fe₂O₃均匀嵌入到MWCNTs构建的三维导电网络的空隙中。电化学测试结果表明,SnO₂-Fe₂O₃/MWCNTs导电纸作为负极电极能够显著提高锂离子电池的循坏和倍率性能。在100 mA/g电流密度下循环30次,SnO₂-Fe₂O₃/MWCNTs导电纸电池比容量达到1 088 mAh/g,而在200 mA/g电流密度下循环200次后,SnO₂-Fe₂O₃/MWCNTs导电纸比容量能稳定保持在898 mAh/g,表现出良好的循环性能,逐渐增大充放电电流,电池的比容量有所下降但其库伦效率仍然保持在96%以上,而在高倍率（1 600 mA/g）下进行充放电时,SnO₂-Fe₂O₃/MWCNTs导电纸比容量仍然能够保持在547 mAh/g,之后再将电流密度降到100 mA/g,比容量重新回到1 000 mAh/g,SnO₂-Fe₂O₃/MWCNTs导电纸表现出十分优异的电化学性能。      

Properties of Indium Oxide Semiconducting Sensors Deposited by Different Techniques

Semiconducting In₂O₃ gas sensors have been fabricated by two different deposition techniques, i.e., spin-coating and screen-printing. In both cases the same starting material - sol-gel-prepared cubic In₂O₃ - was used for the deposition in order to ensure a better comparability of the different sensing layers. The morphology of the layers has been characterized using scanning electron microscopy (SEM) technique. The layers deposited by different methods show similar grain size and porosity. Furthermore, Dc electrical tests have been performed to analyze the sensing properties of the different gas sensors. Reducing gases (CO and propanal) as well as oxidizing gases (NO₂ and ozone) were used as test gases in the background of dry and humidified synthetic air. All measurements were performed at several temperatures. It was found that the spin-coated and screen-printed layers show different sensing properties, i.e., screen-printed sensors showed higher sensor signals than spin-coated sensors for CO, propanal, and NO₂. The most striking differences appeared in the detection of ozone. In this case, spin-coated sensors showed a higher performance than screen-printed sensors. Higher ozone concentrations led to saturation effects for the latter.     

Physics of very thin ITO conducting films with high transparency prepared by DC magnetron sputtering

The preparation of very thin indium tin oxide (ITO) films with extremely high transparency and suitable resistivity, as well as resistivity stability for long term use, is described. In order to obtain these properties, amorphous suboxide films were first prepared and then annealed. Suboxide films with a thickness of 20 to 30 nm were prepared on PET film and glass substrates at a temperature of 60 °C using In₂O₃---SnO₂ targets with a SnO₂ content of 0 to 10 wt% by DC magnetron sputtering in a pure argon gas atmosphere. The films were annealed at a temperature of 150 °C for 1 to 100 h in air. The resistivity of films on PET films was, depending on the SnO₂ content, on the order of 10⁻³ ω cm. An average transmittance above 97% in the visible wavelength range and a resistivity of about 4 × 10⁻³ ω cm, as well as resistivity stability, were attained in ITO films with a SnO₂ content of about 1 wt% prepared on PET films by the low-temperature process. It is thought that these properties result from crystallization which occurred during the annealing, duration up to about 25 h.     

Investigation on the cross sensitivity of NO2 sensors based on In2O3 thin films prepared by sol-gel and vacuum thermal evaporation

In₂O₃ thin films have been prepared from commercially available pure In₂O₃ powders by high vacuum thermal evaporation (HVTE) and from indium iso-propoxide solutions by sol-gel techniques (SG). The films have been deposited on sapphire substrates provided with platinum interdigital sputtered electrodes. The as-deposited HVTE and SG films have been annealed at 500°C for 24 and 1 h, respectively. The film morphology, crystalline phase and chemical composition have been characterised by SEM, glancing angle XRD and XPS techniques. After annealing at 500°C the films’ microstructure turns from amorphous to crystalline with the development of highly crystalline cubic In₂O_3−x (JCPDS card 6-0416). XPS characterisation has revealed the formation of stoichiometric In₂O₃ (HVTE) and nearly stoichiometric In₂O_3−x (SG) after annealing. SEM characterisation has highlighted substantial morphological differences between the SG (highly porous microstructure) and HVTE (denser) films. All the films show the highest sensitivity to NO₂ gas (0.7–7 ppm concentration range), at 250°C working temperature. At this temperature and 0.7 ppm NO₂ the calculated sensitivities (S=R_g/R_a) yield S=10 and S=7 for SG and HVTE, respectively. No cross sensitivity have been found by exposing the In₂O₃ films to CO and CH₄. Negligible H₂O cross has resulted in the 40–80% relative humidity range, as well as to 1 ppm Cl₂ and 10 ppm NO. Only 1000 ppm C₂H₅OH has resulted to have a significant cross to the NO₂ response.     

Influence of the sputtering system''s vacuum level on the properties of indium tin oxide films

The influence of the chamber residual pressure level in the radio frequency magnetron sputtering process on the electrical, optical and structural properties of indium thin oxide (ITO) is investigated. Several ITO films were deposited at various residual pressure levels on Corning glass using In₂O₃:SnO₂ target in argon atmosphere and without the addition of oxygen partial pressure. It is found that a very good vacuum is associated to metallic films and results in less transparent ITO films, with some powder formation on the surface. On the contrary highly transparent and conducting films are produced at a higher residual pressure. The best deposition conditions are addressed for ITO films as transparent conducting oxide layers in silicon heterojunction solar cells. Using the optimal vacuum level for ITO fabrication, a maximum short circuit current of 36.6 mA/cm² and a fill-factor of 0.78 are obtained for solar cells on textured substrates with a device conversion efficiency of 16.2%.     

An investigation by electron spectroscopy for chemical analysis of chemical treatments of the (100) surface of n-type InP epitaxial layers for Langmuir film deposition

The surface chemistry of InP substrates used for the fabrication of electronic devices (MIS structures) was examined by ESCA. Spectroscopic data on related materials such as indium metal, plasma-oxidized indium metal, In₂O₃, InPO₄(xH₂O), P₄O₁₀, AlPO₄, (C₆H₅O)₃PO and (C₆H₅)₃P were collected so as to aid the assignment of components in the spectra of as-received and etched InP surfaces on the basis of the chemical shifts and the intensity ratios. Surface features of InP substrates from several batches were examined in the as-received and the chemically etched forms. The effectiveness of several types of etchants and the features thus produced on the substrate surface were evaluated and are discussed.     

In2O3/InNbO4复合材料的热电性能研究

In₂O₃作为一种良好的光电和气敏材料, 因高温下具有优异的热电性能在热电领域也获得广泛关注。本研究通过固相反应法结合放电等离子烧结(SPS)成功将原位自生的InNbO₄第二相引入到In₂O₃基体中, 优化了块体样品的制备工艺。同时, InNbO₄改善了样品的电输运性能, 使载流子浓度明显提高, 在1023 K时电导率最高可达1548 S·cm^-1, 高于大多数元素掺杂的样品。其中, 0.998In₂O₃/0.002InNbO₄样品的热电性能测试表明, 在1023 K时, 其功率因子可达到0.67 mW·m^-1·K^-2, 热电优值(ZT)达到最高值0.187。综上所述, 通过在In₂O₃中原位复合InNbO₄第二相可以很好地改善In₂O₃基热电陶瓷的电性能, 进而调控其高温热电性能。     

Indium Tin Oxide Thin-Film Sensor for Detection of Volatile Organic Compounds (VOCs)

Indium tin oxide (ITO) (In₂O₃ + 17% SnO₂) thin films were grown on glass substrate by direct evaporation method. Two thick gold pads were deposited to take out contacts. The response of these films at different operating temperatures, when exposed to various volatile organic compounds (VOCs) such as methanol, ethanol, butanol, and acetone in the concentration range 200-2500 ppm was evaluated. Additionally, the effect of film thickness on the response charateristics of methanol and acetone was studied. The linearity and sensitivity of the sensors were measured. The ITO thin-film sensors showed a sensitivity of 0.256 ohms/ppm to acetone vapors, which was almost linear in the range 200-2500 ppm. In order to improve sensitivity and selectivity, a thin layer of various metal and metal oxides such as Cu and PbO was deposited on the sensor surface to work as catalytic layer and the effect on the performance of the sensor was studied. The response and recovery times of the sensor were determined for acetone vapors and were found to be 155 sec and 110 sec, respectively.     

Au修饰SnO2复合纳米材料的制备和气敏性能

以氯金酸和乙酰丙酮氯化锡为主要材料,通过一步水热法制备了SnO₂和Au修饰的SnO₂（Au/SnO₂）纳米粒子.使用TEM、EDS、XRD和XPS等手段对样品的形貌、组成及结构进行表征,研究了两种材料对乙醇的气敏性能.结果表明,两种纳米颗粒的尺寸都比较均一,平均直径约为9-12 nm;SnO₂为四方金红石结构,Au为面心立方结构;在Au/SnO₂样品中,Au与SnO₂的重量比为2.6%,Au元素主要以Au⁰的价态存在并含有少量的Au³⁺价态;与纯SnO₂纳米粒子相比,Au修饰可显著提高气敏元件对乙醇响应的灵敏度和选择性。     

Influence of the common varistor dopants (CoO, Cr2O3 and Nb2O5) on the structural properties of SnO2 ceramics

The influence of dopants commonly used in SnO₂ varistor ceramics, such as CoO, Cr₂O₃ or Nb₂O₅, on the structural properties of SnO₂ was investigated. Several SnO₂-based ceramics containing only one of the dopants were prepared and characterized. Spectroscopic investigations [visible, near infrared (IR) and IR region] were performed to obtain information about dopants valence states inside the ceramics, as well as about their influence on electronic structure of the material. Structural properties were investigated by X-ray diffraction analysis and mechanisms of dopant incorporation were proposed. Obtained results were confirmed with results of the electrical measurements. Microstructural changes in doped ceramics were investigated by scanning electron microscopy (SEM) analysis that showed great differences in densities, grain size, and morphology of the SnO₂ ceramics depending on type of dopants and their distribution.     

New transparent conducting MgIn2O4---Zn2In2O5 thin films prepared by magnetron sputtering

New materials for a transparent conducting oxide film are demonstrated. Highly transparent Zn₂In₂O₅ films with a resistivity of 3.9 × 10⁻⁴ Ω cm were prepared on substrates at room temperature using a pseudobinary compound powder target composed of ZnO (50 mol.%) and In₂O₃ (50 mol.%) by r.f. magnetron sputtering. MgIn₂O₄---Zn₂In₂O₅ films were prepared using MgIn₂O₄ targets with a ZnO content of 0–100 wt.%. The resistivity of the deposited films gradually decreased from 2 × 10⁻³ to 3.9 × 10⁻⁴ Ω cm as the Zn/(Mg + Zn) atomic ratio introduced into the films was increased. The greatest transparency was obtained in a MgIn₂O₄ film. The optical absorption edge of the films decreased as the Zn/(Mg + Zn) atomic ratio was increased, corresponding to the bandgap energy of their materials. It was found that the resistance of the undoped Zn₂In₂O₅ films was more stable than either the undoped MgIn₂O₄, ZnO or In₂O₃ films in oxidizing environments at high temperatures.     

The influence of substrate chemistry on the adhesion of electrolessly deposited Ni(P) on metal oxide coated ceramics

The adhesion of electrolessly deposited Ni(P) on alumina ceramic substrates which were coated with thin SiO₂, SnO₂, TiO₂, Al₂O₃, Y₂O₃, ZrO₂ and (In,Sn)O_x (ITO) films was studied. The adhesion was measured with the aid of the 90° peel test. Strong adhesion of Ni(P) was found for the substrates with ZrO₂ and Al₂O₃ coatings and weak adhesion for the substrates with SiO₂, TiO₂, SnO₂, Y₂O₃ and ITO coatings. The fracture path and the type of interfacial bonding were analysed using scanning electron microscopy, energy-dispersive analysis of X-rays and X-ray photoelectron spectroscopy. In the case of the strongly adhering samples, fracture took place through the metal layer and along the interface. In the case of the weakly adhering samples only interfacial failure was observed between the Ni(P) layer and the metal oxide coating. Cross-section transmission electron microscopy studies of the interfaces suggested that the differences in peel energy values are caused by differences in micromechanical interlocking at the metal oxide-Ni(P) interface. In addition, a weak boundary layer which was found to be present at the Ni(P)-alumina interface was absent in the case of the strongly adhering samples with the ZrO₂ substrate coating.     

Preparation of nanocrystalline SnO2 thin film coated Al2O3 ultrafine particles by fluidized chemical vapor deposition

Fluidized chemical vapor deposition (FCVD) technology was developed for coating SnO₂ thin film on Al₂O₃ ultrafine particles. TEM and HREM analysis found that SnO₂ films with different structures were deposited by controlling the coating temperature, reactant concentration, etc. Nanocrystalline SnO₂ film was coated at 573.15 K by gas phase reaction of SnCl₄ with H₂O. EPMA and EDS studies indicated that the distribution of SnO₂ inner and outer of the agglomerates was uniform. Nucleation and film deposition were coexisted mechanism during the FCVD coating process. The fraction of SnO₂ in the composite particles increased with increasing coating temperature, SnCl₄ concentration, and coating time. The mass fraction of SnO₂ in the composite particles increased strongly with the ratio of P_H2O and P_SnCl4 at low mole ratio of H₂O with SnCl₄, but increased little under the conditions of excess H₂O with respect to SnCl₄.     

Characterization of indium tin oxide film and practical ITO film by electron microscopy

In order to clarify the structure of indium oxide film containing tin and tin oxides, various In₂O₃ based films prepared by vacuum evaporation were studied using high-resolution electron microscope (HREM). Indium tin oxide (ITO) film was composed of In₂O₃ and SnO. SnO crystal also contained (110) or (101) crystallographic shear (CS) structures that indicate excess amounts of tin. The CS structure was also found in a commercial ITO film having the resistivity of 2×10⁻⁴ Ω cm.